November

2017

www.chemengonline.com

Industrial
Crystallization page 30

Facts at Your
Fingertips: Filter Aids Cooling Towers
Focus on Maintenance Membranes
& Reliability
Plant Security
Calcium
Hypochlorite Emergency
Production Shutdown Valves

Particle Size Analysis

P R E S S U R E I S R U N N I N G YO U R P L A N T S H O R T- H A N D E D .
Today, youre expected to do more with fewer people and resources meeting urgent
customer demands, cutting costs, improving efficiencies. While you may know us for our
reliable uid system components, were made for this kind of pressure too. With capabilities
like custom fabrication and assembly or inventory management, Swageloks authorized
sales and service centers offer critical assistance to plants short on resources. Its just one
more way were engineered to perform under pressure.

Learn more at swagelok.com/support

2017 Swagelok Company

For details visit adlinks.chemengonline.com/66434-26

 www.chemengonline.com

November 2017 Volume 124 | no. 11

Cover Story
30 Part 1 Confronting Crystallization Issues
Reliable information about industrial crystallization can be difficult to find, and
to apply to new situations. Following the work process outlined here will help
engineers approach crystallization challenges
38 Part 2 Industrial Crystallization for the CPI
This overview presents the traditional and emerging types of
continuous crystallizers

In the News
7 Chementator
A new C2-based production route to MMA; Deep-learning-
based AI quickly predicts furnace products; Lower costs for
converting alkylation units from HF to sulfuric acid; Extremophilic
microbes enable new methane pathways; New antimicrobial
compounds offer disinfectant alternatives; and more
12 Business News
AkzoNobel doubling capacity at organic peroxides plant in Ningbo;
Mitsui Chemicals starts production at expanded thermoplastic elastomers
plant; Cargill to build biodiesel plant in Kansas; Statoil, Shell and Total enter 30
CO2-storage partnership; and more
14 Newsfront Extending Membranes Reach Across the
CPI Advances in next-generation materials and assembly techniques have
enhanced membranes effectiveness in numerous applications
18 Newsfront Protect Your Plant Both physical security and
cybersecurity must be in place to keep chemical facilities safe from attack

Technical and Practical 14

28 Facts at your Fingertips Filter Aids This one-page reference

provides information about materials commonly used as filter aids in industrial
filtration processes
29 Technology Profile Calcium Hypochlorite Production 18
This process description outlines the manufacture of calcium hypochlorite
from slaked lime, sodium hydroxide and chlorine
44 Feature Report Cooling Towers: Keeping Your
Power Plant Cool General guidelines for selecting the appropriate
power-plant cooling system are presented here
44
51 Engineering Practice Emergency Shutdown Valves:
A Functional Safety Approach The relationship between valve
selection and safety certification still causes confusion. A focus on functional
safety can help to elucidate

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 1

 55 Solids Processing Powder and Bulk Solids Handling:
Particle-Size and Distribution Analysis The size and
distribution of particles are important determining factors in the design and
operation of many process operations involving dry particles and powders.
Follow this guidance to understand the impact of these key characteristics

Equipment and Services

23 Focus on Maintenance-Related Products
Handheld device speeds maintenance, startup efforts; This vibration sensor
provides realtime data; Air bearings enable smooth nanopositioning; Non-
55 contact gas bearing improves rotor balancing; Wireless device supports
predictive maintenance; and more
25 New Products
The launch of a new metering system; Explosion-proof blenders for large-batch
processes; This compact mining crusher handles 3,000 ton/h; Controlled sifting
of bulk materials; Hastelloy drums are designed for hygienic applications; NIR
technology enables precise sorting in fractions of a second; and more
23

Departments
5 Editors Page Tomorrows workforce
As disruptive technologies fuel the digital transformation, needed job skills are
being redefined and are changing quickly
64 Economic Indicators
25

Advertisers
57 Hot Products
60 Product Showcase
61 Classified
62 Reader Service
63 Ad Index

Chemical Connections
Follow @ChemEngMag on Twitter
Join the Chemical Engineering Magazine
LinkedIn Group
Visit us on www.chemengonline.com for Latest News,
Webinars, Test your Knowledge Quizzes, Bookshelf
and more

Coming in December
Look for: Feature Reports on Cost Engineering; and Retrofits & Revamps;
A Focus on Packaging and Transporting; A Facts at your Fingertips
on Distillation; News Articles on CPI Workforce; and Simulation & Modeling
Software; New Products; and much more
Cover design: Rob Hudgins

2 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017

 The perfect formula
for your process automation.

Accuracy for pure chemical product quality with

future-oriented ow measurement
In chemical industry requirements regarding safety, legal standards, e ciency, and quality
are continuously increasing. And emerging opportunities for digital interconnectivity through
Industry 4.0 are gaining signicance within process automation. Our Proline 300 and
Proline 500 o er added value throughout the entire life cycle of your plant.

Seamless integration in existing systems thanks to a unique range of signal outputs:

Heartbeat Technology
Audited and attested reliable
self-monitoring for all new
Proline owmeters
HART, PROFIBUS PA/DP, FOUNDATION Fieldbus, Modbus RS485, EtherNet/IP and
PROFINET
Multifunctional transmitters combinable with all tried-and-tested Promass and Promag
sensors
Comprehensive diagnostic and verication functions with Heartbeat Technology
maximizes your plant safety and availability
www.endress.com/chemical-process

Endress+Hauser AG Phone +41 61 715 7700

Kgenstrasse 2 Fax +41 61 715 2888
4153 Reinach info@endress.com
Switzerland www.endress.com
For details visit adlinks.chemengonline.com/66434-10
For details visit adlinks.chemengonline.com/66434-16
 Editor s Page
EDITORS ART & DESIGN
Tomorrows workforce
DOROTHY LOZOWSKI ROB HUDGINS

T
Editorial Director Graphic Designer he technological advances that we witness in our everyday lives
rhudgins@accessintel.com
dlozowski@chemengonline.com are quite astounding. What were once fantasies in science fic-
GERALD ONDREY (FRANKFURT) PRODUCTION tion have become reality. Smart devices that are now afford-
Senior Editor
gondrey@chemengonline.com SOPHIE CHAN-WOOD able to many, can talk to us, answer our questions, vacuum our
Production Manager
schanwood@accessintel.com floors and do much more. And, robotics, artificial intelligence, additive
SCOTT JENKINS
Senior Editor INFORMATION manufacturing and other technologies have capabilities far more ad-
sjenkins@chemengonline.com SERVICES vanced than the simple assembly-line tasks of early robots. While we
MARY PAGE BAILEY CHARLES SANDS marvel at the thought of self-driving cars and advances yet to come,
Associate Editor Director of Digital Development
mbailey@chemengonline.com csands@accessintel.com many are also concerned that the fast-moving world of automation is a
GROUP PUBLISHER CONTRIBUTING EDITORS
threat to our jobs: Are robots taking over the workplace?
SUZANNE A. SHELLEY
According to a report by the World Economic Forum (WEF)1, the
MATTHEW GRANT
mattg@powermag.com sshelley@chemengonline.com fourth industrial revolution is causing not just a disruption to business
AUDIENCE CHARLES BUTCHER (U.K.) models, but also to the labor markets with enormous change pre-
cbutcher@chemengonline.com
DEVELOPMENT dicted in the skill sets needed to thrive in the new landscape. Cur-
SARAH GARWOOD
Audience Marketing Director
PAUL S. GRAD (AUSTRALIA) rent trends could lead to a net loss of over 5 million jobs globally (in
pgrad@chemengonline.com
sgarwood@accessintel.com the countries covered by the report) in 2015 to 2020, says the report.
JESSICA GRIER
TETSUO SATOH (JAPAN)
tsatoh@chemengonline.com
Most of the job losses are expected to be in office and administrative
Senior Marketing Manager
jgrier@accessintel.com
functions; while gains are expected in computer, mathematical and en-
JOY LEPREE (NEW JERSEY) gineering fields. There are numerous reports by various groups that ad-
jlepree@chemengonline.com
GEORGE SEVERINE
Fulfillment Manager dress potential job losses due to automation. While the predictions vary,
gseverine@accessintel.com one thing that seems sure is that skill requirements are changing rapidly.
DANIELLE ZABORSKI
List Sales: Merit Direct, (914) 368-1090
dzaborski@meritdirect.com
The digital worker
Many experts are focusing on the human side of the technological ad-
EDITORIAL ADVISORY BOARD vances. At the recent Emerson Global Users Exchange (Minneapolis,
JOHN CARSON JOHN HOLLMANN Minn.; October 26), much attention was given to the digital worker.
Jenike & Johanson, Inc. Validation Estimating LLC
In his opening comments, Mike Train, executive president, Emerson
DAVID DICKEY
MixTech, Inc.
HENRY KISTER
Fluor Corp.
Automation Solutions, discussed how the era of increasing efficiency
by cutting costs has come to an end, because productivity through ef-
HEADQUARTERS ficiency has been maximized, and has left workforces stretched. Auto-
40 Wall Street, 50th floor, New York, NY 10005, U.S.
Tel: 212-621-4900
mation is now the driver for productivity, and changes in the workforce
Fax: 212-621-4694 are needed. Train says, The pressure is on industry leaders to take the
EUROPEAN EDITORIAL OFFICES next step to the game-changing performance made possible by digi-
Zeilweg 44, D-60439 Frankfurt am Main, Germany
Tel: 49-69-9573-8296 tally empowering the workforce. The message is that automation is not
Fax: 49-69-5700-2484
about eliminating jobs, but it is changing jobs. Emerson has identified
CIRCULATION REQUESTS: five competencies as critical for succeeding with digital transformation:
Tel: 847-564-9290
Fax: 847-564-9453 automated workflow (leaving people to handle only the exceptions and
Fullfillment Manager; P.O. Box 3588,
Northbrook, IL 60065-3588 not routine jobs); decision support (using data analytics combined with
email: chemeng@omeda.com
expertise); workforce upskilling; mobility; and change management.
ADVERTISING REQUESTS: SEE P. 62
For reprints, licensing and permissions: Wright's Media, 1-877-652-5295,
sales@wrightsmedia.com Moving forward
The need for new skills is evolving rapidly, as jobs change and new
ACCESS INTELLIGENCE, LLC jobs emerge with digitalization. With this pace of change, immedi-
DON PAZOUR
Chief Executive Officer
JONATHAN RAY
Vice President, Digital
ate focus needs to be given to training workers. In the WEF report,
survey respondents cited future workforce planning and change man-
HEATHER FARLEY MICHAEL KRAUS
Chief Operating Officer Vice President, agement as high priorities. The report recommends actions for the
Production, Digital Media & Design
immediate term, including: making use of data analytics, employing
JAMES OGLE
Executive Vice President STEVE BARBER the benefits of a diverse workforce and leveraging
& Chief Financial Officer Vice President,
Financial Planning and Internal Audit flexible working arrangements. Longer term recom-
MACY L. FECTO
Exec. Vice President, GERALD STASKO
mendations include rethinking education systems,
Human Resources & Administration Vice President/Corporate Controller incentivizing lifelong learning, and cross-industry
JENNIFER SCHWARTZ and public-private collaboration.
Senior Vice President & Group Publisher
Aerospace, Energy, Healthcare Now, more than ever, we as employees need to
pay attention to keeping pace with the changing
ROB PACIOREK
Senior Vice President,
9211 Corporate Blvd., 4th Floor
Rockville, MD 20850-3240
needs of our workplaces.
Chief Information Officer www.accessintel.com
Dorothy Lozowski, Editorial Director
1.The Future of Jobs, January 2016; www.weforum.org/reports/the-
future-of-jobs; accessed October 17, 2017
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 5
For details visit adlinks.chemengonline.com/66434-20
Chementator
A new C2-based production route to MMA
C
hemists and Proven technology
engineers
from the Per- Ethylene
(C2H4)
formance
Materials Segment Synthesis gas
of Evonik Industries (CO/H2)
AG (Essen, Germany;
w w w. e v o n i k . c o m ) Natural gas
have developed a new Air
process for making (O2)
methyl methacrylate
(MMA). With a yield Methanol
(CH3OH)
of over 90%, the so-
called Leading in Methacrylates (LiMA) pro-
cess can be considered the most efficient
MMA production process, says Steffen
Krill, head of Innovation Management in the
Methacrylates Business Line.
Today, MMA production is dominated by
routes that start with acetone (C3) or
mainly in Asia isobutene (C4), with only
10% of global production based on ethylene
(C2). The C2 Alpha route that was first devel-
oped by Lucite International UK Ltd. (Wilton,
U.K.; www.luciteinternational.com), which is
now part of Mitsubishi Chemical Corp., was
the winner of the 2009 Kirkpatrick Chemical
Engineering Achievement Award (see Chem.
Eng., December 2009, pp. 1721).
Similar to the C2 Alpha process, the LiMA
process (diagram) uses ethylene, synthesis
gas (syngas) and methanol as feedstocks,
explains Krill. In the first step, ethylene and
syngas are hydroformylated into propional-
dehyde. In the next step, propionaldehyde
and formalin undergo a Mannich condensa-
tion to form methacrolein. This intermedi-
ate is then directly esterified by methanol in
a highly selective, single-step process into
MMA. The high yield (over 90%) is due to
Deep-learning-based AI quickly predicts furnace products
N
TT Communications Corp.
(NTT Com; www.ntt.com)
and Mitsui Chemicals Inc.
(both Tokyo, Japan; www.
mitsuichem.com) have demonstrated
the ability to predict, with a high pre-
cision, the concentration of gaseous
products generated in a furnace. The
predictions are produced in just 20
minutes after sampling process data,
by modeling the relationships be-
tween process data and raw material,
and furnace conditions, using deep-
learning-based artificial intelligence
(AI) developed by NTT Com. Over
50 process parameters are used in
the modeling, including temperatures
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
Edited by:
Evoniks development
Gerald Ondrey
Methacrolein
TRASH BAGS
Propionaldehyde Barrier films used in food
(C3H6O) Direct
packaging are difficult to
Oxidative
Esterification recycle effectively, because
(DOE) they often contain multiple
Formalin polymers that are not com-
(CH2O) patible with one another in
MMA the mixing steps required
for the recycling process.
Now, trash bags made
the new patent-pending process setup in from recycled packaging
film scraps have been de-
combination with a unique catalyst, which
veloped through a multi-
enables the reaction to take place in liquid company collaboration,
phase at temperatures below 100C. The and were recently used in a
lower temperature also increases the lifetime shoreline cleanup program
of the catalyst, which normally has to be re- to remove marine debris.
placed yearly in gas-phase routes operating The collaboration involves
at temperatures of 350C, says Krill. the Dow Chemical Co. (Mid-
In fact, all reaction steps of the LiMA land, Mich.; www.dow.com),
process take place in the liquid phase at packaging maker Bemis Co.
temperatures far below that required by Inc. (Neenah, Wis.; www.
bemis.com) and plastics
gas-phase routes, says Krill. As a result,
company Polykar (Saint-
CO2-equivalent per ton of MMA produced Laurent, Que.; www.polykar.
is reduced by up to 3040%. Also, the raw com). Bemis collected and
materials and reaction products serve as delivered post-industrial
the primary solvents themselves, thereby scrap material from a pro-
eliminating the need for dilutions or solvents. cess that produces a food-
As a result, LiMA generates one-eighth to packaging film made from
one-tenth the intermediary water streams polyethylene (PE) and eth-
compared to C3 and C4 routes. The milder ylene vinyl alcohol (EVOH).
reaction conditions and absence of corro- Polykar utilized the packag-
ing scrap as a raw material
sive media are also expected to significantly
for making the trash bags. A
reduce maintenance requirements, while al- Dow technology chemical
lowing for less expensive materials of con- additives known as Retain
struction, he adds. allows the PE-EVOH films to
The LiMA process has operated for over
8,000 hours in a pilot plant in Darmstadt. (Continues on p. 8)
and flowrates of raw materials and of the Ministry of Economy, Trade and
furnace-reactor parameters. The two Industry (METI), NTT Com, Yokogawa
companies have been working to- Electric Corp. and Yokogawa Solution
gether since 2015. Mitsui Chemicals Service Corp. have started demon-
plans to enhance the reliability and stration testing of a high-level Energy
efficiency of its production facilities Management System (EMS), which
by studying next-generation produc- aims to optimize production facilities
tion technologies using the internet of in the chemical and pulp-and-paper
things (IoT), big data and AI. industries. NTT Com will develop the
Meanwhile, NTT Com plans to use analysis support system that handles
AI-based technology to enhance the process data using an IoT/AI deep-
efficiency of chemical plant opera- learning system. Yokogawa will de-
tions, by quickly clarifying the causes velop ways to optimize the inter-pro-
of quality abnormalities. In a project duction process, using plant big data.
supported by the New Energy and In- Yokogawa Solutions will develop highly
dustrial Technology Development Or- sophisticated production-control tech-
ganization (NEDO) under the authority nology for mass-production factories.
NOVEMBER 2017 7
 be fed directly into Polykars Lower costs for converting alkylation units from
recycling and plastic extru- hydrofluoric to sulfuric acid
sion lines.
Dow initially developed

the Retain technology as a
proprietary polymer modifier
added to PE-EVOH barrier
films to make them easier
to recycle (Chem. Eng.,
August 2016, p. 7). In the
current process, Retain is
added to the recycled scrap
material in a process step
that allows the two polymers
to mix well, and allows the
trash bag products to have
the necessary strength and
toughness properties, ex-
plains Jeff Wooster, director
of global sustainability for
Dow Packaging and Spe-
cialty Plastics.
The key to making the
process work is the specific
chemical design of the com-
patibilizers, which facilitate
the dispersion of EVOH into
the PE during the recycling
process, Wooster says.
The trash bags made
for this shoreline cleanup
represent a demonstration
project that the companies
hope will lead to more com-
mercial-scale uses.
ORGANIC PV FILM
Lechwerke AG (LEW;
Augsburg, Germany; www.
lew.de) has extended its
Energy Faade project
by integrating HeliaFilm, a
solar film made by Heliatek
GmbH (Dresden, Germany;
www.heliatek.com). Over
the next few years, the re-
sulting test platform will be
(Continues on p. 10)
F
or petroleum refin- HF alkylation
DuPont
eries, the cost of
converting hydro- 100% of isobutane recycle
fluoric-acid-based
alkylation units to the rela-
Olefins Feed Product Propane
tively safer sulfuric-acid- pre-treatment Reaction Fractionation post-treatment
Isobutane Butane
based alkylation process
(diagram) has been cost-
ASO
prohibitive and has lacked extraction Alkylate
specific economic ben-
efits. Now, DuPont (Wilm-
ington, Del.; www.du- Sulfuric acid alkylation
pont.com) has developed
a low-cost approach to ~50% of isobutane recycle
converting existing HF
alkylation units to use Olefins Feed Dry alumina Butane
Reaction Fractionation
sulfuric acid that simulta- Isobutane preparation adsorption Alkylate
neously allows an expan-
sion of production capac-
ity. Known as the ConvEx Refrigeration Propane
technology, the suite of
DuPont conversion ca- ~50% of isobutane recycle
pabilities takes advantage
of existing equipment to the conversion protocol, ConvEx technology
keep the capital expense low, says Shane enables refiners to gain significantly more al-
Presley, technical service and development kylation capacity.
manager for DuPont Clean Technologies. HF alky units are typically run at tempera-
Changes to the reaction stage can take tures of 100F, while sulfuric acid units are
two forms. One option involves the installa- typically designed to run at 45F, Presley
tion of the DuPont Stratco Contactor reac- explains, so the addition of a new refrigera-
tor for sulfuric acid alkylation. This allows the tion section for the H2SO4 alkylation process
highest product quality, but involves more is required, but the ability to recycle some
capital expense. Another option involves ret- isobutane from the refrigeration section frees
rofitting existing reactors. up space in the fractionation stage. This al-
The DuPont ConvEx technology becomes lows refiners to generate an additional 100%
particularly attractive economically when or more alkylate when converting from HF to
additional capacity is desired. The differ- sulfuric using ConvEx, Presley notes.
ences in how isobutane is recycled in HF DuPont currently runs a pilot facility to
compared to H2SO4 alkylation units is the show the capacity expansion capabilities of
key to the expansion opportunity provided the ConvEx process and is looking for op-
by the ConvEx technology (see diagram). portunities for conversion of commercial-
By taking advantage of these differences in scale operations.

Molecular pulleys make a better battery anode

S
ilicon anodes are an attractive
alternative to graphite anodes
currently in use in lithium-ion
batteries, because they can
deliver up to five times higher capaci-
ties. However, silicon anodes have a
limited charge-discharge cycle num-
ber. Their volume expands during
each cycle, leading to fracture of the
electrode particles or delamination of
the electrode, reducing its capacity.
Now a team from Korea Advanced
Institute of Science and Technology
8 CHEMICAL ENGINEERING
(KAIST, Daejeon; www.kaist.edu), led
by professors Jang Wook Choi and
Ali Coskun, has reported a molecular
pulley binder for high-capacity silicon
anodes of lithium-ion batteries.
The team integrated molecular pul-
leys, called polyrotaxanes, into a bat-
tery electrode binder. A polyrotaxane
is a molecule consisting of strings
and rings, in which rings are threaded
onto a molecular axle and prevented
from dethreading by two bulky end
groups. Polyrotaxanes can help build
WWW.CHEMENGONLINE.COM
functional molecular machines.
The team included the polyrotax-
anes in battery electrodes to attach
the electrodes onto metallic sub-
strates. The free-moving rings can
follow the volume changes of the sili-
con particles. The rings sliding mo-
tion can hold silicon particles without
disintegration during their continuous
volume change. Previous binders al-
lowed particles to scatter, and the
silicon electrodes thus degraded and
lost their capacity.
NOVEMBER 2017
 Join the ultra-high
shear revolution.
When Ross introduced the first Ultra-High Shear Mixer,
we revolutionized high speed, high shear mixing. Operating
with tip speeds up to six times higher than conventional
rotor/stator mixers, these mixers can produce
sub-micron emulsions and dispersions faster than
any conventional rotor/stator design.

Today, in applications from foods to pharmaceuticals,

coatings and adhesives, the results include smaller particle
sizes, tighter particle size distributions, greater
throughput and superior end-products.

Patent No. 5,632,596: X-Series

Patent No. 6,241,472: MegaShear
Christine Banaszek Patent No. 6,000,840: PreMax
Applications Engineer
Employee Owner

A B

C D

Ross Ultra-High Shear Mixers produce

ultra-fine emulsions and dispersions in inline
(A-C) and batch (D) applications. Many models
also allow you to fine-tune shear to mix
shear-sensitive materials safely.
Scan to learn more.
See the newest generation of
rotor/stator mixing technology.
Visit highshearmixers.com/ultra
Or call 1-800-243-ROSS
Try our Knowledge Base & Product
Selector web app: mixers.com/web-app

For details visit adlinks.chemengonline.com/66434-05

 used to measure the output of the
organic photovoltaic (PV) films in a
direct comparison to conventional
solar technology. The building has
now been upgraded both ener-
getically and visually by this BiOPV
(Building Integrated Organic Photo-
Voltaics) solution.
As part of the Energy Faade
project, which was launched three
years ago, two areas of Lechwerkes
southern faade have now been
equipped with SVK fiber-cement el-
ements covered by HeliaFilm. A total
area of 56 m with an installed capac-
ity of 2.43 kWp is expected to deliver
an estimated 2,000 kWh/yr.
The solar film HeliaFilm, developed
and produced by Heliatek, are inte-
grated directly into the building mate-
rial at the factory of faade element
producer SVK (Sint-Niklaas, Bel-
gium; www.svk.be). They are then
simply connected at the construc-
tion site. The low weight of the films
(1 kg/m2) allows for an easy and low-
cost integration on both new and
existing faades. HeliaFilm is said to
reduce a buildings carbon footprint
by 20 g of CO2 per generated kWh.
CARBON-NEGATIVE PLANT
Climeworks (Hinwill/Zurich, Swit-
zerland; www.climeworks.com) has
partnered with Reykjavik Energy
(Iceland; www.or.is) to combine di-
rect air capture (DAC) technology for
the worlds first time with safe and
permanent geological storage of
CO2. As part of the CarbFix2 project,
Climeworks will demonstrate a safe,
economically viable and highly scal-
able carbon removal technology. This
type of solution has been recognized
as a crucial component in efforts to
achieve global warming targets.
The E.U.-backed collaborative re-
search project centers around one
of the worlds largest geothermal
power plants in Hellisheidi, Iceland,
where CO2 is currently injected and
mineralized at an industrial scale. A
Climeworks DAC module has been
installed on-site to capture CO2 from
ambient air for permanent storage
underground, thus creating a car-
bon-removal solution.
A testing phase has started, dur-
ing which the CO2 is captured from
ambient air, bound to water, and
sent more than 700 m underground.
There, the CO2 reacts with the basal-
tic bedrock and forms solid minerals,
creating a permanent storage solu-
tion. Climeworks technology draws
in ambient air and captures the CO2
with a patented filter. The filter is then
(Continues on p. 11)
10
Extremophilic microbes enable new
methane pathways . . .
M
icrobes inhabiting the ex-
treme environments thou-
sands of feet below the
earths surface possess
unique properties not encountered
elsewhere. A research consortium of
South Dakota School of Mines and
Technology (SDSMT; Rapid City; www.
sdsmt.edu), University of Oklahoma
(Norman) and Montana State Univer-
sity (Bozeman) is investigating these
novel microorganisms and their meth-
ane-oxidation behavior. The goal of the
project is to manipulate the microbes to
enhance their methane-uptake capa-
bilities in order to produce value-added
products, such as methanol and bio-
polymers like polyhydroxyalkanoates
(PHA), as well as bioelectricity. These
extreme-environment microorganisms
exhibit much higher rates of methane
oxidation than their counterparts from
more traditional locations, says Rajesh
Sani, SDSMT professor and lead re-
searcher of the consortium.
We have isolated several organisms
from deep in the biosphere that were
oxidizing methane underground. It was
not previously known that they could
do this, he explains. This is the first-
. . . and these make a meal of
methane/hydrogen mixtures
S
oil bacteria that oxidize methane
(methanotrophs) are important
in capturing methane before it
enters the atmosphere. Now
an international team has isolated and
characterized methanotrophic bacteria
obtained from a New Zealand volca-
nic field that can grow on CH4 or H2
separately, but perform best when both
gases are present. The team obtained
Methylacidiphilum sp.RTK17.1 bacteria
from an acidic geothermal field in Roto-
kawa, New Zealand. The bacteria can
rapidly oxidize CH4 and H2 simultane-
ously. Biochemical assays revealed that
the bacteria use hydrogen as an elec-
tron donor for aerobic respiration and
carbon fixation.
The team included staff from GNS
Science (Taupo, New Zealand), Scion
(Rotorua, New Zealand), University
of Otago (Dunedin, New Zealand),
University of Manitoba (Winnipeg,
Canada), Montana State University
(Bozeman), CSIRO (Australian Capital
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
ever research project to investigate
such microoganisms and their meth-
ods for methane regulation in extreme
environments. Sani and his team are fo-
cused on genome editing the microbes
so they can more effectively convert
methane into valuable products. A
great deal of gene editing must be
done to modify the genes to produce
polymers, Sani says. The genes can
be engineered to create biopolymers
with various properties from methane.
Future work will include manipulating
the microbes to create additional prod-
ucts from CH4 gas. The consortium is
also collecting samples from deep bio-
sphere locations in different regions
of North America to compare the
species diversity.
I believe we will end up with a few
different technologies, says Sani of
the potential to commercial these new
methane-based processes. We have
a technology that can take advantage
of inexpensive, abundant methane,
and convert it into liquid fuels or bio-
polymers, he continues. LanzaTech
(Skokie, Ill.; www.lanzatech.com) has
signed on as an industrial partner for
this project.
Territory), and Monash University (Clay-
ton, Australia; www.monash.edu). A
member of the team, Monash Univer-
sitys Chris Greening, says: This study
is significant because it shows that key
consumers of methane emissions are
also able to grow on inorganic com-
pounds such as hydrogen. This new
knowledge helps us reduce emissions
of greenhouse gases.
The team focused on the meta-
bolic strategies used by bacteria
to survive and thrive in challenging
environments. Methane is a chal-
lenging energy source to assimilate,
and by being able to use hydrogen
as well, the bacteria can thrive when
methane and oxygen are no longer
available. Many industrial processes
release large amounts of CH4, CO2,
and H2 into the atmosphere. By
using these gas-guzzling bacteria,
it is possible to convert these gases
into useful liquid fuels and feeds in-
stead, Greening says.
NOVEMBER 2017
New antimicrobial compounds offer heated with low-grade heat from
the geothermal plant to release
disinfectant alternatives the pure CO2, which then can be
Conjugated backbone stored underground.

A
newly pat-
Charged moiety Earlier this year, the company
ented class of started up the world's first com-
synthetic anti- mercially viable DAC plant near
microbial com- Ar Ar Ar Ar Conjugated
n backbone Zurich, which filters 900 tons of
pounds is aimed at CO2 from the atmosphere and
overcoming the limita- Conjugated backbone supplies it to a local greenhouse
tions of existing indus- Biosafe Defenses (Chem. Eng. July 2017, p. 7).
trial disinfectants, such
as quaternary ammonium compounds developed from research at the Univer- NEW FLAME RETARDANT
and bleaches. Bleaches are effective sity of New Mexico (Albuquerque; www. Chemists from the Swiss Federal
disinfectants on initial application, but umn.edu) and the University of Florida Laboratories for Materials Science
they dont work when they dry and (Gainesville; www.ufl.edu). and Technology (Empa; (Dben-
can degrade surfaces, explains Harry Among the advantages of this class of dorf; www.empa.ch) have devel-
Pappas, CEO of Biosafe Defenses compounds is that they fluoresce under oped and patented an environmen-
tally friendly way to produce flame
LLC (Albuquerque, N.M.; www.bio- certain wavelengths, making it possible
retardants for polyurethane (PU)
safedefenses.com), the developer of to determine where and when to apply foams. Unlike previous retardants
the new antimicrobials. Further, qua- the antimicrobials. Also, the compounds made of chemicals containing chlo-
ternary ammonium compounds can charged groups greatly increase their rine, the new material is non-toxic.
have safety concerns and cannot make solubility in aqueous solutions, allowing Empas new retardant EDA-
claims to kill certain important bacterial a water-soluble agent that generates DOPO, a derivative of the familiar
species, such as Clostridium difficile. ROS and can persist on surfaces. Finally, flame retardant DOPO (9,10-di-
The companys antimicrobials are the new compounds can be utilized in a hydro-10-oxa-phosphaphen-
p-phenylene ethynylyene polyelectro- variety of ways, including in liquid soap anthreneoxide) is now going
lytes, characterized by a conjugated solutions, impregnated into fabrics, such into serial production. Metady-
nea Austria GmbH (Krems an der
backbone that is tuned to absorb light as antimicrobial wipes, and incorporated
Donau; www.metadynea.com)
at specific wavelengths (examples are into plastic and glass surfaces. will manufacture the material and,
shown in the diagram). Our library of Biosafe Defenses is now offering if there is sufficient demand, the
compounds is characterized by cat- partnerships to manufacture the com- global FoamPartner Group (www.
ionic or anionic charge groups and pi- pounds at kilogram scales (they are now foampartner.com) will use it to pro-
conjugated backbones that react with made on the scale of several grams), duce flame-retardant PU foams for
photons to generate reactive oxygen and is looking for licensing opportuni- upholstery and mattresses. Since
species (ROS), Pappas says. The ROS ties. Its lead product has been success- the new method of production of
break microbial cell walls and denature fully tested for toxicity on epithelial and DOPO derivatives was patented
proteins and DNA, effectively killing the endothelial cells, and on hairless mice. in June 2017, Metadynea Austria
has already produced around 1.5
organisms, whether bacteria, virus, fungi It is being targeted for use at hospitals
or yeast. The compounds were originally and food service facilities. tons of the flame retardant.

Multilayer membrane for climate control

A
triple-layer, porous membrane
system developed at the
Functional Materials Labora-
tory at Eidgenssische Tech-
nische Hochschule Zrich (www.fml.
ethz.ch) can be fashioned into evapo-
rative curtains to cool and humidify
indoor spaces, potentially decreasing
the energy demand for climate-control
systems. Juxtaposing opposite forces
in this case, layering a hydrophilic
membrane layer between two hydro-
phobic outer layers allows a water
film to remain stabilized between the
dry outer layers. This open, porous
system lets the water film evaporate
outward on both sides of the materi-
als. At the same time, the inner po-
rous system is able to refill itself from a
water reservoir, explains Mario Stucki,
the lead developer of this technology.
The immense heat of evaporation
of water cools the membranes sur-
roundings, he continues.
The triple-layer membrane materi-
als are assembled via the template
removal method, in which hard tem-
plate particles made from soluble
salts are dispersed as templates in
dissolved polymer solutions. When
the solution is spread, and the solvent
is removed, a solid, multiphase layer
is produced. This base layer is then
coated with an additional layer of liq-
uid dispersion, resulting in the forma-
tion of multilayer complexes. Accord-
ing to Stucki, template removal is the
only membrane production method
that allows for straightforward mul-
tilayer laminate assembly, as other
methods would require the applica-
tion of adhesives between the layers.
Another benefit of these membranes
is that the pore size is extremely
small, which enables water to be ef-
fectively contained within the layers.
At larger pore sizes, the top and bot-
tom layer would leak the water and
possibly lead to much faster fouling,
he adds. Stucki and his team have
demonstrated this passive cooling
process with membrane samples
10 10 cm2 in size. The template-
removal method has previously been
demonstrated on industrial-scale
coating and drying machines, says
Stucki, so scaling up this technology
for mass production is certainly fea-
sible. (For more on membranes, see
pp. 1417.) n

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 11

 Business News
LINEUP Plant Watch 2018. ENB is used primarily in the production
Inovyn starts up KOH of ethylene-propylene-diene rubber (EPDM).
AKZONOBEL
plant in Belgium
BASF October 13, 2017 Inovyn (London, U.K.; Wacker to expand production facilities for
www.inovyn.com) announced the completion of dispersions and powders in South Korea
CALGON CARBON
its new potassium hydroxide (KOH) production September 28, 2017 Wacker Chemie AG
CARGILL facility at its Antwerp/Lillo site in Belgium. (Munich, Germany; www.wacker.com) is investing
The new plant uses membrane technology 60 million to expand its production plants for
ECOLAB
to produce 155,000 metric tons per year polymer binders in Ulsan, South Korea. The
GEORGIA-PACIFIC (m.t./yr) of KOH with 100,000 m.t./yr of chlorine. company plans to build a new spray dryer for
dispersible polymer powders, which will have
INDORAMA
AkzoNobel doubling capacity at a total capacity of 80,000 m.t./yr. Wacker
INOVYN organic peroxides plant in Ningbo also plans to build a new reactor, which will
JACOBS October 12, 2017 AkzoNobels (Amsterdam, more than double the Ulsan plants dispersion
the Netherlands; www.akzonobel.com) capacity for vinyl acetate ethylene copolymer.
KEMIRA Specialty Chemicals business has entered
KURARAY the next phase of a major expansion at its Cargill to build biodiesel
organic peroxides facility in Ningbo, China, plant in Wichita
MITSUI CHEMICALS
which produces dicumyl peroxide (DCP). September 26, 2017 Cargill, Inc. (Minneapolis,
NESTE Capacity at the site was boosted by 40% in Minn.; www.cargill.com) plans to build a
August, and is set to double to a capacity of $90-million biodiesel plant in Wichita, Kan.
SHELL
38,000 m.t./yr by the third quarter of 2018. Set to open January 2019, the new plant will
SOLVAY produce 60 million gal/yr of biodiesel. The
Songwon commissions second plant will be located next to Cargills oilseed
SONGWON
thermoplastic urethanes production line processing plant and replaces an oil refinery
STATOIL October 9, 2017 Songwon Industrial Ltd. managed by Cargills Global Edible Oil business.
SYNTHOMER (Ulsan, South Korea; www.songwon.com)
has commissioned a second thermoplastic Mergers & Acquisitions
TOTAL urethane (TPU) production line at its plant in BASF to acquire selected
WACKER Suwon, South Korea. The new production herbicide assets from Bayer
line will increase TPU capacity from 7,000 to October 13, 2017 BASF SE (Ludwigshafen,
12,000 m.t./yr. Germany; www.basf.com) has signed an
agreement to acquire significant parts of
Solvay to expand production of sulfone Bayer AGs (Leverkusen, Germany; www.
polymers in India and the U.S. bayer.com) seed and non-selective herbicide
October 6, 2017 Solvay S.A. (Brussels businesses for a purchase price of 5.9 billion.
Belgium; www.solvay.com) is expanding its The assets to be acquired include Bayers
global production capacity for sulfone polymers global glufosinate-ammonium non-selective
in India and the U.S. Solvay is constructing a new herbicide business.
production unit dedicated to polyethersulfone
in Panoli, India. Capacity increases are also Indorama will acquire
occurring at Solvays units in Marietta, Ohio DuPont Teijin Films
and Augusta, Georgia. October 10, 2017 Indorama Ventures Public
Ltd. (IVL; Bangkok, Thailand; www.indorama.
Mitsui Chemicals starts production at net) agreed to acquire DuPont Teijin Films (DTF),
expanded thermoplastic elastomers plant a producer of biaxially oriented polyethylene
October 5, 2017 Mitsui Chemicals, Inc. terephthalate and polyethylene naphthalate
(Tokyo; www.mitsuichem.com) commenced films with total film and polymer capacity of
operations on a one-line production augmentation 277,000 m.t./yr. The DTF acquisition includes
for thermoplastic olefinic elastomers at its eight production assets in the U.S., Europe
wholly owned subsidiary Sun Alloys Co. This and China.
expansion will increase the companys annual
production capacity for these products from Statoil, Shell and Total enter
20,000 to 25,000 m.t./yr. CO2 storage partnership
October 2, 2017 Statoil (Trondheim, Norway;
Ineos to increase production www.statoil.com), Royal Dutch Shell (The
capacity for ethylidene norbornene Hague, the Netherlands; www.shell.com)
October 3, 2017 Ineos (London; www. and Total S.A. (Paris; www.total.com) have
ineos.com) plans to expand its ethylidene signed a partnership agreement to develop
Look for more norbornene (ENB) plant in Antwerp, increasing full-scale carbon capture and storage (CCS)
latest news on capacity by 7,500 m.t./yr to 35,500 m.t./yr. in Norway. The first phase of this project could
chemengonline.com The capacity will be available by the end of reach a CO2 storage capacity of approximately
12 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
1.5 million m.t./yr. The project will also be designed to
accommodate future additional CO2 volumes.

Neste to take full ownership of

Neste Jacobs joint venture
September 29, 2017 Neste Corp. (Espoo, Finland;
www.neste.com) and Jacobs Engineering Group (Dallas,
Tex.; www.jacobs.com) have agreed that Neste will acquire
Jacobs 40% shareholding in the Neste Jacobs Oy joint
venture (JV). After this transaction, Neste will hold all
shares in Neste Jacobs.

Ecolab to acquire Georgia-Pacifics

paper chemicals business
September 29, 2017 Ecolab Inc. (St. Paul, Minn.; www.
ecolab.com) will acquire the paper chemicals business of
Georgia-Pacific (Atlanta, Ga.; www.gp.com). This acquisition
will enhance Ecolabs position in the growing tissue and towel
segment, as well as the packaging and board segments
of the paper industry. The paper chemicals business had
revenues of approximately $43 million in 2016.

Kemira to form new

fatty-acid JV in China
September 29, 2017 Kemira Oyj (Helsinki, Finland; www.
kemira.com) has signed an agreement to form a JV
Kemira TC Wanfeng Chemicals Yanzhou with Shandong YOUR DEMANDING
Tiancheng Wanfeng Chemical Technology Co. The JV will
mainly produce alkyl-ketene-dimer wax and its key raw
ENVIRONMENT.
material, fatty-acid chloride, along with polyaluminum
chloride, which is a water-treatment coagulant. The deal OUR PROVEN
is expected to close in the first half of 2018.
RELIABILITY.
BASF to divest Austrian
dispersions plant to Synthomer For over five decades Pyromation has
September 27, 2017 Synthomer plcs (Essex, U.K.; been a valued partner and trusted
www.synthomer.com) Austrian subsidiary has signed a source for temperature sensors in the
contract to purchase BASFs production site for styrene
butadiene dispersions in Pischelsdorf, Austria, for 30 Chemical Industry. Our comprehensive
million. The transaction requires authorization by the line of RTDs, thermocouples and
relevant merger-control authorities and is expected to thermowell assemblies including
be completed by late January 2018. custom designs meet strict industry
Kuraray to acquire certifications and provide superior
Calgon Carbon for $1.3 billion quality control. Find out more about
September 21, 2017 Calgon Carbon Corp. (Pittsburgh, our service offerings, including special
Pa.; www.calgoncarbon.com) and Kuraray Co., Ltd. (Tokyo, packaging, fast delivery and calibration
Japan; www.kuraray.com) have unanimously approved
a definitive merger agreement under which Kuraray will capabilities via our NVLAP-accredited
acquire Calgon Carbon in a transaction valued in excess metrology laboratory.
of $1.3 billion. The parties are targeting a closing by the
end of December 2017.
GET A QUOTE!
Solvay sells global polyamide pyromation.com/chemical
business to BASF for 1.6 billion
September 21, 2017 BASF and Solvay have signed
260.209.6342
an agreement related to the sale of Solvays integrated
polyamide business to BASF for a purchase price of
1.6 billion. The purchase will strengthen BASFs
polyamide 6,6 value chain through increased
polymerization capacities and the backward integration
into the key raw material adipodinitrile. NEC Rated FM/CSA Approved
Mary Page Bailey
For details visit adlinks.chemengonline.com/66434-21
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
13
 Newsfront
Extending Membranes
Reach Across the CPI
Advances in next-generation materials and assembly techniques have enhanced membranes
effectiveness in numerous applications
IN BRIEF
M
embranes are
OLEFINS SEPARATION one of the primary
technologies used
LITHIUM RECOVERY
for separations.
MEMBRANE While they may be best known
MECHANICAL STABILITY for their use in water-treatment
LOOKING TO WATER
operations, advances in mem-
REUSE
brane technologies have ex-
panded their use into many
areas, including the mining,
oil-and-gas, petroleum-refining
and industrial-gas sectors.
These advances have also al-
lowed for membranes to better address the
myriad challenges faced in water-treatment
facilities. This article examines several new
membrane technologies used across a range
of chemical process industries (CPI) sectors.
Olefins separation
Advances in membrane materials have en-
abled their use in complex separations ap-
plications, including those involving various
industrial gases and olefins. For instance,
with the development of a proprietary, silver-
facilitated membrane, Compact Membrane
Systems (CMS; Newport, Del.; www.com-
pactmembrane.com) aims to provide an ef-
ficient technology for separating olefins from
paraffins. The intent is that these membrane
systems, called Optiperm, can be installed
alongside distillation columns or reactors for
debottlenecking, retrofits and capacity expan-
sions to augment production yield by sepa-
rating and concentrating olefins, and reduce
waste and losses from small offtake streams
or purge gases. The benefit of the technol-
ogy is that it allows customers to capture
value they cant get now from streams they al-
ready have, says Erica Nemser, chief execu-
tive officer at CMS. For instance, by installing
a membrane system in a polypropylene reac-
tor system, excess propylene, which would
otherwise be lost, can be recovered from the
purge gas stream and fed back to the reac-
14 CHEMICAL ENGINEERING
CMS
Olefin
Paraffin
Silver (Ag+) carrier
FIGURE 1. The pres-
ence of silver ions fa-
cilitates the transfer
of olefins across the
membrane
tor, reducing both feedstock costs and waste.
This has significant economic benefits for a
modestly sized system, says Nemser. In Au-
gust 2017, CMS began operating a pilot Opti-
perm system on an overhead stream consist-
ing of propylene and propane at Delaware City
Refining Co., which is the first application of
this type of technology at this scale.
The Optiperm membrane is made from a
custom, amorphous fluoropolymer chain em-
bedded with silver (Figure 1). The silver ac-
tually acts as a facilitating agent to allow the
olefin to cross the polymeric membrane, ex-
plains Bill Charlton, olefin specialist at CMS.
The olefins double bond has an affinity for
the silver, so it latches onto each silver site
sequentially as it crosses the membrane. It
doesnt just work by permeation, it is acceler-
ated by the presence of the silver, he adds.
The Optiperm membrane is set apart from
previous silver-based membranes by its cus-
tom fluoropolymer chemistry, which enables
silver to be embedded directly into the poly-
mer structure prior to casting the membrane.
The polymer structure offers protection of
the silver against deactivation, which would
render it unable to attract olefins. Typically,
silver sites are vulnerable to deactivation by
common species present in petrochemicals
and petroleum-refining processes, such as
sulfur and acetylene. According to Charl-
ton, Optiperms unique chemistry also instills
WWW.CHEMENGONLINE.COM NOVEMBER 2017
several other advantages. We see
significantly higher olefin-permeation
rates than have been seen in the
past, our olefin/paraffin selectivity is
much higher as well, and most impor-
tantly, our longevity is much greater
than has been previously reported,
says Charlton.
Currently, the membranes are most
effective at separations involving two-,
three- and four-carbon molecules,
but CMS believes that they could
also handle C5 separations. Future
work will include investigation of liq-
uid-phase separations for C5 and C6
streams. The current iteration of Op-
tiperm requires that the feed be in the
vapor phase and that systems rela-
tive humidity be maintained at around
85%, so a backend drying step may
be recommended. Also, depending
on system operating conditions, re-
compression may be required.
Another technology aimed at ole-
fins separation introduces new levels
of selectivity by integrating metal-or-
ganic framework (MOF) materials into
membrane complexes. A research
team from Eidgenssische Tech-
nische Hochschule Zrich (www.ethz.
ch) has developed a method to create
MOF composite membranes that are
capable of extremely fine separations.
MOF composite membranes have
been shown to allow efficient sepa-
ration of molecules that vary in size
by only a fraction of one angstrom,
such as propylene and propane, ex-
plains Samuel Hess, lead researcher
on this project. In creating compos-
ite membranes, a key aspect is de-
termining a combination of materials
that will instill mechanical stability
while also remaining cost-effective to
produce at industrial scales. Hess
team developed a polymeric precur-
sor membrane with zinc oxide seed-
nanoparticles present at the pores.
This precursor membrane allows the
growth of pore-directed MOF crys-
tals without requiring any additional
seeding or counter-diffusion steps,
says Hess. This procedure avoids
the formation of rigid MOF crystal
layers and maintains the polymers
intrinsic mechanical flexibility, which
is required for integrating such mem-
branes into industrial spiral-wound
membrane modules.
The team has synthesized these
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
MDS
Heated vat leach
Heated vat leach
Back to feed and acid makeup
Na2C03
Ion exchange
Mixing
Baffled (settling) Filter press
FIGURE 2. Several membrane steps enable the recovery of a concentrated lithium stream
from dilute clay
membranes at laboratory scale, and
recently succeeded in fabricating the
precursor membrane via roll-to-roll
coating. Currently, they are working
to scale up production to develop
industry-scale prototypes containing
several square meters of membrane
material. We are optimistic that the
synthesis protocol is adaptable to
larger membrane areas and that the
process can be implemented to pro-
duce MOF-composite membranes
continuously, says Hess. The next
step for this patent-pending technol-
ogy is commercialization the team
is seeking collaborators to imple-
ment the composite membranes in
industrial operations.
Lithium recovery
Increasing demand for energy-storage
solutions has forced lithium producers
to seek alternative processing tech-
niques, and membranes are prov-
ing to be quite promising in this area.
Neometals Ltd. (West Perth, Australia;
www.neometals.com) has developed
a pair of corresponding technolo-
gies: one that directly extracts LiCl
from brine without evaporation using
adsorption and nanofiltration (NF)
known as the Dexter process; and
one that applies an electrolysis cell
to produce high-purity LiOH (known
as the ELi process). LiOH is a major
NOVEMBER 2017
Solids to heated vat leach
Backwash screen
filter 200 & 100
Supernatant
Clarifier
Fin
Heated vat leach
es
MDS proprietary MDS proprietary MDS proprietary
RO membrane NF membrane UF membrane
Li2CO3
REE, Mg, Ca recovery
Waste solids
precursor material in the production
of lithium-ion batteries. The combina-
tion of these processes would enable
efficient consolidated-site production
of LiOH from lithium brine deposits.
The ELi process also offers an alter-
native to lithium production from hard
rock deposits.
The ELi process electrolysis cell
is based on the chlor-alkali process
with specially adapted membranes
(for more information about chlor-
alkali technology, see The Greening
of Chlor-Alkali Production, Chem.
Eng., October 2017, pp. 1620).
By adapting the chlor-alkali process
with alternative membranes, weve
been able to make LiOH directly from
spodumene concentrate at a very low
cost of production, says Mike Tam-
lin, Neometals chief operating officer.
Since the stream entering the electrol-
ysis cell must be extremely pure, the
company developed an integral puri-
fication process that is capable of re-
moving impurities down to the parts-
per-billion (ppb) level. Neometals also
determined the optimal set of operat-
ing conditions to allow conventional
chlor-alkali equipment to be used for
LiOH production through semi-pilot
testing. By utilizing a chloride-based
environment in the electrolysis, rather
than, for example, inputting lithium
sulfate, higher current efficiency is
15
 Aaron Morelos-Gomez
FIGURE 3. Membranes coated with graphene oxide
have the mechanical stability to withstand high
pressures
possible since a sulfate medium does
not have the ionic mobility of chloride.
We have incentive to create the most
pure solution possible, because the
higher the purity, the higher the cur-
rent efficiency, resulting in a higher-
purity end product, which benefits
the electronics industry, says Tamlin.
Neometals will next pilot the technol-
ogy, and expects to produce LiOH at
commercial scale by 2021 initially via
the conventional process while final
detailed design on ELi is completed,
according to Tamlin.
The company also saw an opportu-
nity to improve upon the environmen-
tal footprint of extracting brine water
in lithium processing. Typical brine
extraction requires removing large
amounts of water from water tables
and evaporating it, which is particu-
larly problematic in water-stressed
communities. As lithium production
increases, we realized that finding
a better way to extract lithium from
brine without extracting the water
from the ground permanently was a
worthwhile goal, says Tamlin. The
companys Dexter direct-extraction
process involves pumping brine from
an aquifer, processing it in an absorp-
tion phase with a proprietary sodium-
titanate nanotube absorbent followed
by very selective NF to produce a con-
centrated LiCl stream. The adsorbent
material has very high surface area
and durability, and is extremely selec-
tive against sodium, which is predom-
inant in the brine, but is a contaminant
to the LiOH production process. The
NF step uses specially developed
membranes to concentrate the lith-
ium and provide purification. The brine
water is pumped back into the aquifer
once lithium is removed. By using
16
relatively standard equipment, and
adapting a new type of membrane to
the process, were able to take lithium
out of a saline solution and create
an upgraded solution without using
reagents, says Tamlin. Eliminating
reagents is particularly important for
operations in remote locations, where
transporting materials over long dis-
tances via trucks could be dangerous
or prohibitively expensive. Also, adds
Tamlin, extracting the brine and re-
injecting it directly after removing the
lithium avoids the generation of the
large salt stockpiles that result from
solar evaporation, which can be an
environmental concern, particularly in
windy climates. The entire lifecycle
of lithium production is enhanced,
he emphasizes.
New membrane technologies from
Membrane Development Special-
ists (MDS; Escondido, Calif.; www.
mdsamericas.com) enable the re-
covery of lithium from two diverse
sources: lithium clay and recycled
batteries. Due to the dilute lithium
concentration of clays, achieving
efficient recovery is quite challeng-
ing. MDS patent-pending process
(Figure 2) involves acid digestion of
clays with proprietary NF, ultrafiltra-
tion (UF) and reverse-osmosis (RO)
membrane processes.
In this process, we are concentrat-
ing lithium as a sulfate. The permeate
will contain 5080% of the acid that
is used, which is recycled back into
the process, explains Larry Lien,
managing director of MDS. The tech-
nology enables the use of lithium de-
posits that previously were viewed as
too dilute for feasible recovery. The
technology has been demonstrated
at bench scale, and MDS is currently
working with stakeholders to develop
it for larger-scale operations. Since
the process is based on established
technologies, and requires no under-
ground mining, Lien is confident in the
scaleup potential. Lien projects that
a 1,000-gal system could produce 5
tons of lithium carbonate per day.
After acidifying the clay, a UF unit
removes the suspended solids.
Next, a specialized NF membrane
removes divalent cations like calcium
and magnesium, and in some cases,
rare-earth elements (REE) that can
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
be concentrated in this step as well.
The resulting permeate is a relatively
pure stream of lithium sulfate, chlo-
ride or nitrate, which is concentrated
with acid. We concentrate the lithium
stream up to 1,000 to 2,000 ppm,
depending on what the osmotic pres-
sure will allow, explains Lien. We can
recover up to 96% of the lithium that
is leached out of clays, so it is a pretty
attractive solution, he adds.
End-of-life batteries are another po-
tential source of lithium. Since the lith-
ium used in batteries is already quite
pure, the process is somewhat sim-
pler than recovering lithium from other
sources, and MDS has already com-
mercialized an analogous process for
lead-acid batteries. For lithium recov-
ery, batteries are first acid-digested,
and the carbon and suspended solids
are removed using a specialized hol-
low-fiber UF membrane. Then, sub-
sequent NF and RO steps concen-
trate and separate lithium from cobalt
and other components, while 75%
of the acid and 90% of the water are
recycled for reuse. You end up with
a highly concentrated lithium sulfate
or chloride solution that can be pre-
cipitated out, says Lien. The process
can be configured as a permanent,
fixed installation, or as a mobile, fully
contained skid.
According to Lien, the challenge lies
not in the extraction or purity of the
lithium, but in the logistics of collect-
ing a sufficient number of batteries to
make the process economically sus-
tainable. Here, the infrastructure for
efficient, large-scale recycling is critical
to the projects feasibility. MDS is cur-
rently working to license this technol-
ogy in China, where specific recycling
mandates have been implemented.
According to Lien, the recovery of co-
balt, and other battery materials, such
as graphene, may further contribute
to the economics of the process.
Membrane mechanical stability
Large-volume separations, such as
desalination, and other applications
of crossflow filtration demand that
membranes are not only capable of
precisely selective separations, but
are also sturdy and durable enough
to withstand high pressures and
shear stresses. A new membrane
NOVEMBER 2017
EWM

implement, he says. Other methods rently in final commissioning stages,

FIGURE 4. At this plant, minerals are recovered
from desalination waste streams, resulting in an
economical water-reuse scheme
technology (Figure 3) developed by
the Global Aqua Innovation Center at
Shinshu University (Nagano, Japan;
www.shinshu-u.ac.jp/coi) and Penn
State Universitys Materials Research
Institute (State College, Pa.; www.
mri.psu.edu) enables the creation of
membranes that leverage the desir-
able separations properties of gra-
phene oxide (GO) while maintaining
mechanical stability. Previously de-
veloped GO-based membranes have
required integration of carbon nano-
tubes to overcome structural weak-
nesses, or the creation of GO-poly-
mer composites, which dilute GOs
separation abilities.
This new method begins with a po-
rous polymer support onto which an
adhesive is coated. Then, a water-
based surfactant solution of GO and
few-layer graphene (FLG) is spray-
coated onto the membrane structure.
This water-based solution is treated
with divalent ions to increase its sta-
bility, and can be mixed with other
components in order to tailor the
membrane properties, says Aaron
Morelos-Gomez, lead researcher on
the project. After optimizing the ra-
tios and conditions, we could obtain a
shear-resistant membrane with good
salt rejection, he explains. In addi-
tion to salts, the research also looked
at the removal of dyes from water in
crossflow filtration operations. The re-
search team has created a membrane
20 20 cm2 in area and conducted
several trials at laboratory scale. Mo-
relos-Gomez is confident in the poten-
tial to scale up this technology. Since
we are spray-coating a water-based
solution, the deposition does not have
limitations on area size and is easy to
for fabricating GO-based membranes
employ vacuum filtration equipment,
which can be more difficult to scale up.
We will keep improving this technol-
ogy so we can match the performance
of commercial reverse-osmosis mem-
branes and implement a scaled-up
technology, Morelos-Gomez says.
As the work progresses to commer-
cialization, the team is investigating
additional applications and applying
for patents.
Looking to water reuse
Although membrane systems have
been used for over 30 years in water-
treatment facilities to remove turbidity,
bacteria and viruses, among numer-
ous other contaminants, water reuse
and conservation efforts are driving
operators to look at new process
schemes to maximize recovery, ac-
cording to Harold Fravel, executive
director of the American Membrane
Technology Association (AMTA; Stu-
art, Fla.; www.amtaorg.com). Fravel
lists several examples, including mod-
ularization and closed-circuit desali-
nation. A closed-circuit desalination
system is run in a semi-batch mode
with scheduled purges, which allows
for very high recovery, he says. Other
plants have employed a scheduled
switch in flow direction or changes to
the process water to minimize buildup
of potential foulants and scale. These
efforts reportedly improve recovery
rates from around 7580% to as high
as 9095%.
The byproduct streams from
membrane plants whether the
concentrate from a RO plant or the
backwash flow from a low-pressure
system also present opportunities
for water reuse, explains Fravel. A
few facilities are blending their con-
centrate with wastewater discharge
for reuse applications, he says.
Often, the RO concentrate may con-
tain a host of minerals, and may pres-
ent opportunities for recovery. A new
plant installed in El Paso, Tex. (Figure
4) is the first to employ a proprietary
minerals-recovery process developed
by Enviro Water Minerals Co. (EWM;
Houston; www.envirowaterminerals.
com). The new facility, which was
completed in April 2017 and is cur-
treats a stream of brackish water and
waste brine concentrate from an ad-
jacent desalination plant to recover
minerals for sale and return over
2 million gal/d of treated water back to
the desalination plant. This effectively
eliminates the need for wastewater dis-
posal, which can be costly and create
environmental concerns.
Hubble Hausman, EWMs chief ex-
ecutive officer likens the process to a
petroleum refinery, in that several dif-
ferent process units are used in a spe-
cific configuration to recover individual
components. Each stage is targeting
certain ions to extract. Its incremen-
tal processing using the whole gamut
of different types of membranes, he
continues. EWM uses not only RO
membranes, but also NF, electrodi-
alysis, and bipolar membranes, as
well as other processes such as ion
exchange and more. In order to en-
sure continuous operations that can
handle the throughput requirements
coming from the upstream desalina-
tion plant, EWM has built extensive
redundancies into the system, so
that all units can be regenerated or
cleaned as needed.
The next step for EWM will be to
adapt this process for seawater de-
salination, and Hausman cites that the
industry faces several challenges in
this arena that EWMs technology mit-
igates, including environmental regu-
lations surrounding seawater intake
and discharge. Since our process is
full-recovery desalination, there are no
discharge concerns, he mentions.
Furthermore, since EWMs process
also creates a large amount of sal-
able products from recovered miner-
als, Hausman believes it is feasible for
the company to build robust seawater
intake and docking and transport sys-
tems to be compliant with stringent
regulations. Most other standalone
treatment plants wouldnt be able to
afford such costly intake systems,
he says. Looking forward, EWM also
wants to adapt this process to treat
cooling-tower blowdown water and
produced water from hydraulic frac-
turing two areas where solutions
for effective treatment and reuse are
increasingly critical.
Mary Page Bailey

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 17

 Newsfront

Protect Your Plant

Both physical security and cybersecurity must be in place
to keep chemical facilities safe from attack

IN BRIEF

W
hile almost all CI sectors assessments Schneider-Electric

CFATS businesses in FY 2015 FY 2016

2% 3% 5%
todays world 3%
THREAT VECTORS 4%
are concerned 4%
9%
PHYSICAL SECURITY with security both physi- 2%
2%
SOLUTIONS cal security and cybersecu- 35%
rity chemical processors 43%
SHORING UP 29% 17%
CYBERSECURITY likely have a deeper inter-
est, because the industry 8%
has been identified by the 11% 8% 8%
2%
U.S. Department of Home- 3% 2%
land Security (DHS; Wash- Chemical (2%) Governemt facilities (11%) Chemical (5%) Energy (17%)
Defense industrial base (3%) Information technology (3%) Commercial facilities (3%) Food and agriculture (2%)
ington, D.C.; www.dhs. Emergency services (9%) Transportation systems (8%) Communications (4%) Governemt facilities (8%)
gov) as a potential target Energy (29%) Water and wastewater
systems (35%)
Critical manufacturing (4%) Information technology (2%)
Dams (2%) Transportation systems (8%)
for terrorism. As a result, Emergency services (2%) Water and wastewater
chemical processors that systems 43%)

are considered high risk FIGURE 1. This diagram of the Critical Infrastructure Sectors Assessment for 2015
according to DHS criteria and 2016, as seen in the Industrial Control Systems Cyber Emergency Response
must adhere to regulations Team (ICS-CERT) annual assessment report, shows that the number of assessments
on chemical facilities has grown from 2% in 2015 to 5% in 2016 so there is recogni-
put forth by the depart- tion of the increasing threat
ments Chemical Facilities
Anti-Terrorism Standards (CFATS; see also and then to create an outer perimeter with
Chem. Eng., September 2009, pp. 2123). security that would prevent a saboteur from
According to DHS, the CFATS program getting to these areas, explains Joe Mor-
identifies and regulates high-risk chemical gan, business development manager of criti-
facilities to ensure that they have security cal infrastructure with Axis Communications
measures in place to reduce the risks associ- (Chelmsford, Mass.; www.axis.com/us/en).
ated with certain high-risk chemicals. Initially This cultivated the need for physical barriers
authorized by Congress in 2007, the program and detection methods at chemical facilities
uses a multi-tiered risk assessment process and brought into the light the fact that chemi-
and requires facilities identified as high-risk to cal processors face larger and more signifi-
meet and maintain performance-based secu- cant threats than some other industries.
rity standards appropriate to the facilities and Since then, he continues, it has been real-
the risks they pose. On December 18, 2014, ized that physical security interacts with cyber-
the president signed into law the Protecting security, because if someone were to hack into
and Securing Chemical Facilities from Terror- a chemical plants mainframe and gain access
ist Attacks Act of 2014 (the CFATS Act of to processes via control networks, they could
2014), which reauthorized the CFATS pro- just as easily perform the same type of sabo-
gram for four years. It is expected that DHS tage. So physical security and cybersecurity
will continue the program in the future, as well. are becoming closely intertwined.
Adrian Fielding, global marketing manager,
CFATS integrated protective solutions, with Hon-
CFATS was initially developed over con- eywell Process Solutions (Houston; www.
cerns that an individual or group could honeywellprocess.com) agrees: The physi-
breach the perimeter and infiltrate a chemical cal security and cybersecurity relationship
facility with the intent of damaging storage is very symbiotic. You need one to protect
vessels holding toxic materials, so the first the other. You need physical security to pre-
step was to understand, at each of these vent someone from getting on site and into
facilities, where the chemicals were stored a server room and causing a cyberattack
18 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
Convergint
Deter
Detect
Deny
Delay
Defend
FIGURE 2. The goal of physical security is to keep
the facility and chemical supply chain safe. Se-
curity should aim to first deter, then detect, deny,
delay and, finally, defend. One of the current areas
of focus is in early detection
internally, and you need cybersecu-
rity to prevent someone from hack-
ing into a security system and taking
critical systems down.
Therefore, protecting just one or
the other is not enough, says Jay
Abdallah, global director of cyberse-
curity solutions at Schneider-Electric
(Andover, Mass.; www.schneider-
electric.com). Securing one area is
not sufficient, as the weakest area
can be penetrated, causing a breach.
All areas must be equally secured,
using a combination of multiple de-
tective and preventive controls.
Threat vectors
But before a chemical processor can
secure the facility, it is important to
know the threats from which they re-
quire protection.
In the past, most chemical facilities
had some sort of physical perimeter,
such as fencing, for safety purposes
to keep people from entering the
property, says Darin Dillon, business
Axis Communications
FIGURE 3. Thermal network cameras outperform
a visual camera in dark scenes and can detect
people and objects in 24/7 surveillance, from pitch
dark areas to a sunlit parking lot. Axis thermal
network cameras create images based on the heat
that always radiates from any object, vehicle or
person
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
development manager, with Con- ees and surrounding communities.
vergint Technologies (Schaumburg, Today, the goal of physical security
Ill.; www.convergint.com). However, is to keep the bad apples out of the
after 9/11 it became recognized that facility and away from the chemical
some of the chemicals stored and supply chain, says Dillon.
processed could be stolen, sold on Gaining physical access to a
the black market and/or used as chemical process ends the game
dirty bombs elsewhere or that some- when it comes to risk, since physical
one could enter a facility and turn access is meant to be the last line
valves, releasing toxic or explosive of defense, says Schneider Elec-
chemicals, endangering employ- trics Abdallah. The biggest threats
PARATHERM PROVIDES
20% Off
S ystem
Cleane
rs
throug
h
Dec. 3
1
FOR THERMAL FLUID SYSTEM USERS
n PERFORMANCE
Testing has proven Paratherm heat transfer luids superior
in thermal stability and overall e ciency. (-88C to +343C)
n SERVICE
Independent research shows a preference for Paratherm
among users familiar with major competitors.
#1 reason: better customer service (data on ile).
n COMPATIBILITY
Certiicates of compatibility available for most
competing products. Top o your system with
Paratherm and begin getting all the advantages.
n AVAILABILITY
Global stocking
Bulk Delivery
Short supply? Signiicant delays?
Let Paratherm deliver for you.
n TECHNICAL SUPPORT
Expert engineering, product
support, and training
Comprehensive analysis program
Advanced lab capabilities
Get MORE with Paratherm
+1 877-789-0443
www.paratherm.com/chem-eng
2009 Renaissance Blvd.
King of Prussia, PA 19046 USA
Intl: +1 610-941-4900
A Division of Lubrizol Fax: +1 610-941-9191
info@paratherm.com
For details visit adlinks.chemengonline.com/66434-17
NOVEMBER 2017 19

FIGURE 4. Integration of physical security sys-
tems, along with the use of mobile devices and
apps, is another way processors are hardening
the security of their facilities
from a physical perspective at these
facilities are from natural disasters,
terrorism and physical damage
caused from loss of control (caused
by a cyber or other breach). Due to
the high degree of risk at chemical
processing facilities, security must
always be a high priority.
He adds that cyberthreats that af-
fect process control and safety could
have a huge impact and must share
elevated attention, adding another
dimension to plant security.
Seth Carpenter, cybersecurity
technologist with Honeywell Process
Solutions agrees that loss of safety
and process control are the two
biggest cyberthreats for chemical
processors. Hackers getting into a
system and taking actions that could
compromise the safety of the plant,
personnel or surrounding communi-
ties and gaining access in a way that
could negatively impact production
and availability of the facility are real
issues for todays chemical industry.
The reason these threats exist, says
Joshua Newton, security architect
and team lead within the Connected
Services Organization at Rockwell
Automation (Milwaukee, Wis.; www.
rockwellautomation.com), is because
during the last five to ten years, the
manufacturing and process world
started to move quickly toward tech-
nology enhancements because they
offered better analytics and big data
and all the related production bene-
fits. So there was a push to become
a connected enterprise, he says.
However, it brought with it an inher-
ent risk of exposure to devices.
Neil Peterson, DeltaV product
marketing director, with Emerson
Automation Solutions (Round Rock,
Tex.; www.emerson.com) agrees:
20
Apollo Security
As we went to widely networked
solutions with a lot of open commu-
nications and standards, it allowed
the operating and financial benefits
of communications between con-
trol and business systems, but also
the stage was set for bad things to
happen. It is now very possible for a
hacker or cyber terrorist to get into
a plant network and create havoc,
he warns.
What type of havoc? Malware at-
tacks, which are often introduced
via social engineering (for example,
corrupt links sent via email) or unwit-
tingly through portable hard drives,
gain access and move laterally
through a system gaining creden-
tials, elevating privilege to an admin-
istrator and then moving about the
system installing software and creat-
ing denial of service. This means it
is possible if the right protections
arent in place for every worksta-
tion on a control system to be taken
offline, leaving operators blind to the
process, explains Peterson. Not
only is this a dangerous situation,
but its a costly one because you are
forced to take the system down un-
less you are willing to run blind, so
youre losing production.
And these types of attacks are
on the rise for many industries, in-
cluding energy, critical manufactur-
ing and infrastructure. According
to Schneider Electrics Abdallah, in
2015, the transportation industry
reported 23 attacks and the water
industry reported 25. In 2016, the
energy industry reported 59 attacks,
while critical manufacturing faced
63. Thus far in 2017, 2,000 food-
and-beverage industry companies
fell prey to a well-known ransom-
ware attack called Petya.
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
Clearly attackers are getting more
savvy and those looking for the big-
gest bang for their effort may con-
sider chemical facilities to be of higher
value, says Abdallah (Figure 1).
Attacks such as these are often
indirect attacks in that the malware,
once introduced, moves around the
system on its own. There are also
directed attacks where malware or
ransomware gets into the system
via an attachment or portable hard
drive, corrupts a workstation and
then phones home to the attacker,
says Peterson. From that point, the
attacker starts issuing commands
on the workstation using the users
credentials and begins to pivot and
roam around the network to find a
target. If that target is the control
system, the attacker then attempts
to capture the credentials of the en-
gineer responsible for that worksta-
tion and can remotely access the
control system, making it do what-
ever he wants.
Physical security solutions
The good news is that most pro-
cessors are taking steps to protect
both the physical and cybersecurity
of their facilities. When it comes to
providing physical security, most fa-
cilities are already doing a good job
of it with fences, cameras and ac-
cess control, but they should also
be trying to stay one step ahead of
the bad guys and one of the cur-
rent areas of focus is in early detec-
tion, says Convergints Dillon. We
want to give them earlier warnings if
theres a threat. We can put systems
in place that let the bad folks know
we see them and encourage them to
move along (Figure 2).
Early detection systems include a
variety of cameras and analytics, pe-
rimeter intrusion detection, ground-
based radar and other technologies
that allow security to see potential
intruders before they get to the gate,
so security has ample time to react
when and if they do reach the gate.
Theres a formula that can be
used to create an appropriate early
detection zone, says Axiss Mor-
gan. Using the formula, proces-
sors determine how many minutes
it would take to stop someone from
reaching the critical aspect inside
NOVEMBER 2017
Honeywell Process Solutions
FIGURE 5. Since chemical processors prefer to focus on making chemicals, not defending against cy-
berattacks, control system vendors, such as Honeywell, offer managed services, which assist customers
with services such as assessing their systems and determining where they stand in the defense against
cyberattack, what steps they still need to take, as well as recommending and installing necessary tech-
nologies and keeping up with patches and updates
the plant and, based on that time,
they can figure out how far away, in
distance, they need to detect some-
one approaching the plant. And, at
that distance point, they need to in-
stall early detection methods. Ther-
mal cameras are one of the newer
technologies for early detection, he
says, because thermal technology
offers improved analytics that exam-
ine pixel changes using advanced
algorithms. Thermal imaging has
the ability to detect and analyze pixel
changes and determine if they have
the formality of a human being, and if
those cameras are integrated with a
video management system, security
can be alerted so early action can be
initiated, says Morgan (Figure 3).
Integration of such systems, along
with the use of mobile devices and
apps, is another way processors
are hardening the physical security
of their facilities, says Bill Lorber,
vice president of sales and market-
ing, with Apollo Security (Newport
Beach, Calif.; www.apollo-security.
com). It is very easy to tie access
control and video systems together
so that security people can see when
someone comes in and ensure the
card matches the live image. In ad-
dition you can integrate systems so
that when a door opens or theres
motion in an area, live video auto-
matically appears on the security
system monitor (Figure 4).
He continues: Mobile devices are
becoming much more important in
this system as well, because you are
no longer restricted to a guard sitting
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
in a room with a monitor. The man-
ager of security can also see activi-
ties when a group of people comes
in or access video associated with
events from a remote location via a
mobile device using a live web ver-
sion or app.
This type of integration and auto-
mation allows security to evaluate
a situation in milliseconds versus
having an alarm event followed by
several minutes of locating the cor-
rect camera for that location, then
searching for a binder with instruc-
tions on how to respond and react,
says Dillon. Integration and automa-
tion provide a faster, more efficient
response, which minimizes the cost
of security, wasted time and potential
for errors.
Shoring up cybersecurity Your sustainable cost savings with
The first layer in creating a system
thats hardened against a cyberat- our Sulfuric Acid Recovery plants
tack, says Tony Downes, Global
C
HSE Advisor with Honeywell Process
Solutions, is in the system design. Feed rates up to 145t/h
There are things we can incorpo- L
rate physically at the plant level that P
make it more difficult for someone S
to interfere with the process. For in- M
stance, because its a safety issue R
before its a security issue, we dont
M
have valves without backup sys-
tems, which helps prevent someone
from opening a valve and causing a
release, he says. Theres things we
do for process safety reasons inside
the plant design that make it inher-
ently safer and, if those are in place,
you can then get into defending the
NOVEMBER 2017 21
For details visit adlinks.chemengonline.com/66434-01
 control system, making it even more monitored, says Alexandre Peix- able schedule, so when you see an
difficult for a malicious attacker to do oto, DeltaV cybersecurity marketing anomaly, it is easy to detect.
a lot of harm. manager with Emerson Automation But, because chemical proces-
Some of the simplest methods Solutions. He adds that applications sors often prefer to focus on mak-
of thwarting a cyberattack include should be run on an embedded sys- ing chemicals, not defending against
what Rockwell Automations New- tem, which is harder to compromise. cyberattacks, some control system
ton calls basic cyber hygiene, such Further, processors should use fire- vendors are offering managed ser-
as keeping operating systems up walls, which allow a certain flow of vices. They can hire people to help
to date with patches. Even though communications to devices, but pre- out with anything from assessing their
cyberattacks seem very sophisti- vent others that arent approved. An- systems and determining where they
cated, under most circumstances, tivirus software should be employed stand in the defense against cyber at-
the methods employed are known at workstations to prevent known tack and what steps they still need to
attack vectors that can be prevented threats from infecting them. And on take, as well as recommending and
with patches and updates. top of this, we are starting to see installing necessary technologies and
Beyond installing patches, control whitelisting applications, which pre- then keeping up with patches and
system providers suggest a layered vent software that has not been ap- updates for them, says Honeywells
approach to cybersecurity. Defense proved from running on the system. Carpenter (Figure 5).
in depth is the best approach and However, while all this helps pre- And, theres certainly no shame
not just because we can provide vent attacks, control system provid- in taking help from experienced se-
each layer, but because it is the most ers say that defense is not enough, curity professionals as there is a lot
comprehensive protection. Beyond so monitoring has become more to keep up with in an effort to keep
that, always make sure the cyber- popular as the threat grows larger. facilities properly locked down and
security youre putting in place is Cybersecurity is not just about safe from harm. Whats most im-
context based. What youre trying to protection, says Peixoto. Monitor- portant is taking the steps to protect
protect is your process, so the first ing helps the user detect anomalies against all forms of attack because
layer of defense is making sure that by monitoring data across different chemical facilities are attractive to
if your control systems are exposed networks to make sure everything potential terrorists, says Honey-
to external connections, that they moves the way it should. Control wells Downes. n
are limited, read-only and always systems tend to work on a predict- Joy LePree

Why should you

T +49 2961 7405-0 | info@rembe.de filter your water?
Accumulation of plastic fines in cutter water stream causes uneven
cooling of pellets; blockage of cooling water passages, and an
increase of water temperature that results in poor pellet quality.
The removal of plastic fines is made easy with Tekleen automatic self
cleaning water filtration systems, with their specially designed screen
technology.
Your Specialist for
PRESSURE RELIEF SYSTEMS Cooling
Tower
and
REMBE | All rights reserved

EXPLOSION SAFETY
Shell & Tube
X-Changer

TG TG
Cutter
Water
Reservoir

Consulting. Engineering. Products. Service.

Gallbergweg 21 | 59929 Brilon, Germany

F +49 2961 50714 | www.rembe.de

Inc.
3809 Beam Road Suite K Charlotte, NC 28217, USA
T +1 704 716 7022 | F +1 704 716 7025 2672 S. La Cienega Bl vd, Los Angeles, C A 90034 USA
info@rembe.us | www.rembe.us (800) 336-1942 (310) 839-2828 www.t ekleen.com inf o@t ekleen.com
For details visit adlinks.chemengonline.com/66434-24
For details visit adlinks.chemengonline.com/66434-27
22 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
Focus
Maintenance-Related Products
Handheld device speeds
maintenance, startup efforts
The AMS Trex Device Communicator
(photo) uses the companys Power
the Loop technology. By remov-
ing the need for an external power
supply, the device helps users work
more effectivey and perform faster
device configuration, on the bench
or in the field. This allows users to
perform device-configuration tasks
before power and I/O infrastructure
are in place, without the need for
the installation of the host system,
wiring, piping and other elements.
Technicians can simply connect the
communicator to a loose device to
power it up, speeding configuration
on the bench. Emerson Automa-
tion Solutions, Austin, Tex.
www.emerson.com
This vibration sensor
provides realtime data
Vibration fluctuations in water- and
wastewater-treatment systems often
provide an early indicator of prob-
lems that cause equipment failure,
such as pump cavitation, unbal-
anced fans and bad bearings. The
new Sensaphone Vibration Sensor
(photo) can be permanently mounted
on equipment such as pumps, mo-
tors, generators and diesel engines
to continuously monitor vibration ve-
locity and detect unusual conditions.
The sensor provides constant, real-
time data, and sends an immediate
alert to designated personnel when
vibration levels fall out of a desig-
nated range. It benefits from simple
two-wire 420-mA installation, is
easily configured, and requires no
special software, says the company.
Sensaphone, Aston, Pa.
www.sensaphone.com
Air bearings enable smooth
nano-postitioning
The A-62x PIglide Series of rotary air
bearings have no rolling or sliding el-
ements, and deliver frictionless, non-
contact motion. This is said to result
in negligible reversal error, and to
provide greater stability over straight-
ness, wobble, eccentricity and ve-
Note: For more information, circle the 3-digit number on p. 62, or use the website designation.
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
locity changes. Air bearings replace Emerson Automation Solutions
mechanical contact by a thin film of
air. This air layer is completely friction-
less, eliminating breakaway stiction
and drag friction during operation. The
PIglide RM motorized rotary air bear-
ing stages offer a complete nano-
positioning solution, according to the
company. These rotary positioners
can handle speeds to 2,500 rpm, and
ensure extreme precision with radial
motion errors as low as 50 nm, axial
runout as low as 50 nm, and tilt er-
rors down to 0.3 arc-sec, and they
require no maintenance or lubrication,
says the company. Physik Instru-
ments (PI), Auburn, Mass.
www.pi-usa.us
Smart glasses allow users
to support their machines
Remote Assist (photo) is an inno-
vative service concept that uses
Internet-enabled smart glasses to
enable the companys hotline tech-
nicians to support its machines in
realtime. The technology enables
virtual communication between ma-
chine operators and service techni-
cians via a wi-fi interface. Users who
require assistance to operate their Sensaphone
equipment, deal with fault conditions
and so on can now get virtual sup-
port from this company. A camera
integrated to the glasses transfers
its perspective of the machine di-
rectly to the company technicians
monitor, allowing the remote sup-
port team to respond accordingly.
The glasses are also equipped with
a microphone and headphones for
audio communication with support
personnel at the company. The
Romaco Group, Karlsruhe, Germany
www.romaco.com
This high-performance The Romaco Group
hydraulic oil is eco-friendly
Panolin HLP Synth 32 is a biode-
gradeable hydraulic oil that has been
engineered to meet demanding re-
quirements that are typical of todays
mechanical systems, such as power
density, higher working pressures,
motor speeds, oil-circulation cycles
and temperatures. The hydraulic fluid
23
 ITT PRO Services recently passed the Bosch Rexroth
Fluid Rating List, a scientific, stan-
dardized evaluation procedure that is
designed to test the fuid character-
istics and interaction with key com-
ponents, at 500 bars (conventional
tests are conducted at 350 bar),
says the company. Panolin Group,
Madetswil, Switzerland
www.panolinamerica.com
Non-contact gas bearing
improve rotor balancing
Bently Bearings are pressurized air
bearings that provide non-contact
support for rotors during balancing
operations. Specifically, the device
produces a consistent signal that is
exactly the same for each revolution,
allowing for finer resolution during bal-
ancing operations, says the company.
This helps to eliminate both damage
to the rotor from hard rollers, and the
mess of oil-film bearings in vacuum
environments. Unit loading of air bear-
ings has been demonstrated at over
400 psi, using 600-psi input pressure.
With normal shop pressure of 100 psi,
SpotSee the air bearings will carry 60 psi unit
loading. New Way Air Bearings,
Ashton, Pa.
www.newwayairbearings.com
Wireless device supports
predictive maintenance
The i-Alert Asset Intelligence platform
lets users monitor all machines that
have a compact, wireless i-Alert2
Machine Health Monitor (photo) con-
nected to them. The platform, on-ma-
chine sensor and a mobile app that
provides easy access to the data,
allow users to monitor operation and
manage data from a single web in-
SKF USA terface. The system allows users to
visualize, in a simple timeline, trend
data, machine notes, technical data
and vibration spectrum data that are
collected via the i-Alert2 app. Users
can manage data collection by set-
ting up designated routes and the
app will guide a user to which assets
and what types of data to collect on
the route. Then, the app will generate
a report and email it to the user. ITT
PRO Services, Seneca Falls, N.Y.
www.itt.com
Integrated platform handles
Sensonics
various monitoring inputs
The SpotSee connectivity platform
connects the companys various mon-
itoring devices to sense vibration,
24 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
tilt, shock, temperature and humidity
and world-class analytics capabili-
ties to help users spot potential dam-
age to their operations or logistics net-
work, with enough time to intervene.
The companys OpsWatch device
(photo) enables realtime monitoring
of low-frequency shock and vibra-
tion. The system provides alerts when
vibration is outside the normal range,
to reduce risk of unplanned downtime
and support preventive maintenance
efforts. SpotSee, Dallas, Tex.
www.spotsee.io
System ensures lubrication
to multiple points
The MultiPoint Automatic Lubricator
TLMP Series (photo) delivers proper
lubrication for multiple bearing points
in rotating machinery applications. The
sturdy system can supply from 1 to
18 lubrication points on a controlled
and timely basis in order to deliver the
right lubrication amount at the required
frequency to optimize bearing perfor-
mance and equipment reliability. It has
pluggable outlets and is packaged as
a complete kit that is designed for easy
installation and user-friendly program-
ming via a keypad with an LED display.
The TLMP system requires low-level
and malfunction alarms, with notifica-
tions even at remote location to alert
when the lubricant reservoir is empty
or when an outlet is blocked. SKF
USA, Lansdale, Pa.
www.skfusa.com
Keep an eye on vibration to
prevent machine damage
This companys range of 420-mA
sensing devices detect vibration
in critical plant equipment compo-
nents, such as motors, fans, pumps
and compressors. The sensor family
includes the PZDC piezoelectric and
VEL/GDC electrodynamic, absolute
velocity vibration transmitters, and
the DNX80 relative-shaft vibration,
thrust-position and speed-proximity
probe transmitters. The electro-
dynamic VEL/GDC sensor (photo)
provides a 420-mA loop-powered
output that is proportional to velocity
vibration, and offers the advantage
of dual-case isolation in conjunction
with a low impedence circuit, making
it ideal for high-noise environments,
says the manufacturer. Sensonics
Ltd., Berkhamsted, U.K.
www.sensonics.co.uk n
Suzanne Shelley
NOVEMBER 2017
New Products
The launch of a
new metering system
Launched last month at Weftec (Chi-
cago; October 24), the new Bravo
chemical metering system provides
improved process control with reli-
able, accurate and repeatable flow,
and reduced chemical consumption,
says the company. Bravo is an inte-
grated, modular and scalable solu-
tion used in a variety of industries for
disinfection, pH control, flocculation,
corrosion inhibitors, oxygen scaven-
gers and containment elimination.
Bravo incorporates NSF/ANSI 61 cer-
tified progressive-cavity (PC) metering
pumps. The unique design of a PC
pump offers several advantages com-
pared to traditional chemical-metering
pumps due to pumping characteris-
tics that allow for consistent, precise,
repeatable metering with low shear,
minimal pulsations and no vapor lock.
These pumps also wear predictably,
so there is no risk for catastrophic fail-
ure. Seepex Inc., Enon, Ohio
www.seepex.com
This compact mining crusher
handles 3,000 ton/h
The new ERC25-25 eccentric roll
crusher (photo) can process hard rock
and ores efficiently and economically in
underground mining operations. It fea-
tures a compact design and an inte-
grated screen that is 20 to 50% lower
than conventional primary crushers, a
feature that greatly simplifies transpor-
tation, installation and maintenance
below ground, says the company.
The patented design features a roll
mounted eccentrically between the
crushing and the screening chambers,
which offers greater efficiency and pro-
ductivity compared with other crusher
types. The large, constant stroke of
the ERC25-25 crusher combines
with the integrated screen to pro-
vide very high crushing intensity and
throughputs of up to 3,000 ton/h.
thyssenkrupp Industrial Solutions AG,
Essen, Germany
thyssenkrupp-industrial-solutions.com
Custom pressure vessels with
agitation and dispersion options
This company has fabricated a 300-
gal vessel (photo) designed for 5 psi
internal pressure at 300F. All of the
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
wetted surfaces are stainless-steel thyssenkrupp Industrial Solutions
type 304L polished to 240-grit finish.
The vessel is agitated by a special
disperser blade driven to 1,150 rpm
by a 75-h.p. explosion-proof motor.
The agitator shaft utilizes a mechani-
cal seal running in an oil bath. A 50-
psig ASME Code-stamped baffled
jacket surrounds the sides and ves-
sel bottom for heating and cooling.
All elastomers, nozzles, sensors, dip
tubes, valves and operator controls
are supplied based on the end users
specific requirements. Numerous
other custom-engineered options are
available on fabricated pressure ves-
sels, including jacketing, agitation,
pressurization, sanitary requirements
and more. Charles Ross and Son
Co., Hauppauge, N.Y.
www.mixers.com
Explosion-proof blenders for
large-batch processes
The E8815 stainless-steel, large-
batch explosion-proof blender
(photo) is manufactured to Class
I, Div. I, Groups C & D explosion-
proof electrical rating. ATEX ratings Charles Ross and Son
and non-explosion-proof models are
also available. These blenders are
designed for pharmaceutical and
chemical-blending applications. Ad-
ditional options include the following:
jacketed containers available for use
with refrigerated or heated circula-
tors; temperature sensors; thermal
camera; and several standard blend-
ing assemblies. E8815 blender mod-
els range from 10 to 25 gal in volume,
with stainless-steel exteriors and
standard powder-coat finish avail-
able. Servo-controlled blending-con- Eberbach
tainer auto lift and pour functionality
makes large-batch processing easier
to control and integrate. Eberbach
Corp., Ann Arbor, Mich.
www.eberbachlabtools.com
A smart system gets the
compressor lubrication right
The XperLUBE system (photo) uses
automotive-style solenoid injectors
to deliver lubricant in precise quanti-
ties. Unlike traditional lubrication de-
vices, XperLUBE integrates fully with
modern control systems and adapts
to changes in operating conditions.
A key feature is the way each injec- Hoerbiger Ventilwerke
NOVEMBER 2017 25
 E Instruments tor records the precise volume of oil
delivered at every stroke. This mea-
sured lube rate is used as a feed-
back signal to ensure that the actual
lube rate always matches the target
value. Standardized, modular design
makes XperLUBE easy to retrofit to
existing compressors. Users can start
with a simple standalone installation
or opt for a more powerful system
linked to the plants distributed con-
trol system (DCS) if necessary.
Hoerbiger Ventilwerke GmbH & Co. KG,
Vienna, Austria
www.hoerbiger.com
A portable emissions analyzer
for combustion operations
The E9000 emissions analyzer (photo)
features a heated sample line and is
suitable for regulatory and mainte-
nance use in boiler, burner, engine,
turbine, furnace and other combus-
tion applications. The analyzer can
Bolz Intec
accommodate up to nine total gas
sensors, including electrochemical
sensors for O2, CO, NO, NO2, SO2 or
H2S, or NDIR sensors for CO2, CxHy
For details visit adlinks.chemengonline.com/66434-07
26 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
(HC) or high CO. An internal thermo-
electric chiller provides automatic con-
densate removal. The devices internal
data storage has memory to conduct
up to 16,000 tests, and the onboard
software automatically logs data.
E Instruments International LLC,
Langhorne, Pa.
www.e-inst.com
Hastelloy drums designed for
hygienic applications
These lidded drums (photo) are dull
TIG (tungsten-inert gas) welded with
welding filler material and without
gaps. The seams are rolled flat and
finely polished inside and out. The
drums are also easy to clean and
residue-free, and have a high stabil-
ity, even at maximum load. They are
available in volumes from 0.5 to 300
L, and in different diameters. The sur-
faces are polished or electro-polished
for optimum product output with
roughness less than 0.25 m. Seal-
ing materials include silicone, EPDM,
Viton, and FEP-coated (fluorinated
ethylene propylene) seals with FDA
NOVEMBER 2017
approval. In addition to the industry- outlet for oversized and foreign par-
standard materials, the company ticles. It prevents unwanted agglom-
now also offers drums for extreme erates from remaining in the final
conditions in Hastelloy 2.4602/C product. All product-wetted parts
22 nickel alloy, which is highly cor- are mainly stainless steel (1.4301).
rosion resistant to acids and chlo- Cleaning and replacing the sieve
rine dioxide. Bolz Intec GmbH, decks is extremely simple, since
Argenbhl-Eisenharz, Germany the Contromat can be dismounted
www.bolz-intec.com without tools. The control sifter is
also available in an optional ATEX Allgaier Werke
Controlled sifting of version. Fuchs Maschinen AG,
bulk materials Granges-Paccot, Switzerland analyzes the images and determines,
The Contromat VE www.fuchsag.com in fractions of a second, whether a
450 (photo) and particle needs to be sorted out. The
VE 630 (which is NIR technology enables precise bulk material then passes by a strip
square shaped) sorting in fractions of a second of compressed-air nozzles, and the
handle sifting ca- Materials with the same visual appear- rejected particles are blown out. The
pacities between ance can now be precisely, quickly sorting precision is said to be at least
0.15 and 0.3 m. and cost-effectively sorted with the 95% in one sorting step. The MSort
Previously, the new MSort NIR (photo), which uses NIR type AP sorts bulk materials in
Contromat had near-infrared (NIR) spectroscopy to the grain range of 1050 mm with
been delivered Fuchs Maschinen
physically analyze the material. At the a throughput of up to 40 ton/h. This
without an outlet beginning of the sorting process, the machine is especially suitable for
for foreign particles, which remained material flow passes by an NIR cam- separating plastics in glass recycling
on the sieve and had to be removed era through a chute in free-fall. The processes. Allgaier Werke GmbH,
manually or by means of a suction camera allows the individual particles Uhingen, Germany
nozzle. Now, the new Contromat to be uniquely identified and the im- www.allgaier-group.com
version is rectangular, and has an ages to then be analyzed. Software Mary Page Bailey and Gerald Ondrey

At RedGuard, we build the worlds safest blast-resistant

buildings because we know whats on the table.

For details visit adlinks.chemengonline.com/66434-23

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 27

 Facts At Your Fingertips
Filter Aids
Department Editor: Scott Jenkins
C
ake filtration is a common op-
eration across many sectors
of the chemical process indus-
tries (CPI). In cake filtration, the solid
being filtered acts as a screen so that
particles of the suspension are re-
tained by the medium, resulting in the
formation of filter cakes.
In some cases, filtration can be
difficult if the material being filtered
is highly viscous, highly compact-
ible or deformable, or if the filter cake
formed in the filtration is very small or
highly resistant to flow. For such situ-
ations, the addition of filter-aid mate-
rial can greatly improve the efficiency
and effectiveness of the filtration.
Filter aids enable cake filtration to
be used for a larger group of sus-
pensions, including those with wider
particle-size distributions, larger sol-
id concentrations, and gel-like and
highly compactible particles. This
one-page reference provides infor-
mation on the properties of common
filter-aid materials and how they are
used in industrial filtration.
Filter aid function
Filter aids are inert particulate or fi-
brous materials that are introduced
into a filtration operation in one of
two ways as a filtration pretreat-
ment called precoat or by adding
filter aid to the liquid to be filtered,
referred to as bodyfeed.
Precoat. Filter aid precoat is added
to form a layer of a second filter medi-
um to protect the main product of the
filtration. In a typical precoat process,
the filter aid material would be sus-
pended at low concentrations (0.5%
is common) in a tank that is agitated
to maintain the filter aid in a slurry. Fil-
ter aid material is typically added at
rates of 5001,200 g/m2 (1025 lb/
ft2) of filter area. The precoat is formed
on the surface of the mesh screen
or cloth membrane by recirculating
the filter aid slurry through the filter.
The coarse particles deposit on the
screen (septum) first, followed by the
finer particles. This occurs until a thin
layer (typically 1.5-3.0 mm) of filter aid
forms on the filter septum.
Bodyfeed. Bodyfeed, also called ad-
28
FIGURE 1. Diatomaceous earth is the fossilized
remains of ancient micro-organisms
mix refers to the addition of filter aid
material to the liquid that is to be fil-
tered, either by adding it directly to the
tank of liquid to be filtered or by dos-
ing filter aid from a slurry tank into the
filter inlet. Bodyfeed filter aid is used to
improve the flowrate of difficult-to-filter
materials by increasing cake porosity
and permeability, and decreasing filter
cake compressibility. A basic objective
of filtration with bodyfeed filter aid is to
achieve the highest possible flowrate
that achieves the clarification of the liq-
uid that is required. The type of filter aid
and its grade (particle size distribution),
as well as the filter aid dosage depends
on the solids content and other vari-
ables specific to each application. In
general, a filter aid dosage of half of the
percent solids by weight in the suspen-
sion to be filtered is common.
Filter aid materials
Several materials can be used as
filter aids, including asbestos, cel-
lulose, agricultural fibers, saw dust,
rice-hull ash, paper fibers and oth-
ers. More common filter aid materi-
als include diatomaceous earth (DE),
perlite and cellulose.
Diatomaceous earth. DE (Figure 1)
is the silica-based fossilized remains
of ancient diatoms (single-celled or-
ganisms). DE can be mined from
ancient seabeds, processed, and
classified to make different grades
of filter aids. The smaller the filter-aid
particle size, the smaller the process
particles can be removed, but the fil-
tration rate is lower. The particle size
capture by various filter aids may
also vary because of liquid viscosity,
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
Perlite Institute
FIGURE 2. Perlite is a glassy volcanic rock that
forms jagged particles after processing
surface charge, and so on.
Perlite. Another example of a com-
mon mineral filter aid is perlite (Fig-
ure 2). The inert perlite is a type of
naturally occurring, glassy volcanic
rock that forms particles with jag-
ged shapes upon processing. When
crushed and heated, perlite expands
explosively when water trapped in
the mineral structure vaporizes. Per-
lite can expand to about ten times its
original volume. After the expansion,
perlite forms jagged particles, which
interlock, and create microscopic
flow channels that allow filtrate to
travel through.
Cellulose. Cellulose is a fibrous, or-
ganic material that can be used as a
filter aid, and is used in filtration sys-
tems where silica-based materials
may not be compatible. The fibrous
structure of cellulose is designed to
adsorb sediment and fine particles.
The filterability of cellulose is poorer
than DE and perlite, but cellulose can
be incinerated, and can lead to filter
cakes that hold together more than
with other filter aids.
Filter aid selection
Preliminary laboratory tests can help
to identify the proper kind of filter
aid for a given application. First, the
chemical resistance and purity of the
filter aid material must be considered
for the liquid being filtered. Second,
the required grade (particle size) of the
filter aid should be determined. Third,
the quantity of filter aid needed for the
process should be calculated. A first
approximation of the quantity of filter
aid is one that results in a filter cake
volume that is equal to the volume of
material to be separated. n
NOVEMBER 2017
Technology Profile
Calcium Hypochlorite Production
By Intratec Solutions Slaked lime,
Slaked lime,
caustic soda, Sodium method Calcium method
chlorine

C
alcium hypochlorite,
Ca(OCl)2, is among the few
metal hypochlorites that is
stable enough to be pro-
duced as a solid salt. Because of this
fact, it is the main bleaching agent pro-
duced commercially as a solid (some-
times referred to as bleach powder).
The process
The following paragraphs describe
the production of calcium hypochlo-
rite (70 wt.%) from slaked lime, sodi-
um hydroxide and chlorine, a typical,
so-called sodium process. Figure 1
presents a simplified flow diagram of
the process.
Reaction. Initially, caustic soda so-
lution is mixed with recycled bleach
mother liquor composed of calci-
um hypochlorite and sodium chloride
dissolved in water in the caustic
mixing vessel. The resulting solution is
sent to the lime-mixing vessel, where
slaked lime is fed to form a milk-of-
lime slurry. This slurry is forwarded to
the salt nucleator vessel, where it is
mixed with chlorinator liquor recycled
material and recycled bleach mother
liquor. The resulting solution is su-
persatured with sodium chloride and
calcium hypochlorite, which initiates
the precipitation of the crystals. The
mixture from the salt nucleator ves-
sel is fed to the chlorinator along with
gaseous chlorine, which reacts with
calcium hydroxide and sodium hy-
droxide to form calcium hypochlorite
and sodium chloride. In this way, fur-
ther crystals of calcium hypochlorite
and sodium chloride are formed and
growth of pre-existing crystals occurs.
Separation. The chlorinator out-
Slaked lime
(97 wt.%) 3 4
1 2
Caustic
soda
(50 wt.%)
Chlorine
chlorine
Slaked lime,
Sodium method
chlorine,
sodium hypochl.
hypochlorite
Quicklime,
water, caustic Sodium method
soda, chlorine
n Raw material n Pathway n Main product
FIGURE 2. The diagram shows multiple production pathways for calcium hypochlorite
let slurry is fed into the a two-stage,
upward-flow cylindrical elutriator-clas-
sifier at its midpoint. Bleach mother
liquor from the calcium hypochlorite
centrifuge is fed into the bottom por-
tion of the lower stage of the elutriator
as the elutriating fluid. From the upper
portion of the elutriator, an aqueous
slurry containing most of the calcium
hypochlorite is withdrawn and sent
to calcium hypochlorite centrifuge.
An aqueous slurry containing denser
sodium chloride crystals are removed.
The bottom product of the elutria-
tor, an aqueous slurry containing the
denser sodium chloride crystals is
sent to the salt centrifuge.
The sodium chloride slurry from the
bottom of the elutriator is centrifuged,
and the sodium chloride wet cake
is then conveyed to an intermediate
tank. The salt-centrifuge mother liquor
is sent to the Ca(OCl)2 centrifuge.
Finishing. The wet cake from the cal-
cium hypochlorite centrifuge is dried
in a turbo dryer, and gases from the
dryer are scrubbed and released. The
dry calcium hypochlorite is squeezed,
prilled and then classified. The over-
sized and undersized solids are re-
turned for further processing, while
the calcium hypochlorite product is
directed to packing.
Process water
6 Sodium
chloride
8 (31 wt.%)
11
7 8. Salt tank
5 9
RW
Calcium
10
hypochlorite
ST
Calcium Quicklime,
Calcium method
water, chlorine
Quicklime,
Sodium method water, sodium
hypochlorite
Ca(OCl)2 production pathways
Calcium hypochlorite was initially pro-
duced by passing chlorine gas over
slightly moist calcium hydroxide. Cur-
rently, calcium hypochlorite is mainly
produced from slaked lime and so-
dium hydroxide. Figure 2 presents dif-
ferent pathways for calcium hypochlo-
rite production.
Economic performance
The total operating cost (raw materi-
als, utilities, fixed costs and deprecia-
tion costs) estimated to produce cal-
cium hypochlorite was about $1,120
per ton of calcium hypochlorite in the
fourth quarter of 2013. The analysis
was based on a plant with capacity to
produce 25,000 metric ton per year of
calcium hypochlorite.
This column is based on Calcium
Hypochlorite Production via Sodium
Method Cost Analysis, a report
published by Intratec. It can be found
at: www.intratec.us/analysis/calcium-
hypochlorite-production-cost. n
Edited by Scott Jenkins
Editors note: The content for this column is supplied by In-
tratec Solutions LLC (Houston; www.intratec.us) and edited by
Chemical Engineering. The analyses and models presented are
prepared on the basis of publicly available and non-confidential
information. The content represents the opinions of Intratec only.
More information about the methodology for preparing analysis
can be found, along with terms of use, at www.intratec.us/che.
1. Caustic mixing vessel
2. Lime mixing vessel
3. Salt nucleator vessel
Off-gas
4. Chlorinator
5. Elutriator
6. Salt centrifuge
7. Calcium hypochlorite centrifuge
Wastewater 9. Turbo dryer
10. Crusher and classifier
11. Scrubber
12. Steam boiler
13. Cooling tower
14. Chiller
12

13 ST Steam
CW
CW Cooling water
FIGURE 1. This flow diagram depicts a typical sodium process for production calcium hypochlorite RW 14 RW Chilled water

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 29

 Cover Story

Confronting
Crystallization Issues
Reliable information about industrial crystallization can be difficult to find and to apply to new
situations. The work process outlined here will help engineers approach crystallization challenges

P
Brooke Albin and roject and plant engi-
Charles Moyers neers frequently face
MATRIC issues with crystal-
lization processes,
but often possess little prior
experience to address them.
IN BRIEF In probing for answers, engi-
INVESTIGATE SYSTEM neers often discover that reli-
BASICS able prediction of equipment
WHAT CAN BE LEARNED
capacities from machine ge-
IN THE LABORATORY? ometry and physical proper-
ties of liquids and solids is
ACCURATE PHASE- improbable, and that most
EQUILIBRIUM DATA of the literature describing
SELECTION OF A crystallization and separation
CRYSTALLIZATION equipment is confusing. They
SCHEME are also likely to find that fea-
LABORATORY
sibility and scaleup correla-
CRYSTALLIZATION TESTS tions are based primarily on
empirical know-how devel-
CRYSTAL MORPHOLOGY oped by crystallization equip-

PILOT PLANT TESTING ment users and manufactur-

ers. Given that, how should
TROUBLESHOOTING
engineers proceed toward
CLOSING THOUGHTS obtaining a reliable and eco-
nomic solution to their current
cystallization problem?
Using the work process
outlined in this article can help
guide engineers in approach-
ing crystallization process
problems. This includes devel-
oping a strong understanding FIGURE 1. Particle morphology is an important parameter
of the systems solubility data, for crystallization processes
conducting laboratory tests to
gain hands-on experience with a material needs, distillation is usually considered first.
and setting up a pilot-scale system. However, distillation may not be practical
because of azeotrope formation, low relative
Investigate system basics volatilities of the components to be separated
It is important to first understand why crystal- or other reasons. Sometimes, materials are
lization could be an appropriate separation unstable at high temperatures, which might
method and which types of crystallization prohibit using distillation. Crystallization is a
are available. For separation or purification good fit for some of these applications.
30 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
 Crystallization is used industrially to create
a particulate solid phase (product), which
is recovered and purified by washing and
drying. Sometimes the solid product is a
waste product, but more often, the product
is a valuable commodity. Crystallization falls
into two main categories: solution crystalli-
zation and crystallization from the melt (also
referred to as fractional crystallization).
Solution crystallization implies that material
is crystallized from a mixture containing a
solvent. Crystals are formed by either con-
centrating the desired component by solvent
evaporation or cooling or both, and the solid
phase is typically formed at a temperature
well below its freezing point. In melt crystalli-
zation, crystals are generated by cooling the
solution, and are recovered at temperatures
near the pure component freezing point. The
melt crystallization product is recovered as a
liquid, and particulate solids processing can
largely be avoided. This can be helpful if the
product is preferred in liquid form.

What can be learned in the laboratory?

When evaluating the feasibility of crystalli-
zation as a separation technique for a new
process, small-scale testing can provide
valuable insight. Significant development
work can be accomplished in the labora-
tory at this early stage. Using solubility in-
formation, a basic process scheme can be
proposed and tested. Often, through this
work, the type of crystallization technique
to be used, as well as operating conditions,
are defined. Furthermore, the number of
crystallization stages required and an ap-
propriate solid-liquid separation technique
can all be determined at laboratory scale.
Conducting small-scale crystallization tests
also allows a first look at crystal morphol-
ogy (Figure 1) and particle size distribution,
and provides a framework for estimating
product purity and yield.
In addition, in existing commercial crystal-
lization processes, sometimes troubleshoot-
ing is needed to resolve an issue, or re-design
is needed due to changes to the process,
such as increasing production capacity or
switching to a new feedstock with different
types or concentrations of impurities. Typi-
cally, for these scenarios, there becomes a
need for either increased yield, quality or ca-
pacity for the crystallization operation.
For existing processes, it often makes
sense to do off-line testing at smaller scale.
This enables the investigators to gain a
deeper understanding of problems, since it
is usually simpler to change conditions as
well as deal with potential solids handling FIGURE 2. Laboratory-scale
issues in small-scale equipment. Moreover, testing of crystallization pro-
cesses can give investigators
good qualitative observations can be ob- valuable information about
tained by working with smaller equipment. how to address problems at
For example, using glass crystallizers, which larger scales
are readily available for laboratory-scale
work, can provide a real advantage. Also at
this scale, the cost of raw materials is much
lower. Downtime can be minimized, since,
in many cases, the commercial process can
continue to operate while improvements are
being made independently. Figure 2 shows a
laboratory crystallizer unit.
Accurate phase-equilibrium data
Regardless of what may be the specific
focus or objective of the development or
troubleshooting work involving crystalliza-
tion, reliable solubility data are essential. Ob-
taining accurate solubility curves or phase
diagrams is a critical first step. Theoretical
freezing curves can be generated using the
Vant Hoff equation, if the pure component
melting point and heat of crystallization are
known [Equation (1)].

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 31

 Cover Story
20.0 a pure sample of component A or B will
crystallize. At the eutectic point, both com-
10.0 ponents will crystallize together at the given
composition, such that separation (or purifi-
Desired
0.0 cation) is not possible. This point represents
Freezing temperature (C)

component A

urv
e the conditions at which the maximum yield
c Undesired
-10.0 can be achieved.
rium component B
u ilib Consider a scenario where the solution
eq Solidus line
-20.0 uid is cooled. As the solution is cooled to 0C,
d-liq Liquid + solid A
Soli solids begin to form, and the solution com-
-30.0 position shifts accordingly to become less
Liquid + solid B
concentrated in component A. Thus, fur-
-40.0 ther cooling is necessary to continue crys-
Solid A + solid B tallization. As the temperature is lowered,
-50.0 pure crystals of component A will theoreti-
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 Mass fraction A
1.0 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0.0 Mass fraction B
cally form until the solution is cooled to its
Eutectic point eutectic point, shown at 40C in the figure.
80% feed
2:1 B:A From this curve, given the starting composi-
FIGURE 3. The phase diagram Vant Hoff Equation: tion and the final temperature, the theoreti-
shown here presents solid- cal product yield and the remaining solution
liquid equilibrium data for
a two-component eutectic (1) (known as mother liquor) composition can
system be calculated.
Where x2 is the solubility mass fraction, Hf Using the same example, say the final
is the crystal heat of formation, R is the gas crystallizer temperature is 35C. After solids
constant, T is saturation temperature, and removal is complete, the remaining mother
TM is the melting point temperature. liquor still contains about 40 wt.% of com-
With this approach, freezing temperature ponent A, and 60% component B. The theo-
versus concentration is plotted to construct retical product yield for this case is found by
a phase diagram. While theoretical solubil- doing a material balance, which simplifies to
ity curves can be calculated, it is preferred the following Equation (2), where x1 is the
to ascertain the solubility of the system ex- feed mass fraction of component A, y1 is the
perimentally. At the least, it is recommended feed mass fraction of component B, x2 is the
that several data points from the calculated final mass fraction of component A, and y2 is
curve be verified in the laboratory, since real- the final mass fraction of component B.
ity often differs from what is calculated theo-
retically, or even from what is reported in the % yield = [(x1 (x2 y1)/y2 )]/x1 100 (2)
scientific literature.
A good approximation of solubility can be For the given example, the resulting yield of
determined quite easily in the laboratory. It is component A is calculated to be 83.3%.
essential to have a reliable temperature mea- For this type of two-component system,
surement device and an accurate method for the data are used to compute a chart that
quantifying the composition of the solution. combines product yield and total solids in
First, a slurry of the solids suspended in so- suspension (TSS) as a function of tempera-
lution is prepared and held at a stable tem- ture and initial feed concentration. The chart
perature for a length of time sufficient for it to organizes the overall material balance for the
equilibrate. Then, a sample of the saturated system and serves as a basis for preliminary
mother liquor is taken while either filtering out evaluation of product yield as a function of
solids, or after allowing them to settle. The process variables. Development and use of
saturated solution is analyzed to determine this chart narrows the choices available for
its equilibrium composition. A curve can be zones of probable operation and also pro-
generated by repeating the procedure over a vides guidance regarding necessary staging
range of temperatures. of the process. A typical yield chart is pre-
The phase diagram depicted in Figure 3 sented in Figure 4.
shows solid-liquid equilibrium data for a bi- This has proven to be a valuable tool for
nary (two-component) eutectic system. The quickly estimating the yield that can be ob-
freeze curve indicates the temperature at tained with a given feed concentration and
which a solid begins to crystallize from a so- operating temperature. The value for TSS is
lution with the corresponding composition. also included for consideration, since there
It shows the range of conditions at which is a practical upper limit that should be ob-
32 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
 100
90
80
70
Products yield, %
60
50
40
30
20
10
0
-40 -30 -20
Saturation temperature, oC
FIGURE 4. This yield chart shows yield as a function of crystallizer temperature and total solids in sus-
pension (TSS)
served in order to end up with a
slurry stream that is manageable
and can be pumped and transferred
without plugging. The operating TSS
is usually the highest TSS with which
the equipment can comfortably op-
erate. This level often ranges from
30 to 40% TSS.
For the example above, wherein
the feed contains 80% of the de-
sired product, component A, and
20% of the undesired component
B, a maximum of ~87% yield can
be obtained. To reach this maxi-
mum, cooling to 40C is necessary.
However, if cooling were completed
in only one step, the slurry den-
sity would be exceedingly high. At
greater than 60% TSS, it is unlikely
that this slurry could be processed.
Thus, splitting the process into mul-
tiple steps is probably required.
To reach the maximum yield, but
limit slurry density to less than or
equal to 40%, it will be necessary to
have three stages of crystallization,
as follows:
1. In the first stage, 80% feed is
cooled from its initial temperature
to roughly 10C. Crystals begin to
form at 0C and continue to build
up until they reach 40% TSS as the
solution is cooled to 10C. Nearly
50% yield is achieved in the first
stage. The crystals are removed via
an appropriate solid-liquid separa-
tion step and the mother liquor con-
tinues to the next stage.
2. In stage two, the mother liquor
from the previous stage contains
roughly 65% solute (desired compo-
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
50% feed
60% feed
70% feed
60% TSS 80% feed
PROCESS
50% TSS 90% feed
95% feed
PLANTS FOR
40% TSS
30% TSS
20 % TSS
-10 0 10.0
nent A). This becomes the feed for
stage two. Since its saturation point
is 10C, cooling below this point
will trigger the formation of solids.
The final temperature will be 30C,
which corresponds to the maximum
40% TSS. Approximately 60% of the
product contained in the stage-two
feed is recovered in this step (that is,
60% of the remaining 50% from step
one is recovered), bringing the over-
all yield to about 80%.
3. The third stage is necessary for
obtaining the maximum yield, which
will be reached at just above the eu-
tectic point (40C). Often, it is not
worth approaching conditions too
near the eutectic, where impurities Hydrogenation
are more likely to solidify.
It is important to note that, often, Solids blending / drying
systems do not behave according to
theory. For instance, the solid-liquid Pharma, food, cosmetics
equilibrium state may not be easily
achieved by simply cooling to equi- Finechemicals
librium temperature. The region of
conditions where a solution is stable
below its equilibrium line is referred
to as the metastable zone. When op-
erating in the metastable region, the
solution is supersaturated, but crys- Your fast lane to
tals do not form. For a system with a advanced mixing technology:
large metastable zone, considerable
sub-cooling or seeding (the addition Phone: +1 201 825 4684
of fine crystals as nucleation points) Ext.: 205
will likely be necessary to trigger nu- usa@ekato.com
cleation of the dissolved solute.
Crystallization scheme selection
Selecting the operating mode for www.ekato.com
crystallization is dictated by labora-
tory evaluation and desired product
For details visit adlinks.chemengonline.com/66434-09
NOVEMBER 2017 33
 Cover Story
lization is used when a very low operating
temperature is required in order to achieve
good product yields or due to reactivity or
degradation at higher temperatures.
In addition, evaporative cooling (also
known as vacuum cooling or vacuum crys-
tallization), a hybrid process that achieves
cooling by evaporation at sub-atmospheric
pressure, can be considered when solubility
has a moderate dependence on tempera-
ture. It offers the advantage of low oper-
ating temperatures relative to evaporative
crystallization, while avoiding fouling on
cold surfaces.
Melt crystallization is a less common and
more specialized technique that is capable
of producing extremely high product purity,
and it can be useful when a liquid product is
acceptable. When melt crystallization is pos-
sible, it offers the benefit that solids handling
operations can be avoided, and the associ-
ated separation and drying equipment is not
necessary. One limitation is that the product
must be able to be handled at its melting
point. If a material is either unstable at its
melting point or its melting point temperature
is very high or very low, such that process-
ing at that temperature is impractical, melt
crystallization is not a possible solution. An
example of a laboratory melt crystallizer is
presented in Figure 5.

Laboratory crystallization tests

FIGURE 5. The equipment
shown here is a laboratory-
scale falling-film melt crystal-
lizer
34
form. However, determining whether to use
evaporation, cooling, or some combination
of both can often be accomplished even
before testing begins. The phase diagram
and yield charts can prove quite useful in se-
lecting a preliminary crystallization scheme.
Studying the phase diagram is a good place
to start. When solubility is not significantly
affected by changes in temperature, evap-
orative crystallization is a likely candidate.
Most commonly, commercial crystallization
processes incorporate evaporative crystal-
lization, and often, multi-effect evaporation
or vapor recompression is utilized to reduce
energy demand.
Conversely, cooling crystallization can be
effective when the solid-liquid equilibrium
is strongly dependent on temperature. Al-
though cooling crystallization is simpler, it is
associated with more fouling problems due
to formation of encrustations on cold sur-
faces and is often avoided. Yet, sometimes
cooling crystallization is necessary, such as
for processing materials with very high boil-
ing points. In other cases, cooling crystal-
CHEMICAL ENGINEERING
Once a recovery chart has been assessed
and a preliminary crystallization scheme has
been selected, actual crystallization tests can
be carried out in the laboratory using authen-
tic or synthetic process solution. These tests
are used to verify that the scheme and condi-
tions that were selected are appropriate and
will provide valuable practical experience re-
garding processing of the given feed stream.
During crystallization tests, both ease of
nucleation and crystal growth are observed,
which helps to determine a practical cooling
or evaporation rate. Cooling or evaporation
must be approached so that solidification
occurs slowly enough to grow crystals of
adequate size and purity. Either cooling or
evaporating too aggressively can lead to fine
crystals crashing out of solution or encrusta-
tion on cold or hot surfaces due to localized
high supersaturation. Suitable crystallizer
residence times can be estimated based on
the time needed for sufficient crystal growth.
Solid product is recovered by some means
of solid-liquid separation. Laboratory-scale
pressure filters and basket centrifuges are
available, and are convenient for these early
WWW.CHEMENGONLINE.COM NOVEMBER 2017
studies. Product purity is measured by an
appropriate analytical method, such as gas
chromatography (GC) or high-pressure liquid
chromatography (HPLC), and yield can be
calculated. Particle shape (habit) can be de-
termined using microscopy, and a number of
analytical methods are available for perform-
ing particle size analysis. One simple method
for measuring particle size distribution uses
a sonic sifter to separate product crystals
based on their ability to pass through a stack
of sieves with gradually decreasing screen
size (known as sieve analysis). The average
size and mass for each group of particles is
determined, and the data are plotted for a
visual representation of crystal size.
Typically, it is premature to do product-
purity studies at this stage, but conducting
product recovery and washing tests are use-
ful for understanding how easily desired yield for removing residual mother liquor from a FIGURE 6. This photomicro-
and purity can be obtained. solid crystalline product. By incorporating a graph image shows crystal
platelets in various stages of
In practice, crystals that are recovered few sequential wash steps, the bulk of the growth
from the mother liquor are rarely 100% pure. mother liquor can be effectively removed.
Impurities are expected to be present due Nonetheless, washing must be optimized to
to occlusions (when impurities are physically improve purity with a minimal loss of yield,
trapped inside the crystal lattice), inclusions since some dissolution of crystals will cer-
(when impurities are incorporated into the tainly occur.
crystal structure), and due to imperfect solid- During this step in testing, recommenda-
liquid separation. Any solid-liquid separation tions can also be made regarding seeding.
technique will leave behind some amount of Sometimes nucleation for solid formation
impurity-containing mother liquor. In some can be achieved solely by controlling tem-
cases, adjusting the solid-liquid separation perature. In other situations, seeding may
technique can result in better removal of im- be required, and even agitation can play a
purities, giving a better outcome. Another role. Seeding is often necessary when the
common option is to perform washing of metastable zone is large, such that the so-
the crystals. Washing is a standard method lution endures significant supersaturation

Integrating eiciency.
Maximizing safety.
Enabling digitization.
Hall 7A
Booth 330
Mobile Communication and Safety

Exploring mobility-our goal is maximizing the

potential of networked mobile devices in hazardous
areas to open up new possibilities for our customers.
Experience our Mobile Worker concept and discover
how you can make your processes safer and more
eicient with innovative, complete solutions.

Learn more at www.ecom-ex.com

For details visit adlinks.chemengonline.com/66434-19

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 35

 Cover Story
before nucleation. An appropriate seeding
technique can prevent large amounts of fine
crystals from crashing out of solution, versus
growing fewer larger crystals that are easier
to filter and transport. Often this must be
done carefully so that crystals begin to form
and grow in such a way as to produce the
desired crystal size.
Crystal morphology
Crystal morphology is an aspect of crys-
tallization that can have a major impact on
processing. Moreover, it is not a variable that
is easily manipulated. Usually for industrial
processes employing crystallization, there
is little concern with specific morphology as
long as the particles filter well (without exces-
sive plugging) and can be transferred easily.
However, when certain crystal shapes, such
as needles, are present, serious handling
problems can occur. In these instances,
filters can blind off quickly, and settling of
particles may be slow. Needle-shaped crys-
tals may also be more prone to breakage.
When crystal morphology hinders operation,
production capacity may be significantly af-
fected, and downstream processing often
must be modified to compensate for slower
and less efficient solid-liquid separation.
When presented with any crystallization problem, it is important to begin with a strong
understanding of the systems solubility data. Careful assessment of solubility curves
and yield charts . . . can provide valuable insight into the root cause of an issue, as well
as potential solutions
Crystal size is also a concern, but offers
more possibilities for control. With an ap-
propriate seeding technique, a reasonable
cooling rate, and adequate residence time,
a manageable crystal-size distribution can
often be attained.
Attrition of crystals is known to occur, and
can be a particular challenge for some frag-
ile solid materials. When crystal breakage is
severe, particle size can decrease to such
an extent that solid-liquid separation is im-
pacted. In this case, measures to improve
handling procedures are necessary. Attri-
tion can be mitigated by using a moderate
flowrate and a pump design that is suited for
gently handling slurries. When these controls
are unable to produce the desired size, spe-
cialized crystallizer designs intended to grow
large crystals can be tested by collaborating
with crystallizer equipment vendors.
A simple light microscope is useful for
36 CHEMICAL ENGINEERING
studying crystal shape and size. An exam-
ple of a photomicrograph of a crystal prod-
uct sample taken with a light microscope is
shown in Figure 6. With this tool, engineers
can track the appearance of crystals with
response to changing process variables.
Observation with a microscope can reveal
changes in habit that result from the pres-
ence of various impurities. It allows compari-
son of crystals before and after washing to
see any notable improvements. In addition, it
provides a look at crystal breakage (attrition)
that could result from processing.
Pilot plant testing
Pilot-scale operation also serves an impor-
tant purpose in the development of a new
process, and is a good tool for troubleshoot-
ing. A crystallization pilot plant minimizes risk
of scaleup by using equipment that is geo-
metrically similar to commercial equipment,
and is used to obtain reliable engineering
design data. Process recycles are often in-
corporated at pilot scale, and this can be
extremely important in refining the material
balance and verifying the crystalline product
purity that can be achieved. Furthermore, pi-
lot-scale crystallizers are able to accommo-
date production of larger quantities of prod-
uct material to use for market testing and
development. Testing of scalable solid-liquid
separation and drying equipment is often
conveniently conducted in the pilot unit.
Process optimization
There are three primary objectives in com-
mercial crystallization processes: achieving
product purity, yield and capacity. While it
is desirable to maximize each of these vari-
ables, in reality, when one of these is pushed
too far, the other variables will be negatively
impacted. Thus, prioritization is necessary to
develop a crystallization process with an op-
timum balance among these elements.
In cases where higher purity (better quality)
is desired, multiple methods can be investi-
gated as potential routes for improvement.
Sometimes, (as mentioned above), a better
solid-liquid separation is needed, to sepa-
rate the impurity-containing mother liquor
WWW.CHEMENGONLINE.COM NOVEMBER 2017
away from a solid product. Other
times, this can be accomplished by
changing the solid-liquid separation
technique. A new type of centrifuge
or filter may be beneficial. Adjusting
the washing procedure might give
rise to incremental improvements as
well. In still other cases, the crystals
are small, and growing larger crys-
tals can help improve solid-liquid
separation. Yet another factor influ-
encing purity is the rate of crystalliza-
tion. In general, slower crystallization
yields a better quality product. When
all else fails to produce the target
purity, recrystallization of a first stage
product could be a solution.
When a higher yield is needed, the
approach might also include grow-
ing larger crystals or selecting an-
other solid-liquid separation device
to decrease the loss of solids. Incor-
porating recycle streams might also
be a way to increase overall yields,
since the product contained in the
saturated mother liquor has another
opportunity to undergo crystalliza-
tion. For certain systems, concen-
trating the crystallizer feed or cooling
to a lower temperature might be an
option to improve yields, but when
slurry density (solids in suspension)
becomes too high, solids handling
issues can be a challenge. It may be
necessary to add an additional crys-
tallizer stage to manage the higher
mass of solids.
For boosting production capacity,
more effective heat transfer is usu-
ally the answer. This allows the crys-
tallizer to accommodate a higher
feedrate, which in turn, decreases
the residence time. As a result, par-
ticle size may decrease, and purity
follows suit. Thus, increasing capac-
ity must be approached with regard
to the proper balance of capacity
versus yield and purity. However,
engineers can attempt to compen-
sate by improving washing or solid-
liquid separation, or both.
Closing thoughts
It is more efficient to make the effort
to understand an issue and solve
problems early in process develop-
ment than after a poor design is in
place. Nonetheless, in many situ-
ations, issues must be solved at a
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
later stage. In either case, following
the work process outlined in this ar-
ticle is an effective way to approach
the matter.
When presented with any crystal-
lization problem, it is important to
begin with a strong understanding of
the systems solubility data. Careful
assessment of solubility curves and
yield charts, as covered in this article,
can provide valuable insight into the
root cause of an issue as well as po-
tential solutions before proceeding
to experimental testing. Laboratory
tests provide the basis to work out
the fundamental design and operat-
ing conditions of the system. There
is no substitute for gaining hands-on
experience in working with a specific
material and directly observing the
crystallization process. This often re-
veals characteristics that can impact
processing, but are subtle and might
not be appreciated otherwise.
Once the basic process design
has been established and opera-
tion is reasonably well-understood,
a pilot plant is recommended to de-
fine recycle schemes and to gather
scaleup data before finally imple-
menting at commercial scale. n
Edited by Scott Jenkins
Authors
Brooke Albin is a project man-
ager at MATRIC (Mid-Atlantic
Technology, Research and Inno-
vative Center; 1740 Union Car-
bide Drive, South Charleston, WV
25303; Email: brooke.albin@
matricinnovates.com; Website:
www.matricinnovates.com). In
this role, she is responsible for
the coordination and execution of
research and development (R&D) activities for numer-
ous clients. She has 10 years of experience in develop-
ment of new processes to produce chemicals from
biofeedstocks, and has specialized skills in the area of
solids handling and crystallization. She received her
B.A. in chemistry and B.S. in biology from Alderson-
Broaddus College, and earned her M.S. in chemical
engineering at West Virginia University.
Charles Moyers is a senior engi-
neering scientist at MATRIC (Mid-
Atlantic Technology, Research
and Innovative Center; same ad-
dresss as above; Email: charles.
moyers@matricinnovates.com;
Website: www.matricinnovates.
com). He is a fellow of AIChE and
has co-taught several AIChE edu-
cation courses, including Indus-
trial Crystallization, Liquid-Solid Separation, and Dry-
ing. He holds a B.S. from Virginia Tech, an M.S. from
West Virginia University and a Ph.D. from the University
of Delaware, all in chemical engineering.
For details visit adlinks.chemengonline.com/66434-12
NOVEMBER 2017 37
 Cover Story

Industrial Crystallization
for the CPI
This overview presents the traditional and emerging types of continuous crystallizers

C
Michel Malfand rystallization is an impor- Vapors
Crystal Evap Consult tant technique for the
purification of solids in
the chemical process in-
dustries (CPI). The operation can
be performed batchwise or in con-
IN BRIEF tinuous operation, and is used for
GENERATING a wide variety of products, rang-
SUPERSATURATION ing from sugar, salts and other bulk Suspension of crystals
TYPES OF chemicals, to pharmaceuticals and
CRYSTALLIZERS other fine chemicals.
This article provides an overview
CHOICE OF A of the most important types of con-
FLOWSHEET
tinuous crystallizers, with a brief sum-
mary of the pros and cons of each
type (for more on crystallization pro- Steam
cesses, see part 1 on pp. 3037). Slurry to centrifuges

Generating supersaturation TR

Crystallization from solution is done

by creating a supersaturated solution
Condensates
of the product in the solvent. Creating
the supersaturation condition can be
achieved by any (or a combination) of
the following methods:
Evaporation Feed Circulation pump
Cooling (adiabatic)
FIGURE 1. A forced circulation (FC) crystallizer circulates a slurry through
Cooling (surface) an external heat exchanger, usually with an axial flow pump
Cooling (by gas injection)
Reactive transport disengagement height (TDH)), and
Anti-solvent addition one vessel (the crystallizer-vapor separator).
pH adjustment The FC can also be equipped with an elutri-
ating leg, which is used to improve the coeffi-
Types of crystallizers cient of variation (CV) by removing the coars-
For continuous operation, the main crystalliz- est solids in the system. The heat exchanger
ers in operation in the CPI include the follow- can be vertical or horizontal. The circulation
ing (for more details, see Ref. 14): rate in the heat exchanger tubes is usually
Forced circulation (FC) between 6 and 8 ft/s, and temperature rise
Draft tube baffle (DTB) (TR) across the heat exchanger is 4 to 6F (or
Oslo less than 1F for surface cooling).
Indirect forced circulation (IFC) The FC shown in Figure 1 employs a cen-
Forced circulation (FC). An FC crystallizer tral inlet, but many designers are still using
(Figure 1) consists of a single heat exchanger, tangential or radial inlets.
a circulating pump (usually an axial flow FC crystallizers can be used as an evap-
pump, which permits large flow and small orator-concentrator when the product to
38 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
 Vapors
concentrate is incrusting the heat exchange
surface (for example, for phosphoric acid
and gypsum) and as a crystallizer (for ex-
ample, for sodium chloride, sodium sulfate
and sodium carbonate).
FC is most commonly used as an evapora-
tor and crystallizer, and can also be used as a
surface-cooled crystallizer, adiabatic-cooling
crystallizer or reactive crystallizer. In addition, Overflow
it can be used for viscous products (such as Feed Delta TR
citric acid anhydrous or mono hydrate). Steam
The washing cycles are usually performed
monthly, if the tubes are correctly submerged.
Crystals produced in an FC are usually Slurry to centrifuges
small (150400 microns) with a large CV
(5060%), but such crystals are sufficiently Condensates Slurry

large to be separated by a pusher-type cen-
trifuge (salt with 3% moisture is usual).
The crystal size distribution (d50) in an FC
crystallizer can be improved by achieving the
right balance between primary nucleation
and secondary nucleation [1]. Increasing the
retention time will also increase the the sec-
ondary nucleation [2].
Draft tube baffle (DTB). A DTB crystallizer
(Figure 2) has an internal circulation that is
performed by an agitator instead of a pump.
The low speed agitator permits a reduction of
the secondary nucleation and increases the FIGURE 2. A draft-tube baffle
size of crystals, a feature that gives the DTB a (DTB) crystallizer uses an
agitator to generate internal
reputation for producing large crystals. circulation
The DTB is equipped with baffles, which
permit the system to operate as an evapo-
rative crystallizer. The baffles are often ref-
ered to as fines killers because they destroy
fine crystals, enabling the production of
larger crystals.
DTB is largely used as an adiabatic cool-
ing crystallizer, for producing salts, such as
potassium chloride, boric acid and other bo-

A Guide to Advanced and Next-Generation

Battery Technology and Materials

This comprehensive guidebook

provides descriptions of the Availability from stock
major battery technologies
and materials in the advanced
and next-generation
battery markets, as well as
information on many of
the companies operating
in the advanced and
next-generation battery
industries.
Corrosion resistant pipes
Included in this guidebook is a table that BUTTING stores ordinary 5 000 t welded pipes with euro-
represents a list of selected technology- pean origin in more than 140 different sizes, from DN 15 to
development companies in the advanced DN 800, in 15 different material grades according to
batteryspace, along with their areas of focus, DIN EN, ISO and ASTM.
contact information and technology status.
We have also specialised in the production of special ma-
Itlists both established companies and startup
terials and nickel alloys for more than 35 years.
companies that have made technologicalstrides
in recent years toward commercially viable BUTTING Group
battery technologies. Michael Frstenberg
28014
Phone: +49 5834 50-408
Learn more at store.chemengonline.com michael.fuerstenberg@butting.de www.butting.com

For details visit adlinks.chemengonline.com/66434-13

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 39

 Cover Story
Downcomer
Slurry to centrifuges
FIGURE 3. An Oslo crystal-
lizer was designed to produce
large crystals
FIGURE 4. In an indirect
forced circulation (IFC) cystal-
lizer, large crystals do not
make contact with either an
agitator or a circulation pump
Small crystals
Steam
Heater
Condensates
40
Vapors crystallizer, and was first developed specifi-
cally to produce large sodium chloride crys-
tals. As with the FC crystallizer, the Oslo has
an external recirculation loop, one heat ex-
changer and one fluidized-bed vessel. How-
Clear liquid
ever, the Oslo crystallizer recirculates a clear
liquid instead of a slurry, as in the FC. There
is no secondary nucleation, and normally
there is no limit for the size of crystals.
Feed Usually Oslo crystallizers are installed with-
out a leg and without fine killers.
Steam The Oslo crystallizer has one technical dis-
advantage: short washing cycle (due to en-
TR crustation of the downcomer). The price can
also be high compared to a DTB. Despite
these shortcomings, new Oslo crystallizers are
still being used today.
Condensates
Indirect forced circulation (IFC). The IFC
is a relatively new type of continuous crystal-
lizer that uses a different hydraulic concept
rates, or as a reactive crystallizer, for produc- (Figure 4). Only medium-sized crystals come
ing ammonium sulfate. into contact with the agitation device; the
The TR in a DTB is very small (0.52F) and larger crystals are indirectly circulated with-
again it is necessary to find the good com- out making contact. To increase the crystal
promise between primary and secondary nu- size, the system can be equipped with a leg
cleation to achieve the best size distribution. and, if necessary, a fines killer. The d50 in an
Usually DTBs are not installed with a leg. IFC is 23 times higher than achieved in an
Oslo or crystal growth. The Oslo crystal- FC, and the CV is around 20%, compared to
lizer (Figure 3) is the oldest type of industrial 4050% for the FC and DTB.
Vapor
Design of a new crystallizer
Indirect forced For a new product, or a new application, the
circulation IFC
question to be asked is, what is the best de-
sign? To answer this question, the designer
needs to know the following:
Crystallizer Option Partial fines Physical data
destruction
Solubility curves
Steam
Specific gravity and heat capacity of
Fines liquid and solid
Heat of crystallization
Viscosity and boiling-point elevation
Condensates of the liquid
Market requirements for the product
Purity
Crystal size distribution (CSD)
Moisture
Temperature limitations
Quality of condensates
Small and larger Utilities available
crystals
Steam
Electricity
Larger crystals
to centrifuge Cooling water
Chilled water
What are the habits of the market for the
application (type of crystallizer and arrang-
ment generally used for this application)?
Multiple effect? mechanical vapor re-
Milling device
compression? thermo compression?
Feed
Evaporative? or adiabatic cooling? or
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
 reactive? or surface cooling ?
Other parameters
Flexibility
Operability and operators training
Maintenance
For new applications, it is often neces-
sary to perform laboratory tests to con-
firm the physical data (first bullet above),
followed by pilot tests to verify the crys-
tallizability and the characteristics of the
crystallized product.
One of the benefits of the IFC crystal-
lizer is that laboratory and pilot tests are
fully representative of the product pro-
duced in an industrial plant. This is not
necessarily the case for a DTB crystal-
lizer, because the crystal size is affected
by the tip speed of the agitator that gen-
erates secondary nucleation.
Choice of a flowsheet
More and more, several types of crys-
tallizers are associated with additional
equipment, such as the following:
Preconcentration (falling film, plate and
other types of concentrators)
Vapor condensation (surface or mixing)
Vacuum equipment (ejectors, vacuum
pumps or combined systems)
Vapor compression
Chilled water
Meshes, catchalls and treatment of
vapors
Solid-liquid separation (hydrocyclones,
settlers, legs, pusher centrifuges, solid
bowl centrifuges, filters and so on)
Over time, the flowsheets used for in-
dustrial applications are evolving to take
into consideration the needs of the mar-
ket and the new material of construction
available, so that for each application,
there has emerged something like a stan-
dard. Some examples are given below.
Salt in caustic soda. A first example is
the concentration of caustic soda from
a diaphragm electrolyzer, with salt crys-
tallization in a triple-effect FC crystalliz-
ers (in pure nickel). It took more than ten
years to arrive at the final flowsheet. Ini-
tial static decanters are now replaced by
elutriated legs.
Potassium chloride. For a long time,
KCl crystallization has been done in adia-
batic cooling DTB crystallizers (up to
seven stages).
Ammonium sulfate. (NH4)2SO4 is a by-
product from many sources, primarily
from the production of caprolactam and
methyl methacrylate, but also from waste
ammonia or sulfuric acid solutions. Over
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
the last 1015 years, DTBs are replacing
Oslo crystallizers for this application, but
some end users continue to make large
investments with Oslo crystallizers today.
Sodium chlorate. NaClO3 is produced by
electrolysis of NaCl. Typically, electrolyte
leaving the cells at 85C is sent to a DTB
evaporative crystallizer. For many decades,
the crystallization was done at 30C, which
required steam for evaporation and chilled
water or steam for boosters.
In the mid 1980s, the author and J.C.
Studler developed a new flowsheet in
which no steam and no chilled water are
required, by operating between 3045C,
and recovering the heat of the cells. This
flow sheet is now a standard.
Sodium sulfate. Na2SO4 is produced from
mines in Spain, Turkey and other countries
by water injection. It is also a byproduct of
many different processes in the CPI.
The main use for Na2SO4 is for laundry
detergent, and therefore it is necessary that
the product be very white. Normally, a first
crystallization as glauber salt is required
Today, most crystallizers for this ap-
plication are FC crystallizers, which pro-
duce crystals with a d50 of 180200 m
and a large CV. One plant in Spain has
installed a DTB crystallizer, giving crystals
that seem larger than those produced by
the FC crystallizer, but in fact, agglomer-
ates are being produced.
One plant in France has installed an
IFC crystallizer giving 300 m monocrys-
tals with a CV of 2025% and less than
4% fines at the outlet of the dryer. For this
application IFC is the new standard. n
Edited by Gerald Ondrey
References
1. Genck, W., A clear view of crystallizers, Chem. Eng. July 2011,
pp. 2832.
2. Mullin, J.W., Crystallization, 4th ed., Butterworth-Heinemann,
Burlington, Mass., 2001.
3. Gallot, J.C. and Schur, A., Crystallizers and Agitators, Chem. Eng.,
December 2006, pp. 3841.
4. Randolph, D. and Larson, M.A., Theory of Particulates Pro-
cesses, Academic Press, N.Y., 1968.
Author
Michel Malfand is president of Crystal
Evap Consult (42 Bd Risso, 06300 Nice,
France; Telephone:+33-4-9331-0075;
Email: michelmalfand@aol.com), and a
consultant on evaporation and crystalli-
zation. Malfand is the inventor of the indi-
rect forced circulation (IFC) crystallizer,
which is patented around the world. He
has been with the company since 2004.
Prior to this, he has worked at Applexion
(for 3 years), Agrochem (12 yrs), and Swenson (18 yrs). He
studied chemical engineering at HEI (cole des Hautes tudes
dIngnieu) in Lille, France.
NOVEMBER 2017 41
 Feature Report

Cooling Towers:
Keeping Your
Power Plant Cool
General guidelines for selecting the appropriate power-plant cooling system are presented here

T
Luc De Backer he main purpose
Hybrid
Enexio US of a power plant is
to convert a source
of energy into elec-
IN BRIEF tric power. Most power

Wet
Dry

HEAT SINK AND COOLING plants rely on heat as the

SYSTEMS energy source (thermal
power plants). Thermal
CLOSED-CYCLE
power plants burn fossil 0 10 20 30 40 50 60 70 80 90 100
SYSTEMS Water requirements, %
fuel (coal, oil or natural gas)
WET COOLING SYSTEMS or use nuclear fission, and FIGURE 1. Closed-cycle cooling systems can be classified by the water requirements

DRY COOLING SYSTEMS are based on the principle of heat engines. fore related to the conversion efficiency and
An engine is a thermodynamic cycle that the steam turbine output.
HYBRID COOLING produces a net power output by supply-
SYSTEMS ing heat from a high temperature reservoir Heat sink and cooling systems
SELECTION: (heat source), and rejecting heat to a low The heat sink is one of the major compo-
DRY VERSUS WET temperature reservoir (heat sink). nents in the steam cycle, and its major pur-
The heat sink is a fundamental element of pose is to reject the heat duty of the steam
any thermodynamic cycle in an electrical- condenser to the atmosphere. The cooling
power-generating plant. The point of in- system performance is directly related to
teraction between the plant cycle and the the steam turbine backpressure, which
heat sink is usually the main condenser. The determines the steam-turbine generator
critical phase in the power plant energy-con- output, in such a way that higher values
version process is the conversion from heat of the steam turbine backpressure corre-
into mechanical energy by means of the heat spond with lower values of the steam tur-
engine. A fundamental efficiency expression bine generator output and vice versa. The
for this conversion is the Carnot (ideal) effi- steam turbine backpressure is a function
ciency, given by Equation (1): of the heat sink (or condensing) tempera-
ture, since saturated steam conditions typ-
T2 ically exist at the low-pressure (LP) steam
Carnot = 1
T1 (1) turbine exhaust.
Open cycle (or once-through) cooling sys-
Where T1 is the temperature (in Kelvin) of tems usually have the lowest heat sink tem-
the heat source and T2 is the temperature perature and therefore the highest efficiency
(in Kelvin) of the heat sink. The heat source and output. Thus, these type of cooling sys-
temperature T1 is governed by the choice tems have traditionally been the choice of
of the fuel and technological constraints on power plant designers until the 1970s, par-
the combustion or reactor processes. The ticularly for power plants that can be located
focus of this article is the selection of the nearby a vast body of water (sea, lake or
cooling system which has a direct impact river). However, once-through systems have
on the steam condensing temperature T2 large water withdrawal requirements (up to
(temperature of the heat sink) and is there- 60 m3/s for a 1,000-MWe plant) and are
44 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
characterized by significant environ-
mental impacts (for example, thermal
pollution and water intake entrain-
ment). In view of increasingly strin-
gent environmental laws and regu-
lations and the decrease in cooling
water availability, a significant shift in
the type of cooling system has oc-
curred in the last thirty years toward
closed-cycle cooling systems.
The disadvantages of closed-cy-
cle cooling lie mostly in the higher
capital and operating costs. More-
over, lower thermal efficiency due to
higher heat-sink temperatures leads
to greater fuel use per unit of gen-
erated power and more waste heat
produced. In addition, other envi-
ronmental impacts including fog-
ging, noise, land-use, drift, chemi-
cal blowdown, aesthetics and so on FIGURE 2. This photo shows natural draft cooling towers
may be encountered. While water during hot summer operating condi- sified according to their water make-
withdrawal can be decreased sub- tions, particularly for the closed-cy- up requirements, with dry and wet
stantially with closed-cycle cooling cle dry cooling systems. cooling systems on opposite sides of
systems, there is increased water the spectrum, as shown in Figure 1.
consumption (by evaporation, drift, Closed-cycle systems Dry cooling systems: heat is re-
and so on) for wet evaporative cool- Closed-cycle cooling systems for jected to the atmosphere using
ing towers or reduced power output power plant heat sinks can be clas- ambient air, so in theory, there is

STOP USING TAPERED PINS

Hammer-In Tapered Pins do not conform to ASME PCC-2-2015

Pop-A-Plug Heat Exchanger Tube Plugging System

Pop-A-Plug Tube Plugs are pressure rated up to 7000 PsiG (483 BarG) and conform to ASME PCC-2-2015
(Article 3.12) recommended tube plugging repair methods, offering a permanent mechanical solution to
safely seal leaking heat exchanger tubes. Hydraulic installation takes only minutes and eliminates the
potential for circumferential cracking and other issues caused by welding. Pop-A-Plug Tube Plugs have full
material traceability and testing documentation available.

Maximize uptime by visiting cw-estgroup.com/ce11 today!

EST Group

For details visit adlinks.chemengonline.com/66434-11

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 45

 TABLE 1. PROS AND CONS OF DRY
COOLING
Advantages of Disadvantages of
dry cooling dry cooling
No water required Low cooling efficiency
No plume in winter High capital cost
No environmental impact Large plot required
no make-up water required for the
cooling system.
Wet cooling systems: since most
of the cooling is achieved by evap-
oration of water, wet cooling sys-
tems have the highest water needs
and are the 100% reference with
respect to water requirements for
closed-cycle cooling systems.
Hybrid cooling systems: any com-
bination of a wet and dry technol-
ogy that has an intermediate water
requirement between a purely dry
and wet cooling system. Typically,
hybrid cooling systems consist of
a dry section and a wet section.
Dry cooling systems depend on
the dry-bulb temperature, since the
driving force for heat transfer is the
difference in temperature between
the process fluid and the air. Wet
cooling systems depend on the
wet-bulb temperature, since the
driving force for heat and mass
transfer is the difference in enthalpy
between the water and air.
Wet cooling systems
A closed-cycle wet cooling system
(like evaporative cooling towers) is
an indirect cooling system, which
implies that the heat of condensa-
tion is first rejected inside the con-
denser (typically a steam surface
condenser) using circulating cool-
ing water, and in a second step,
the hot cooling water is cooled in a
cooling tower by rejecting the heat
into the atmosphere.
An evaporative cooling tower
cools water by a combination of heat
and mass transfer. The water to be
cooled is distributed in the tower by
spray nozzles, splash bars, or film-
type fill, which exposes a very large
water surface area to atmospheric
air. Atmospheric air is circulated
by fans (mechanical draft cooling
tower), natural draft currents (natural
draft cooling tower), or induction ef-
fect from sprays (this technology is
rarely used today). A portion of the
46
FIGURE 3. Shown here is a round mechanical draft cooling tower
water absorbs heat to change from
a liquid to a vapor at constant pres-
sure. This heat of vaporization at
atmospheric pressure is transferred
from the water remaining in the liquid
state into the airstream.
Natural-draft (hyperbolic) cooling
towers (Figure 2) have been used
primarily for large power installa-
tions like coal-fired power plants,
and in particular for nuclear power
plants. The major advantage of
natural-draft cooling towers is that
the auxiliary power consumption is
significantly lower, since there are
no fans associated with the cooling
tower, but they are characterized
by a higher investment cost and a
negative visual impact because of
the tall structure.
For smaller-capacity power plants
or in areas where the labor cost is
high, mechanical-draft cooling tow-
ers are more frequently selected; the
cooling tower cells can be arranged
in a round configuration (see Figure
3) or in the typical standard rectan-
gular configuration.
The difference between the leaving
water temperature and the entering
air wet-bulb temperature is the ap-
proach to the wet bulb or simply the
approach of the cooling tower. The
approach is a function of cooling
tower capability, and a larger cooling
tower produces a closer approach
(colder leaving water) for a given
heat load, flowrate and entering air
condition. Thus, the amount of heat
transferred to the atmosphere by
the cooling tower is always equal to
CHEMICAL ENGINEERING
the heat load imposed on the tower,
while the temperature level at which
the heat is transferred is determined
by the thermal capability of the cool-
ing tower and the entering air wet-
bulb temperature.
Evaporative cooling systems need
water to make up for the evapora-
tion, blowdown and drift. The total
make-up water flowrate that is re-
quired for an evaporative cooling
system or cooling tower in particular
is the sum of the evaporation rate,
blowdown rate and drift rate.
Usually the drift rate is expressed
in terms of the circulating water flow-
rate and with the current high effi-
ciency drift eliminators, the drift rate
can be limited to 0.0005% of the cir-
culating water flowrate.
The thermal performance of a
cooling tower depends principally on
the entering air wet-bulb tempera-
ture. The entering air dry-bulb tem-
perature and relative humidity, taken
independently, have an insignificant
effect on thermal performance of
mechanical-draft cooling towers,
but they do affect the rate of water
evaporation within the cooling tower.
Dry cooling systems
In a dry cooling system, heat is
transferred from the process fluid
(water or steam) to the air by means
of extended heat exchanger sur-
faces or fin tube bundles. The per-
formance of dry cooling systems is
primarily dependent on the ambient
dry bulb temperature of the air and
no water is evaporated in the heat
WWW.CHEMENGONLINE.COM NOVEMBER 2017
 FIGURE 4. This schematic shows the principle op- used in a separate condenser (sur-
eration of a mechanical draft Heller system face condenser or direct-contact jet
condenser) to condense the steam
Steam coming from the LP steam turbine.
turbine
Examples of indirect dry cooling sys-
tems are the Heller system (Figure
4) and the indirect dry-cooling tower
(IDCT). A natural draft tower or a me-
chanical draft configuration with axial
flow fans can be used with indirect
dry cooling systems.
DC jet Air-cooled heat exchangers can
condenser Indirect
cooling be classified as an indirect dry cool-
tower ing system as well, although these
Circulation water pump
are rarely used to cool the water for
the steam-condensing process in a
power plant.
Direct dry cooling system. The LP
steam turbine is connected directly
Condensate booster pump
with the cooling/condensing system
transfer process. Consequently, if cooling systems: indirect and direct. via the large-diameter steam duct
no water is available for the cool- Indirect dry-cooling systems. and the process fluid is steam. This
ing system, dry cooling is the way With this type, the low-pressure (LP) is the case in an air-cooled con-
to go. Table 1 summarizes the ad- steam turbine exhaust is not directly denser (ACC).
vantages and disadvantages of dry connected with the cooling system Until recently, forced-draft, air-
cooling systems. but with a condenser and the pro- cooled condensers with single-row
There are two major types of dry cess fluid is water. Cold water is finned tubes arranged in an A-

Call the Experts

for all your solids processing

Solids Mixing Applications:

Ribbon & Cone Blenders APIs Ag-Chemicals
Fluidizing Mixers
Biologics Catalysts
Sigma Blade Mixers
(also for high-viscosity mixing) Ceramics Chemicals

Food Ingredients
Size Reduction
Herbicides Minerals
Wet & Dry Size Reduction
Steel & Ceramic Lined Mills Nutraceuticals Pesticides
Jars & Jar Rolling Mills Pharmaceuticals Pigments

Polymers Powdered Metals

Vacuum Drying
Dryers & Complete Systems Proteins Resins Vitamins

Q
U
A
EXCELLENCE
I
T
Y C O R P O R AT I O N
Environmentally Safe VpCI /MCI Technologies

Quality &
Innovation Since 1911

www.pauloabbe.com 855-789-9827 sales@pauloabbe.com

For details visit adlinks.chemengonline.com/66434-18 For details visit adlinks.chemengonline.com/66434-06

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 47

 frame configuration have been the workhorse for direct
dry-cooled power plants (Figure 5). However, high con-
struction costs and operational issues associated with
forced-draft installations have led to the development of
the induced-draft, air-cooled condenser using the same
single-row heat exchanger technology (Figure 6).
The induced-draft ACC has the following advantages
11 15 June 2018 compared to the traditional forced-draft ACC:
Weight of the supporting steel structure is reduced by
Frankfurt am Main approximately 50%
Reduced length of the large-diameter exhaust steam
duct
Shorter delivery time
Reduced air inlet height and total height of ACC
Number of steel structure pieces reduced by 60%
Pre-assembling easier (more ground pre-assembly)
2530% less man hours for construction; reduced
construction duration
Less vibration issues due to elimination of fan bridge
and consequently longer lifetime for gearboxes and
fans
ACC performance is less sensitive to wind effects since
the bundles reduce the aerodynamic effect of the wind
on the fans
Reduced hot air recirculation since the exit velocities
are significantly higher
Today, more and more power plants rely on dry cooling
technologies, because of the large make-up water re-
quirements of wet cooling towers. One of the drawbacks
of dry cooling systems is the performance hit under hot
ambient conditions.

Hybrid cooling systems

A hybrid cooling system consists of a dry section and a
wet section. One recently commercialized hybrid cooling
BE INFORMED. system is described in the box on p. 50.
It is important to note that the water use of a hybrid
BE INSPIRED. cooling system will depend on the mode of operation: if
the wet section is used at its maximum capacity to get
BE THERE. the maximum performance and turbine output, the water
consumption will be the highest.
World Forum and Leading Show The make-up water usage of the system shown in
for the Process Industries Figure 7 can be controlled by adjusting the capacity of
the wet section, simply by shutting down the fans of
3,800 Exhibitors from 50 Countries the wet cooling tower in such a way that the dry sec-
tion will handle a larger portion of the total condensing
170,000 Attendees from 100 Countries heat duty.
One of the unrecognized features of hybrid cooling
systems is the high level of control flexibility with respect
to water usage and electric output. In a traditional wet
cooling system and for a given condensing heat duty,
the make-up water usage cannot be changed because
the water usage is determined by the ambient condi-
tions and the heat load. With a hybrid cooling system,
the make-up water consumption can be changed over
www.achema.de a very broad range for a given design and in most cases
with a limited impact on the electric output of the steam
turbine generator.
In a hybrid system with a relatively small wet section
For details visit adlinks.chemengonline.com/66434-08
48 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017

FIGURE 5. This computer graphic shows a forced-draft, air-cooled condenser (ACC) with A-frame ar-
ranged heat exchangers
(consisting of a cooling tower and
surface condenser), the steam tur-
bine backpressure can be reduced
significantly at hot ambient con-
ditions compared to a 100% dry
cooling system, so the power plant
can continue to operate at full load
with a value of the turbine back-
pressure that can be significantly
lower than would be the case for
an all-dry cooling system. When it
gets colder, the capacity of the dry
section will increase in such a way
that the wet section does not need
to operate at all because the dry
section will be able to handle 100%
of the condensation heat duty.
The significant performance im-
provement of the hybrid cooling
system (Figure 7) compared to an
ACC during hot ambient conditions
is illustrated by the graph shown
in Figure 8. As can be noticed,
the hybrid cooling system shows
a significantly lower steam turbine
backpressure during hot ambient
conditions while the wet section
could be shut off if the dry-bulb
temperature is lower than 20C, if
a set point of 150 mbarA would be
selected, for example.
Selection: dry versus wet
If only capital cost has to be con-
sidered, wet cooling is usually the
preferred system since it is more
efficient from a thermal engineering
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
point of view for a given design
ambient condition, the heat sink
temperature will always be lower for
a wet cooling system.
However, wet cooling systems
are characterized by a large water
consumption rate (water loss by
evaporation, drift and blowdown).
Energy and water are essential inter-
dependent resources. As the world
population is increasing, demand
for energy and water is on the rise.
Competing demands for water sup-
ply are affecting the value and avail-
ability of the resource. Operation of
some power plant facilities has been
curtailed due to water concerns, and
siting and operation of new energy
facilities must take into account the
value of water resources.
Evaporative or wet cooling sys-
tems generally are the most eco-
nomical choice for closed-cycle
cooling systems where an adequate
supply of suitable make-up water
is available at a reasonable cost.
However, wet cooling systems suf-
fer from certain environmental is-
sues like plumes (which may result
in fogging and icing conditions in
areas close to the power plant), drift
(PM10 emissions), blowdown (con-
centrated cooling water) and risk for
Legionella, so dry cooling systems
are certainly more environmentally
friendly, and are considered as a
green technology. So, if there is
NOVEMBER 2017
FIGURE 6. A schematic of an induced-draft, air-
cooled condenser is shown here.
not enough make-up water avail-
able for wet evaporative cooling or
if there are environmental concerns
(drift, plume, and so on), dry cooling
is a feasible alternative.
The next question is then how to
select between a direct dry (ACC)
or indirect dry (Heller) system. From
a capital investment point of view
only, air-cooled condensers are
somewhat less expensive than
Heller systems. However, Heller
systems can be beneficial in the
following cases:
The power plant is designed
around a fast start-up concept: air-
cooled condensers have a large
volume compared to the condens-
er volume of an indirect dry cool-
ing system, so the start-up time
of a Heller cooling system can be
much shorter
The power plant is located in re-
gions that are vulnerable to high
wind velocities or wind gusts the
performance of indirect dry cooling
systems is less impacted by wind
as compared to the traditional
A-frame air-cooled condensers;
however, induced-draft air-cooled
condensers are less sensitive to
the wind as well, as stated above
Plot area restrictions: indirect dry
cooling systems are easier to ar-
range on the site plot plan com-
pared to ACCs; the ACC cells are
typically arranged in a rectangular
plot area that is located close to
the turbine building. Heller sys-
tems are characterized by a high
degree of flexibility when there are
restrictions in plot area or location
Low noise limit: if there is a low
noise level to be guaranteed at the
site boundary, Heller systems are
preferred; moreover, because of
the flexibility in the arrangement of
the indirect dry cooling tower cells,
49
 Steam in
A HYBRID COOLING SYSTEM
The parallel condensing system, shown in
Figure 7, is a hybrid cooling system that
Steam turbine
consists of an air-cooled condenser and a
steam surface condenser that is typically
cooled by a mechanical draft wet cool-
Steam flow to ACC ing tower, with the steam coming from
the low-pressure (LP) steam turbine being
condensed in parallel by the air-cooled con-

Steam flow to SSC

denser and surface condenser.
This type of hybrid cooling system was
first introduced by GEA (now Enexio) for
a relatively small 31 MW waste-to-energy
ACC plant (Exeter Energy facility) in Connecti-
cut. It utilizes whole and shredded tires as
Cooling tower primary fuel. Later, a larger version was
implemented for gas-fired power plants in
Argentina (Tucuman). The largest system
in the world started commercial opera-
tion in 2010 for the Comanche III unit in
Pueblo, Colorado a 750-MW coal-fired
Condensate out power plant that is owned and operated
by Xcel energy.
FIGURE 7. This schematic shows the operation of a hybrid cooling system for power plants
of the cooling system significantly.
a location can be selected that is denser already in place (typically During moderate or cold operating
further away from the critical noise located in close proximity of the conditions, the dry section can han-
reception point steam turbine exhaust), can be dle 100% of the heat duty, which al-
Retrofit of an existing wet cool- very challenging lows plant operators to save water
ing system to a hybrid or 100% A very promising technology is and avoid having to deal with the
dry-cooled system: if the power hybrid cooling, since it combines negative effects of plume coming
plant was originally equipped with the best features of both worlds, from the cooling tower in winter. n
a wet cooling system, it is much particularly if there is a little bit of Edited by Gerald Ondrey
easier to add an indirect dry cool- make-up water available. The yearly
ing add-on to the circulating wa- water consumption can be reduced Additional articles on cooling towers can be
ter system or to convert it to a significantly compared to 100% wet found in the Chemical Engineering archives
at www.chemengonline.com (for example,
100% indirect dry cooling system cooling, and the investment cost Vengateson, V., Cooling Towers: Estimate Evaporation
connecting the water piping of can be reduced significantly com- Loss and Makeup Water Requirements, Chem. Eng.
the indirect cooling tower to the pared to 100% dry systems for a April, 2017, pp. 6467).
existing circulating water piping is given thermal duty to be handled.
rather straightforward connect- The wet section only needs to be Author
ing a large diameter steam duct of engaged during hot summer oper- Luc De Backer is vice president
an ACC to the steam turbine ex- ating conditions and will allow op- of Technology with Enexio US (En-
exio Power Cooling Solutions,
haust with a steam surface con- erators to increase the performance 300 Union Blvd, Suite 350, Lake-
wood, CO 80228; Phone: +1
400 303-987-4027; Fax.: +1 303-
987-0101; Email: luc.debacker@
ACC enexio.com, Website: www.en-
350
exio.com). De Backer started his
Turbine back pressure, mbar, absolute

professional career in Belgium

300 with Hamon Thermal Europe in 1995 and developed
his expertise in the single-row tube technology for air-
250 cooled condensers. He moved to the U.S. in 2000 and
became a member of the ASME to co-author the ASME
200 PTC 30.1 performance test code for Air-Cooled Steam
Condensers. He was also the technical chairman for
150 Hybrid the Heat Exchange Institute (HEI), issued the first HEI
standard for air cooled condensers. De Backer focused
100 on wet cooling systems as the technical specialist for
Bechtel. In 2008 he established the center of excel-
lence for hybrid cooling systems for GEA in Phoenix,
50
Arizona. He is also founder of Advanced Cooling Solu-
tions, a partnership company that specializes in cool-
0 ing systems for power plants. De Backer holds a Ph.D.
0 5 10 15 20 25 30 35 40 in chemistry, an M.S. in chemical engineering and an
Ambient dry bulb temperature, C
M.S. in chemistry, all obtained from the Free University
of Brussels, Belgium. Currently he lives with his family
FIGURE 8. This graph compares the performance of an air cooled condenser (ACC) and a hybrid cooling in San Tan Valley, Arizona.
system
50 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
Engineering Practice

Emergency Shutdown Valves:

A Functional Safety
Approach to Selection
The relationship between valve selection and safety certification still causes confusion. A focus
on functional safety can help to elucidate
Ville Khknen facturers design or
Metso Flow Control Inc. design process is
being evaluated by

A
mong the many varied a third party (Figure
viewpoints on the topic of 1). Additionally, cer-
emergency shutdown (ESD) tification ensures
valves, there are several as- that a product is
pects that continue to spark discus- compliant with a
sion and cause confusion due to a standard.
lack of complete clarity, including the However, certi-
relationship between valve selection fication does not,
and safety certification. In this article, by itself, guaran-
we aim to clarify a few of the most tee anything about
misunderstood points associated valve performance.
with the selection of ESD valves. And A new certificate
in doing so, we hope to bring greater does not make the
recognition to the concept of func- valve or valve unit
tional safety, which is associated with suitable for the
the safety integrity level (SIL) stan- safety loop. Valve
dards laid out by the International selection is still the
Electrotechnical Commission (IEC; most critical as-
Geneva, Switzerland; www.iec.ch): pect. The same
IEC 61508 (Functional Safety of steps regarding
Electrical/Electronic/Program- valve suitability for FIGURE 1. Certification of ESD valves ensures that products are compliant
mable Electronic Safety-Related the process must with standards, but does not guarantee valve performance
Systems) be considered in
IEC 61511 (Functional safety the ESD service as with any other comes from a conversation the au-
Safety instrumented systems for valve. So, included in this article are thor had a few years ago with several
the process industry sector) valuable steps to take for ESD valve experienced plant personnel who
Functional safety is a much selection to make sure the whole were absolutely confident that ball
broader set of concerns than the picture is taken into consideration. valves are not suitable for gas pro-
question of which valves to select. cesses. This assertion was based
Certification has been a key issue Valve selection on observations of real valve per-
of confusion recently: many people Ideas, opinions and experiences formance from years before, when
think a SIL 3 certificate for valves is abound regarding which type of an incorrect material selection led
a must; likewise for a solenoid valve. valve to use in a specific service. to a situation in which the valve was
Still, certification is just one part of Some of these opinions can bring performing poorly and was finally
ESD valve selection. Certification valuable field-proven information; destroyed. The plant personnel con-
is not mandatory according to IEC others may be simply based on the cluded that the valve failed because
61508 and 61511, but it can bring wrong conclusions. it was the wrong type (ball valve).
valuable information when a manu- A good example of this situation Yet in similar processes across the

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 51

 globe, there are thousands of ball
valves doing a very good job. There-
fore, the valves problems were
based on the fact that its materials
of construction were not suitable for
the application any type of valve
made from incorrect materials would
have led to a failure in this situation.
Failures can be divided into two
categories: systematic failures and
random failures. When selecting
valves, it is imperative to make sure
that the valve chosen is capable of
performing in the intended service. If
a valve repeatedly fails in the same
manner, it is likely a systematic failure
and cannot be avoided. In this case,
improving the valves performance
will occur only by changing some-
thing in the selected components of
the valve.
In ESD valve selection, the safety
loop must be free of systematic er-
rors. This requirement concerns not
only the valve body, but also other
valve components. For example, the
actuator must be capable of achiev-
ing sufficient torque or force to op-
erate the valve. And the intelligent
safety solenoid must have the ca-
pacity to reach the required shut-off
or opening time of the unit, which is
specified in safety requirements.
As an example of a systematic error,
we can use the material selection
mistake in chloride service. With dry
chlorine, even carbon steel is a suit-
able valve body material. However,
when enough moisture is present,
hydrochloric acid forms, and the car-
bon steel body is no longer a suitable
material. To avoid systematic failures,
the body material needs to be en-
hanced to a grade that can withstand
the more aggressive flow media. In
this example, the root cause of the
failure is the selection of an unsuitable
material selection. In such a situation,
the same failure will occur regardless
of the type of valve chosen.
The key to avoiding such system-
atic failures is the use of application-
based valve selection.
Functional safety
In recent years, awareness of func-
tional safety within the chemical
process industries (CPI) has been
increasing. Having a greater num-
ber of people aware of the IEC stan-
dards and the ideas behind them is
a positive development. Still, there is
52
FIGURE 2. The key to avoiding systematic valve failures is application-based valve selection, which is
supported by functional safety calculations and regular testing and maintenance
a lot of confusion around the stan-
dards, as well as the requirements
for valves and how to comply with
these requirements. A commonly
held belief is that the simplest solu-
tion is just to ask for a SIL certificate
and all will be fine.
However, the SIL certificate alone
is not enough. The certificate usu-
ally describes what the final element
is, such as a valve, and for which
SIL that valve is suitable. SIL-3
certification does not necessarily
mean that the final element fulfills
SIL-3 requirements. It does mean
that the valve is capable of working
in a SIL-3 loop, but there are more
points to be considered.
First is the SIL capability, which the
certificate can confirm. Second is the
hardwares fault tolerance (HFT) to
that particular SIL. In the certification,
there is typically a different approach
based on the various parties who
have granted the certificate. Usually,
certificates speak only to SIL capabil-
ity, such as a valve being SIL 3 capa-
ble. Some certificates have an extra
note that includes fault tolerance. For
example, a valve could be be SIL
3 capable in an HFT 1 (hardware
fault tolerance) configuration, which
means there must be two valves in a
one out of two (1oo2; duplex) con-
figuration to satisfy the SIL 3 require-
ment. Or, there can simply be the text
SIL 3 without any further comments.
The text 1oo2 means that one final
element, like a valve, can fail and the
safety function is still available.
HFT is an important aspect in the
IEC standards, and is usually the first
topic that causes controversy. With
study of IEC 61508, we can follow
the safety fail fraction (SFF) method
for defining HFT. For a valve, this
means if the SFF is more than 90%,
we can use one valve to satisfy the
HFT of the SIL 3 requirement.
The calculation in Equation (1) is
quite simple if the required values
are available. Usually, these lambda
values can be found from the valve
manufacturers certificate. If not,
CHEMICAL ENGINEERING
then usually generic values can be
used based on similar components.
SFF = (dd + S) / (Dd + Du + S)
(1)
Where dd is the detected danger-
ous failure rate; S is the safe failure
rate; and Du is the undetected dan-
gerous failure reate. The discussion
about SFF is typically related to the
valve part, because the SFF method
is suitable for mechanical compo-
nents like valves, and if the ratio of
safe failures to all failures justifies the
hardware fault tolerance.
Currently, it is more common to
follow IEC 61511 and use the table
method, in which the HFT is se-
lected based on the predefined table
by a different operating mode. Final
elements, such as valves, are typi-
cally, but not always, in low-demand
service. Therefore, the HFT for SIL 3
becomes the minimum of two valves
in a 1oo2 setup. The minimum HFT
for SIL 1 and 2 is one final element.
The HFT is not the only require-
ment that needs to be considered.
The probability of failure on demand
average (PFDavg) also must be cal-
culated for the setup. If the PFDavg
does not satisfy the needed safety
integrity level demand, a few op-
tions exist. The easiest is to double
the components. For example, SIL
2 could be satisfied with one valve,
but if the PFDavg is low and refers to
SIL 1, we do not have a capable final
element configuration.
Figure 3 presents a few options to
satisfy the PFD requirement. Figure 3
(left) shows the base level with a 48-
month testing interval. Figure 3 (mid-
dle) shows the same components,
but the testing interval is shorter.
Instead of 48 months, there is a 24-
month testing interval and in this
case, there is a significant change in
the PFD value.
Sometimes, it is not that easy to
change the testing interval to a proof
test, because it will have an impact
on the plant operation. Therefore,
WWW.CHEMENGONLINE.COM NOVEMBER 2017
FIGURE 3. The average probability of failure on demand (PFDavg) must satify the required safety integrity level (SIL) demand. Periodic testing intervals like those
shown here are the backbone of testing
in Figure 3 (right), the solenoid valve
has been replaced with an intelligent
safety solenoid and partial-stroke
testing has been utilized to increase
the amount of testing, while keeping
the proof test interval at the same
length (48 months). This will increase
the testing flexibility.
ESD valve maintenance
Very often, ESD valves are con-
sidered to be install and forget
valves. However, although they do
MONITOR VISCOSITY SIMPLY
SENSE MIXER MOTOR HORSEPOWER
WITH UNIVERSAL POWER CELL
EASY INSTALLATION
Noholesintanksorpipes
Awayfromsensitiveprocesses
VERSATILE
Onesizeadjuststomotors,from
smallupto150hp
Workson3phase,xedorvariable
frequency,DCandsinglephasepower
SENSITIVE
10timesmoresensitivethan
justsensingamps
CONVENIENT OUTPUTS
Formeters,controllers,computers
4-20milliamps0-10volts
WWW.LOADCONTROLS.COM
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
not control the process all the time tervals are the backbone of testing
and are mostly in a normal state, and are a minimum requirement to
ESD valves must be considered to keep the valve in duty. Some ser-
be on duty at all times. A valve that vices are more severe than others,
has been in a pipeline for several and in PFDavg calculations, this is
years without any operation, test- not always noticed and addressed.
ing or maintenance might not work Partial-stroke testing can be a great
when it is needed. Therefore, test- help to check the valve condition
ing and maintenance are a vital part while the valve is in operation. But to
of an ESD valve life. keep the needed and defined SIL, a
The first point to consider here is proof test must also be made.
the periodic testing intervals from The testing interval is important
the PFDavg calculations. These in- in both calculations and in a real
PROFILING A PROCESS
Powerchangesreectviscositychanges
Goodbatcheswilltthenormalprolefor
thatproduct
24
POWER DECREASE
22
SHOWS BATCH
20
IS DONE
18
16
POWER
SENSOR
14
12
10 DRY MIX ADD LIQUID
HIGH SPEED LOW SPEED MIXER
8 MOTOR
6 BEGIN HIGH
SPEED MIX
4
0
BATCH 1 BATCH 2 BATCH 3
CALL NOW FOR YOUR FREE 30-DAY TRIAL 888-600-3247
For details visit adlinks.chemengonline.com/66434-14
NOVEMBER 2017 53
 process. Equation (2), from the In-
ternational Society for Automation
(ISA; Research Triangle Park, N.C.;
www.isa.org) standard TR-96.05.01,
shows the following:
(2)
DC = diagnostic coverage
d = Dangerous failure rate
TIPST = Partial stroke test interval
TIFST = Full stroke test interval
MTTR = Mean time to restore
Testing is needed to keep the re-
quired safety integrity level.
From the graph in Figure 4, the
green line represents the PFD value,
which when increasing, results in
a decreasing SIL level at a certain
period of time. If the requirement is
SIL 2, as in this example, the limit
is reached in just over three years.
But a problem occurs, for example,
if the plant shutdown period is four
years. The other line in Figure 4
marked with blue color is the PFD
value with partial-stroke testing. The
PFD value increases, but at a lower
pace. Eventually, we will reach the
limit of the required SIL and cannot
avoid the full stroke and proof test,
but the advantage is now that the
testing period for full testing can be
more flexible.
It is important to remember that
proof testing cannot be avoided by
conducting the partial-stroke test
alone, but the testing interval can
be changed. The example calcula-
tions in Figure 3 include 77% diag-
nostic coverage.
Concluding remarks
It is promising that the awareness
of functional safety has increased
during the past few years. At the
same time, however, more confu-
sion around this topic has arisen.
In this article, we outline a few of
the main steps when it comes to
valves and functional safety. Even
though SIL and PFD calculations
are a hot topic at the moment, we
must still remember that the most
important aspect is application-
based valve selection. After we
have done a good job in selecting
the valve and other components,
we can then take advantage of the
PFD calculations. It is important
not forget to maintain ESD valves.
This is vital to keep the required SIL
and ensure that the valve works in
the process when needed to carry
out its safety function.
Edited by Scott Jenkins
Author
Ville Khknen is the director of
industry management at Metso
Flow Control Inc. (Tlnlahden-
katu 2, FI-00100, Helsinki, Fin-
land; Phone: +358 20 484 100;
Email: ville.kahkonen@metso.
com). He has over ten years of
experience in different roles, in-
cluding business management,
research and development, engi-
neering and marketing. He has been with Metso more
than 10 years. Khknen holds a masters degree in
materials science and industrial management from Hel-
sinki University of Technology and has studied at the
Helsinki School of Economics.

In todays operating environment, its

ENSURE more important than ever that the
piping within your Mechanical Integrity
YOUR Program complies with standards such
as API-570 and API-574.
PROCESS
Quest Integrity offers a
100%inspection
PIPING comprehensive solution of internal and
for piping circuits using our external pipe
INTEGRITY proprietary, surfaces
ultrasonic-based intelligent Inspectionresults
tailored to comply
pigging technology combined
withAPI-570and
with LifeQuest Fitness-for- API-574
Service software. LifeQuestFitness-
for-Service results
Ensure your piping integrity tailored to comply
by identifying degradation with API-579
before loss of containment
occurs.

QuestIntegrity.com
CHALLENGE CONVENTION

For details visit adlinks.chemengonline.com/66434-22

54 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
Solids Processing
Powder and Bulk Solids Handling:
Particle Size and Distribution Analysis
The size and size distribution of particles are important determining factors in
the design and operation of many process operations involving dry particles and
powders. Follow this guidance to understand the impact of these key characteristics
John Lawrence
Kansas State University
B
ulk solids are dry particles
with particle sizes that
range from a few millimeters
to a few nanometers. The
characteristics of bulk solids change
with particle size and particle-size
distribution. As such, particle size is
one of the key parameters in powder
characterization [1].
Information about the particle-
size distribution of a powder is also
an important step in many chemical
process operations, and improper
particle-size analyses can result in
poor product quality and high rejec-
tion rates, which leads to economic
losses. Particle size and its distri-
bution also have a significant effect
on the bulk density, mechanical
strength, and electrical and thermal
properties of the finished product [2].
Meanwhile, particle-size distribution
determines a variety of important
physical and chemical properties
such as mechanical bulk behavior,
surface reaction, taste, miscibility,
filtration properties, and conductivity
[3]. Based on 1993 British Standards
[4], any discrete particles whose
sizes are less than 1,000 m are
called powders.
Understand these key attributes
The importance of particle size and
particle-size distribution in various
bulk-solids-handling operations is
discussed further here, and then
discussion of several measurement
techniques of particle size follows.
Storage and flow. Particle size in-
fluences the flowability of a mate-
rial. Flowability is the ratio between
the cohesive forces acting on the
particles (which make them stick to-
gether) and the normal forces (which
are trying to break them apart) [5].
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
Unconfined yield strength, c
FF=1
No flow
e
siv
ohe
r yc
Ve
esiv
Coh
Easy-flowin
Free-flowing
Consolidation stress, 1
FIGURE 1. Shown here are flow function values
for easy-flowing materials (higher flow-function,
or FF, values) and cohesive or difficult-flowing
materials (lower FF values)
For example, for a material that has
two particle sizes (D50 = 30 m and
40 m), there will be significant vari-
ance in flowability. Finer particles
have higher cohesive strength com-
pared to coarse particles.
The flowability of each sample can
be determined by measuring the flow-
function (FF) characteristics of the ma-
terial using a ring-shear tester. FF is
defined as the applied normal load di-
vided by the unconfined yield strength,
according to Equation (1):
Normal stress
FlowFunction (FF) =
Unconfined yield strength
Higher unconfined-yield-strength
values yield lower FF values (which
signifies a difficult material, in terms
of its flowability). Lower unconfined-
yield-strength values create higher
flow-function values (which signifies
an easy or free-flowing material), as
shown in Figure 1.
For example, for a normal stress
of 4 kilo Pascal (kPa), easy-flowing
materials have an unconfined yield
strength between 0.4 and 1 kPa,
which yields FF values between 10
and 4. By contrast, difficult materi-
als have an unconfined yield strength
NOVEMBER 2017
FF=2
Large particles
e
FF=4
g
FF=10
Fine particles
FIGURE 2. This diagram shows what happens
when particle-size differences lead to percolation
segregation inside of a hopper or vessel
between 4 and 2 kPa, which yields
FF values between 1 and 2.
For the same material, if the par-
ticle size decreases, its cohesive
strength increases, reducing its flow-
ability. During the design of a mass
flow hopper, the flow-function (flow-
ability) determines the ideal hopper
angle, and dictates whether its walls
are steeper or more shallow, as well
as the ideal outlet dimension (open-
ing size). Mass flow behavior refers
to first-in, first-out material flow in a
hopper. Easy-flowing materials with
a higher FF value require the hopper
(1) angle to be more shallow, whereas
materials with a lower FF value (that
is, difficult-flowing materials) require
a steeper wall angle and wider outlet
dimension in order to ensure mass
flow during operation.
By way of example, consider two
samples of fluegas-desulfurization
gypsum with 11% moisture, one
with a D50 median particle size of 25
m and the other 35 m. The 25-m
particle size demonstrates higher
unconfined yield strength compared
to the sample with 35-m particle
size [5]. This means that, to ensure
mass flow, the 25-m size particles
would need a steeper hopper angle,
55

FIGURE 3. Particles typically have an irregular
shape; to measure particle size and size distribu-
tion, simplifying assumptions must be made using
spherical shapes as a proxy measurement
compared to that required for the
35-m size particles.
Particle-size distribution also has a
major effect on the wall-friction angle,
which also determines the hopper
angle that is required to ensure mass
flow. Higher wall-friction angle corre-
lates to difficult-flowing material (those
with lower FF values). For example, in
Ref. 5, when the same samples de-
scribed above were used to study
the wall-friction angle on a mild steel
plate, it was demonstrated that 25-m
particle required a higher wall-friction
angle, compared to that of the 35-m
particle size sample.
As the particle size decreases, the
effect of van der Waals forces and
liquid bridges increases. This hap-
pens because the increase in the
number of particle contacts that oc-
curs with shrinking particle size leads
to an increase in the overall cohesive
strength of the material.
Pneumatic conveying. Particle
degradation during conveying is one
major problem that is associated
with dilute-phase pneumatic convey-
ing. Dilute-phase pneumatic convey-
ing systems refer to those systems
that provide pneumatic conveying at
relatively high velocity (greater than
4,000 ft/min) and relatively low pres-
sure (on the order of 515 psi). At
this high velocity, conveying material
impacts on the elbows, resulting in
particle degradation. For instance,
when conveying granulated sugar
in a dilute-phase system, the mate-
rial impact on piping elbows often
causes many of these particles to be
degraded into a finer powder form.
Operators in many industries want
to keep particle-size distribution
constant during pneumatic convey-
ing. However, in many instances,
bulk solids experience an increase
in particle-size distribution as a result
of impact-force degradation. One
way to monitor and analyze particle
56
100
90
80
70
Cumulative mass, %
60
50
40
30
20
10
0
20 40
D10=47 m
FIGURE 4. Particle-size distribution of bentonite powder with D10, D50, and D90 sizes
degradation is to track the particle
size before and after conveying.
The pick-up velocity is an essen-
tial aspect to consider during the
design of dilute-phase pneumatic
conveying systems. This velocity
is influenced by the mean particle
size of the material. The higher the
mean particle size of the material,
the higher the pick-up velocity, and
vice versa. Similarly, the particle size
also influences the feedrate of the
material in a particular size pipeline.
Mills [6] found that if the mean par-
ticle size of flyash was reduced from
110 to 75 m, the capacity would be
increased one-fold.
Segregation. Particle size and its
distribution also determine the seg-
regation tendency of the products.
Wider particle-size distribution typi-
cally results in higher segregation
based on the differences in particle
size and density. Different types of
segregation such as sifting, per-
colation segregation, fluidization and
dusting occur as a result of the
materials particle-size distribution.
Sifting segregation occurs during
silo filling and chute discharge, as
larger particles tend to move away
from the discharge point and finer
particles tend to settle near the
discharge point
Percolation segregation (Figure
2) occurs during transportation,
when larger particles tend to move
up and finer particles tend to settle
at the bottom of the vessel
Fluidization and dust segrega-
tion causes larger particles to
settle due to greater density, and
CHEMICAL ENGINEERING
Bentonite Powder: Particle-Size Aanalysis
60 80 100 120 140 160 180 200
Particle size, m
D90=127 m
D10=80 m
finer particles tend to move to the
top of the vessel
Production processes. During
chemical-manufacturing processes,
the particle-size distribution of bulk
solids are typically analyzed at differ-
ent stages in the production process.
The process faces the risk of signifi-
cant production losses if the particle-
size distribution is not monitored ac-
curately to ensure an optimal value
or range. During the manufacturing
of powders, and during grinding and
sieving operations, routine analy-
sis of particle-size distribution must
be carried out until the material has
reached the final acceptable quality
required by the final product.
Measuring size and distribution.
The measurement of particle size
is very complex, because most fine
particles have a shape that is neither
regular nor uniform (Figure 3). There-
fore, for these types of irregularly
shaped particles, size is often ex-
pressed in terms of a circle or a sphere
(as a simplifying assumption), which
is deemed to be equivalent to the ir-
regularly shaped particle; it is called
the equivalent spherical diameter.
This means the volume or surface of
irregular shape is converted to an
equivalent volume or surface of
sphere or circle and expressed as an
equivalent spherical diameter.
For example, an irregularly shaped
particle has a surface area of 0.002
mm2, its equivalent diameter is 0.05
mm. Particle-size distribution is de-
fined as the size and frequency of
particles in a population and di-
mensional measurement of irregu-
WWW.CHEMENGONLINE.COM NOVEMBER 2017
 Standardized Universal Synthesis Unit ready for Operation
The QVF Universal Reactor of De Dietrich Process Systems is the solu-
tion if larger quantities than with a 3-neck lask in the lab scale should be
synthesized. With this unit it is possible to run safely reactions in the liquid
phase between -20 and +150C under inert gas. Light boiling compo-
nents can be distilled off at atmospheric pressure or under vacuum. The
Universal Reactor is equipped with the required valve arrangement, pip-
ing and ATEX classiied instrumentation, ready for operation in ex-rated
areas and needs only to be connected to heating and cooling media. The
construction of the reaction unit permits simple and reliable cleaning via
CIP nozzles. This type of reaction system has been standardized for glass
reactors from 6 to 50l.

De Dietrich Process Systems www.dededietrich.com

For details visit adlinks.chemengonline.com/66434-01

Non-invasive hydrocarbon mass low

Measurement, product identiication and tank dewatering
With the FLUXUS HPI meter, it is possible to combine non-invasive mass
low metering with hydrocarbon product identiication. As hydrocarbon
products can be distinguished through the ultrasonic signal, the FLUXUS
HPI meter is the meter of choice in tank storage applications when differ-
ent hydrocarbons are successively passing through the lines. Moreover,
it is also the ideal tool for tank dewatering applications as water / hydro-
carbon cuts can clearly be detected.
The measurement of standard volume and mass lows is carried out ac-
cording to Industry Standard Algorithms such as TP-25, ASTM D1250 and
D4311.

Flexim www.lexim.com
For details visit adlinks.chemengonline.com/66434-02

Complete Flow Energy Management Solution for

Sierra Instruments
www.sierrainstruments.com
For details visit adlinks.chemengonline.com/66434-03
Gas, Liquid, & Steam Applications
Sierra Instruments new Big-3 products offer engineers a complete low
energy management solution for lows that cost money like compressed
air, natural gas, steam and hot and chilled water. The Big-3 is made up of
Sierras QuadraTherm 640i/780i thermal low meters for gas, Innova-
Mass 240i/241i vortex low meters for steam, and InnovaSonic 207i
ultrasonic low meter for liquid. Now, for the irst time, facilities managers
can work with one USA company to specify, install, and support all low
meters for any gas, liquid or steam application.
The Big-3 sets a new standard in low meter technology with ease-of-use
through uniied software apps, integration across platforms, best in class
sensor technology and performance and, USA manufactured and calibrat-
ed. Learn how to optimize the low energy in YOUR facility today.

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 57

 TABLE 1. PARTICLE-SIZE-MEASURING
TECHNIQUES AND SIZE RANGES
Instrument Techniques Size range, m
Mechanical sieving (dry) 38 to 100,000
Mechanical sieving (wet) 20 to 3,000
Air jet sieving 20 to 200
Ultrasonic sieving 5 to 100
Gravimetric 1 to 3,000
sedimentation
Coulter counter 0.5 to 300
Laser-light diffraction 0.02 to 1000
Centrifugal sedimentation 0.01 to 10
Microscopic image 0.01 to 1
analysis
larly shaped particles [7]. It is also
expressed as D10, D50 and D90
terms. D10 is the diameter of particle
at which 10% of a samples mass is
comprised of smaller particles in that
sample size; D50 is the diameter at
which 50% of a samples mass is
comprised of smaller particles in that
sample size and D90 is the diameter
at which 90% of a samples mass is
comprised of smaller particles in that
sample size.
There is no single standard
method to measure particle size;
each method has its own pros and
cons. Some of the standard meth-
ods that are used to measure par-
ticle size and size ranges are shown
in Table 1, and several of them are
discussed next.
Mechanical sieving
Mechanical sieving is one of the old-
est methods for measuring particle
size and carrying out size-distribu-
tion analysis of free-flowing, dry bulk
solids and powders. It is the most
widely used method since it pro-
vides reliable results. This approach
involves shaking or vibrating a sam-
ple through a series of woven-wire
sieves of known mesh size.
Sieve analysis is done by pass-
ing a known weight of sample ma-
terial through a set of sieves that is
arranged from coarse mesh at the
top to finer mesh at the bottom of
the stack. The amount of material
retained on each sieve is weighed
to determine the percentage weight
in the size fraction retained on each
sieve. Some of the common mesh
numbers and aperture sizes are pro-
vided in Table 2. The mesh number
system is a measure of the num-
ber of openings per linear inch in a
screen; the higher the number, the
lower the mesh opening size.
Based on the data collected after
sieving (as shown in Table 3), the
58
TABLE 2. COMMON SIEVE MESH
NUMBERS AND APERTURE SIZES
US Mesh Number Aperture size, m
10 2,000
30 500
60 250
120 125
230 63
mean particle size is calculated using
the formula in Equation (2):
Where:
dpm = Arithmetic mean of adjacent
sieve sizes
M = Summation of sample mass
collected in each sieve
dp = Mean particle size of the sample
For example, if the following data
were obtained from a sieve test
(Table 3), the mean particle size is
calculated using Equation (3):
Note that this method is only appli-
cable for particles larger than 0.038
mm (38 m). Since the length of the
particle does not affect its passage
through the sieve opening, the par-
ticle size goes with the maximum
width and maximum thickness of the
particle, which may not represent its
actual size. This is one drawback to
using sieving technology.
As noted, the particle-size distri-
bution is calculated by tabulating the
sieve size and the amount of sample
that is retained in the sieve. Then
the cumulative mass percentage is
calculated in terms of sieve size and
cumulative mass percentage. These
data are plotted in a graph, such as
the one shown in Figure 4. From the
graph, the particle sizes for D10, D50
and D90 are calculated by correlating
the particular cumulative mass per-
cent and particle size. D10, D50 are
the particle sizes correlated at 10%
and 50% cumulative mass percent-
ages and so on. Figure 4 shows the
particle-size distribution of bentonite
powder. The particle sizes of benton-
ite powder at the D10, D50 and D90
cumulative mass percentages of that
sample size are 47 m, 80 m and
127 m, respectively.
CHEMICAL ENGINEERING
TABLE 3. SAMPLE DATA WERE OBTAINED
FROM A SIEVE TEST
Sieve number, m Sample weight, g
230 (63 m) 40
170 (90 m) 71
120 (125 m) 54
70 (212 m) 35
Total 200
Sieve options
Dry mechanical sieving. Dry me-
chanical sieving systems can be op-
erated in two different ways with
a vertical or horizontal orientation.
(2) Similarly, two types of vertical siev-
ing systems are available, in terms of
mechanism of action vibrational
sieving and tapping sieving. With
horizontal sieving, the sieves move
in horizontal circles in one plane [3].
This type of sieve is widely used.
With vibrational sieving, an elec-
tromagnetic drive creates vibrational
motion that is transmitted to the
stack of sieve trays. The amplitude
of vibration varies from 0 to 3 mm.
With tapping sieving, the tapping
motion is achieved using the me-
chanical eccentricity (Figure 5).
Advantages of a mechanical sieve
(3) include the following:
Easy to operate
Low equipment cost
Reliable and repeatable
Disadvantages of a mechanical
sieve include:
May result in agglomeration of fine
powders (this can be avoided by
using wet sieving if the material is
not hygroscopic)
In many cases, the particle sizes
are too small for separation by
sieving
Below 38-m sieve size, it will be
very difficult to get material to pass
through
The amount of energy used to
sieve the sample is arbitrarily de-
termined
Over time, the sieving operation
may cause attrition of the particles
and increase the particle-size dis-
tribution, while insufficient time of
operation may fail to break down
loose agglomerates, which can
alter the actual results in both
cases. Therefore, observing an
optimum time of operation is es-
sential, which can be established
by experiment.
Chain, brushes and rubber cubes
are often used as sieving aids for ma-
terials that are sticky in nature due to
electrostatics and additives [3].
WWW.CHEMENGONLINE.COM NOVEMBER 2017

FIGURE 5. In this tapping-type mechanical sieve,
mechanical eccentricity is used to create a tap-
ping motion that forces the particulate material to
pass downward through the stack of sieve trays
Air-jet sieve analysis. This type of
sieve analysis is used for powdered
materials that require sufficient dis-
persion and de-agglomeration [8].
This equipment consists of a rotating
slotted nozzle, which is placed un-
derneath the sieve and lid (Figure 6).
A negative pressure (vacuum) pneu-
matic system is designed to gener-
ate a strong jet of air that allows the
particles to disperse and be sucked
through the slotted nozzle.
Air-jet sieves operate differently
than mechanical sieves. In a me-
chanical sieves, large particles are
separated first, followed by next
smaller, and finally the very finest-
mesh particles. However, in air-jet
sieving, very fine particles are re-
moved first, followed by next bigger
and finally the largest particles.
The material that has a particle
size smaller than that of the mesh
size of the sieve is conveyed to the
solid-gas separation unit by either
a cyclone or air filter system. The
material that is larger than the sieve
mesh is retained, weighed, trans-
ferred to next sieve in line for air-jet
stream operation. This keeps fine
particles from agglomerating.
ASTM International (American
Soc. for Testing Materials, West
Conshohocken, Pa.; www.astm.
org) E11 Standard Specification
for Woven Wire Test Sieve Cloth and
Test Sieves, and ISO (International
Organization for Standardization;
Geneva, Switzerland, www.iso.org)
3310 Test sieves [9] provide techni-
cal requirements for the sieves and
appropriate testing methods for
sieve analysis.
Laser-diffraction techniques. An-
other important, widely used method
CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM
FIGURE 6. The rotating nozzle in an air jet sieve
helps to minimize agglomeration for powdered
materials that are susceptible to it
(Source: Hosokawa)
to measure particle size is based on
laser-diffraction techniques. This
method is particularly well-suited for
measuring particle size less than 38
m. However, it can be used to mea-
sure particle size between 0.1 and
3,000 m. The equipment tends to
be costly, however (on the order of
$50,000 or more).
The principle of measurement is
the halo of the diffracted light pro-
duced when a laser beam passes
through a dispersion of particles sus-
pended in air. The light that is scat-
tered at various angles by different
size particles is measured by a multi-
element detector, and the magnitude
of the scattered light intensities are
recorded [7]. Large particles scat-
ter light at small angles relative to
the laser beam, while small particles
scatter light at larger angles.
The angular-scattering intensity
data are analyzed to calculate the
size of the particles that are respon-
sible for creating the scattering pat-
tern, using the Mie theory of light
scattering. The particle size is then
reported as a volume-equivalent
sphere diameter [9], using sophisti-
cated data-processing methods and
automation. This generates a con-
tinuous measurement for analyzing
process streams.
Sampling techniques
Proper sampling is a very important
operation when determining reliable
testing options for assessing parti-
cle-size distribution. Operators must
follow the golden rules of sampling
in order to avoid discrepancies in the
data. They are as follows:
1. A powder should be sampled
when in motion
2. The whole stream of powder
should be taken for many short in-
crements of time rather than part
of the stream being taken for the
whole of the time
NOVEMBER 2017
Capturing a representative sample is
crucial in particle-size analysis. Im-
proper sample collection may lead
to incorrect particle-size distribu-
tion, which may lead to lower-quality
product and production losses.
Particle-size measurement is es-
sential when handing powders, to
minimize both quality and produc-
tion losses. Particle-size measure-
ment by mechanical sieve gives ac-
curate results if the particle size is
more than 38 m. Laser-diffraction
equipment is widely used for mea-
suring particle sizes less than 38 m
and up to 0.1 m. n
Edited by Suzanne Shelley
References
1. Herdan, G., Small Particle Statistics, Butterworth, Sev-
enoaks, U.K., 1952.
2. Jillavenkatesa, A., Dapkunas, S. J., Lum, L. H., Particle
Size Characterization. National Institute of Standards and
Technology, Special Publication 960-1, U.S. Government
Printing Office Washington: DC., 2001.
3. Retsch, The Basic Principles of Sieve Analysis, 2004; Ac-
cessed at www.ninolab.se/fileadmin/Ninolab/pdf/retsch/
documents/af_sieving_basics_2004_en.pdf
4. British Standards, Glossary of terms relating to particle
technology; BS 2955 1993.
5. Schulze, D., Powders and Bulk Solids: Behavior, Charac-
terization, Storage and Flow, Springer-Verlag, Berlin and
Heidelberg, 2008.
6. Mills, D., Pneumatic Conveying Design Guide, Elsevier
Butterworth-Heinemann, Burlington, Mass., 2004.
7.Stanley-Wood, N., Particle characterisation in bulk pow-
ders, in Characterization of Bulk Solids edited by Mc-
Glinchey, D., Publisher: Blackwell Publishing Ltd, U.K.,
2005.
8. Retsch, Air Jet Sieving Machine AS 200 jet; accessed
at www.retsch.com/products/sieving/sieve-shakers/as-
200-jet/function-features/, 2017.
9. Malvern, Laser Diffraction; Accessed at www.malvern.
com/en/products/technology/laser-diffraction, 2017
Author
John Lawrence serves as the
research director of KSU Bulk Sol-
ids Innovation Center at Kansas
State University (Email: jlawren@
ksu.edu), and manages the re-
search, education, training and
testing activities of the center. He
is a bulk-solids-handling special-
ist, focusing in the areas of hopper
and bin design, material-flow
properties, material quality and processing, and pneu-
matic conveying and modeling. Lawrence formerly
served as the lead researcher and director at Intelli-
Farms, a grain-management company in Missouri. He
holds a Ph.D. in agricultural and biological engineering
from Purdue University, and did postdoctoral research at
the University of Arkansas and at Kansas State Univer-
sity (Manhattan). Lawrence is also an associate editor
for the ASABE journals, and serves as program chair for
the PRS 702 group Crop & Feed Processing & Storage
of ASABE. He has published many articles and pre-
sented his research at several scientific and profes-
sional conferences. He is a member of both AIChE and
American Society of Agricultural and Biological Engi-
neers (ASABE)..
59
 Product Showcase

Advertise in
the Buyers' Guide 2018

Contact:
Diane Burleson

Tel: 512-337-7890
Fax: 512-213-4855
Email: dburleson@accessintel.com

For details visit

adlinks.chemengonline.com/66434-201

Statement of Ownership, Management, and Circulation (Requester Publications Only)

1. Publication Title: Chemical Engineering 2. Publication Number: 0009-2460 3. Filing Date: 9/26/17 4. Issue Frequency: Monthly 5. Number of Issues Published
Annually: 12 6. Annual Subscription Price $149.97. Complete Mailing Address of Known Ofice of Publication: Access Intelligence, 9211 Corporate Boulevard,
4th Floor, Rockville, MD 20850-3852 Contact: George Severine Telephone: 301-354-1706 8. Complete Mailing Address of Headquarters or General Business
Ofice Publisher: Access Intelligence, LLC, 9211 Corporate Blvd., 4th Floor, Rockville, MD 20850-3852 9. Full Names and Complete Mailing Addresses of Pub-
lisher, Editor, and Maging Editor: Publisher: Matt Grant, 9211 Corporate Blvd., 4th Floor, Rockville, MD 20850-3852 Editor: Dorothy Lozowski, 9211 Corporate
Blvd., 4th Floor, Rockville, MD 20850-3852 10. Owner if the publication is owned by a corporation, give the name and address of the corporation immediately
followed by the names and addresses of all stockholders owning or holding 1 percent or more of the total amount of stock: VSS Communications Partners, LP, 55
East 52nd Street, 33rd Floor, New York, NY 10055 11. Known Bondholders, Mortgagees, and Other Security Holders Owning or Holding 1 Percent or More of
Total Amount of Bonds, Mortgages, or other Securities: None 12. Non-proit organization: not applicable. 13. Publication: Chemical Engineering 14. Issue Date
for Circulation Data: September 2017.
Average No. of No. Copies of
15. Extent and Nature of Circulation: Copies Each Issue Single issue
During Preceding Nearest to
12 Months Filing Date
a. Total Number of Copies (Net press run) 32,908 32,795
b. Legitimate Paid and/or Requested Distribution
(1) Outside County Paid/Requested Mail Subscriptions 28,346 27.398
(2) Inside County Paid/Requested Mail Subscriptions 0 0
(3) Sales Through Dealers and Carriers, Street Vendors, Counter Sales or Other Paid
or Requested Distribution Outside USPS 2,024 2,114
(4) Requested Copies Distributed by Other Mail Classes 68 78
c. Total Paid and/or Requested Circulation 30,438 29,590
d. Nonrequested Distribution (By Mail and Outside the Mail)
(1) Outside County Nonrequested Copies 554 321
(2) Inside-County Nonrequested Copies 0 0
(3) Nonrequested Copies Distributed Through the USP by Other Classes of Mail 0 0
(4) Nonrequested Copies Distributed Outside the Mail
(Include Pickup Stands, Trade Shows, Showrooms and Other Sources) 455 455
e. Total Norequested Distribution 1,009 776
f. Total Distribution (Sum of 15c and 15e) 31,447 30,366
g. Copies not Distributed (Ofice, Returns, Spoilage, Unused) 1,461 2,429
h. Total (Sum of 15f and g) 32,908 32,795
i. Percent Paid and/or Requested Circulation 96.79% 97.44%
16. Electronic Copy Distribution: None Reported
17. Publication of Statement of Ownership for a Requester Publication is required and will be printed in the November 2017 issue of this publication
18. Signature of Fulillment Manager: George Severine Date: 9/26/17
PS Form 3526-R, July 2014

60 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017

Software New & Used Equipment

DUAL SHAFT
MIXERS
New 50, 100 & 200 gal.
mixers in stock!

Scan to learn more.

Try our mobile app:
mixers.com/web-app

1-800-243-ROSS
www.DualShaftMixers.com
For details visit For details visit For details visit
adlinks.chemengonline.com/66434-246 adlinks.chemengonline.com/66434-241 adlinks.chemengonline.com/66434-245

HEAT EXCHANGERS GET CONNECTED TODAY

Liquid Cooled
www.chemengonline.com

For details visit

adlinks.chemengonline.com/66434-242

Air Cooled
Consulting FOR GASES & LIQUIDS!
Talk Directly with Design Engineers!
CRYSTALLIZATION & Blower Cooling Vent Condensing
PRECIPITATION

(952) 933-2559 info@xchanger.com

For details visit

adlinks.chemengonline.com/66434-248

Dr. Wayne J. Genck

Genck International WABASH SELLS & RENTS
Boilers
3 Somonauk Court, Park Forest, IL. 60466 20,000 - 400,000 #/Hr.
Tel (708) 748-7200 Fax (708) 748-7208 Diesel & Turbine Generators
genckintl@aol.com http://www.genckintl.com 50 - 25,000 KW
Gears & Turbines
25 - 4000 HP
Design/Scale-up Purity We stock large inventories of:
Air Pre-Heaters Economizers Deaerators
Size Distribution Caking Pumps Motors Fuel Oil Heating and Pump Sets
Laboratory Investigations Drying Valves Tubes Controls Compressors
Pulverizers Rental Boilers & Generators
Filtration Particle Habit 24/7 Fast Emergency Service
Troubleshooting Polymorphism 800-704-2002
Product Micro-Analysis Kinetics Studies Phone: 847-541-5600 Fax: 847-541-1279
www.wabashpower.com
Industrial Seminars
wabash POWER EQUIPMENT CO.
For details visit 444 Carpenter Ave., Wheeling, IL 60090
adlinks.chemengonline.com/66434-243
For details visit
adlinks.chemengonline.com/66434-247

ADVERTISE IN THE CLASSIFIED

Contact Diane Burleson
Tel: 512-337-7890 Fax: 512-213-4855
Email: dburleson@accessintel.com For details visit
adlinks.chemengonline.com/66434-244

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 61

 New Product Information
Complimentary Subscription Application

Yes! I want to receive/continue to receive a FREE subscription to Chemical Engineering.
(Subscribers outside the USA will be served the digital edition of the magazine)
Name Title

Company

Address

City State/Province Zip/Postal Code

Country Telephone

Email | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | |

What is your title? n 03 Engineering

Fax order to: 847.291.4816 or subscribe/renew online at
n 01 Executive (Owner, Partner, President, n 04 Research & Development
CEO, COO, CFO, VP, GM, Company n 05 Chemistry/Metallurgy
www.chemengonline.com/chemical-engineering-magazine.
Official) n 06 Safety & Environmental
n 02 Manager (Director, Dept. Head, Work n 07 Sales & Marketing n 14 Catalysts 51 Chemical Distributor
Exec, Manager) n 08 Purchasing n 15 Solvents
n 03 Plant/Facility/Operations Manager n 26 Other n 16 Dyestuffs 60 Financial Services
n 04 Supervisor/Foreman Which category best describes the n 17 Industrial Gases 61 Business/Legal Services
n 05 Engineer primary end product manufactured or n 18 Other Fine/Specialty Chem 62 Consulting/Misc Services
n 06 Research/Development Manager service performed at your company? n 19 Biotechnology
n 07 Production Manager n 01 Mining, Oil, Gas n 20 Wood, Pulp & Paper 70 Engineering, Design, Construction
n 08 Purchaser/Buyer n 02 Commodity Chemicals n 21 Food & Beverages 71 Independent Laboratories, R&D
n 09 Scientist/Chemist/Metallurgist/ n 03 Inorganic Chemicals n 22 Stone, Clay, Glass, Ceramics 72 Environmenal Services
Specialist n 04 Organic Chemicals n 23 Metals
n 10 Non-technical Manager/Associate n 05 Plastics Materials & Synthetic Resins 80 Educational Services
n 11 Regulatory/Safety Manager n 06 Soaps, Surfactants, Detergents n 35 Industrial Machinery 81 Association, Society, Trade Group
n 12 Sales/Marketing Manager n 07 Pharmaceuticals, Drugs n 36 Computer Hardware/Software
n 13 Consultant n 08 Cosmetics, Personal Care n 37 Other Manufacturing (specify): 90 Government
n 18 Other n 09 Paints, Coatings & Allied Products
Please indicate ALL functions for which n 10 Petrochemicals, Refining n 40 Transportation/Storage 99 Other Non-manufacturing (specify):
you are responsible: n 11 Fertilizers, Agrichemicals n 41 Public Utilities, Waste Mgmt. ___________________________
n 01 Administration/Management n 12 Adhesives, Sealants
n 02 Plant Operations n 13 Rubber, Misc. Plastics n 50 Wholesale/Retail Trade

Fax order to: 847.291.4816 or subscribe/renew online at www.chemengonline.com/chemical-engineering-magazine.

Advertising Sales Representatives CEMAG17

North America Terry Davis Jason Bullock, CBC Diane Burleson

Matthew Grant Sales Director District Sales Manager Inside Sales Manager
Publisher, Sales & Marketing Chemical Engineering Chemical Engineering Chemical Engineering;
mattg@powermag.com 2276 Eastway Rd., Decatur, GA 30033 1940 Fountain View #514 11000 Richmond Ave, Suite 690,
Tel: 404-634-5123; Fax: 832-201-8823 E-mail: tdavis@chemengonline.com Houston, TX 77057 Houston, TX 77042
Alabama, Canada, Connecticut, Delaware, Florida, Tel: 713-974-0911; Fax: 713-952-9628 Tel: 512-337-7890
Georgia, Idaho, Kentucky, Latin America, Maine, Maryland, E-mail: jbullock@chemengonline.com E-mail: dburleson@chemengonline.com
Massachusetts, Mississippi, Montana, New Hampshire, Alaska, Arizona, Arkansas, California,
New Jersey, New York, North and South Carolina, North and Colorado, Hawaii, Illinois, Indiana, Product Showcase,
South Dakota, Ohio, Oregon, Pennsylvania, Rhode Island, Iowa, Kansas, Louisiana, Michigan, Literature Reviews,
Tennessee, Utah, Vermont, Virginia, Washington D.C., West Minnesota, Missouri, Nebraska, Classiied Display Advertising
Virginia, Wyoming Nevada, New Mexico, Oklahoma,
Texas, Washington, Wisconsin

International Dipali Dhar Ferruccio Silvera Rudy Teng

Chemical Engineering Chemical Engineering Sales Representative
Petra Trautes 40 Wall Street, 50th Floor, New York, NY 10005 Silvera Pubblicita Chemical Engineering;
Chemical Engineering Tel: 718-263-1162 Viale Monza, 24 Milano 20127, Italy 8F-1 #181 Wulin Road
Zeilweg 44 E-mail: ddhar@accessintel.com Tel: 39-02-284-6716; Hsinchu 30055 Taiwan
D-60439 Frankfurt am Main India Fax: 39-02-289-3849 Tel: +86 13818181202, (China),
Germany E-mail: ferruccio@silvera.it/www.silvera.it +886 921322428 (Taiwan)
Phone: +49-69-58604760 Katshuhiro Ishii Andorra, France, Gibraltar, Greece, Fax: +86 21 54183567
Fax: +49-69-5700-2484 Chemical Engineering Israel, Italy, Portugal, Spain E-mail: rudy.teng@gmail.com
Email: ptrautes@chemengonline.com Ace Media Service Inc., 12-6, 4-chome Nishiiko, Asia-Paciic, Hong Kong, Peoples
Austria, Czech Republic, Benelux, Adachi-ku, Tokyo 121, Japan Republic of China, Taiwan
Eastern Europe, Germany, Scandinavia, Tel: 81-3-5691-3335; Fax: 81-3-5691-3336
Switzerland, United Kingdom E-mail: amskatsu@dream.com
Japan
62 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
Advertisers Index
Advertiser............. Page number Advertiser............. Page number Advertiser............. Page number
Phone number Reader Service # Phone number Reader Service # Phone number Reader Service #

Abbe, Paul O. .........................47 Paharpur Cooling Ross, Charles & Son Co...........9
1-855-789-9827 Towers Limited.........................4 1-800-243-ROSS
adlinks.chemengonline.com/66434-18 +91 33 4013 3000 adlinks.chemengonline.com/66434-05
adlinks.chemengonline.com/66434-16
ACHEMA 2018 .......................48 Seepex Inc .............................26
adlinks.chemengonline.com/66434-08 Paratherm .............................. 19 1-937-864-7150
1-610-941-4900 adlinks.chemengonline.com/66434-07
ARC Advisory Group ............. C3 adlinks.chemengonline.com/66434-17
1-781-471-1000 Sick Inc. ..................................6d
adlinks.chemengonline.com/66434-04 Pepperl + Fuchs GmbH..........35 adlinks.chemengonline.com/66434-25
adlinks.chemengonline.com/66434-19
H. Butting GmbH Sierra Instruments, Inc. ..........57
& Co. KG ................................39 *Plast-O-Matic Valves, Inc. ..... 6i adlinks.chemengonline.com/66434-03
+49 5834 50-408 adlinks.chemengonline.com/66434-20
adlinks.chemengonline.com/66434-13 Swagelok .............................. C2
Pyromation, Inc. ..................... 13 adlinks.chemengonline.com/66434-26
Cortec Corp. ..........................47 1-260-209-6342
1-800-4CORTEC adlinks.chemengonline.com/66434-21 Tekleen Automatic
adlinks.chemengonline.com/66434-06 Filters Inc. ...............................22
Quest Integrity Group, LLC ....54 1-800-336-1942
De Dietrich Process adlinks.chemengonline.com/66434-22 adlinks.chemengonline.com/66434-27
Systems GmbH ................ 21, 57
adlinks.chemengonline.com/66434-01 RedGuard ..............................27
adlinks.chemengonline.com/66434-23
Ekato Process
Technologies GmbH ..............33 Rembe GMBH........................22
1-201-825-4684 x205 1-704-716-7022
adlinks.chemengonline.com/66434-09 adlinks.chemengonline.com/66434-24

Endress + Hauser
Consult AG ...............................3 Classiied Index November 2017
+41 61 715 7700 Advertiser Page number
adlinks.chemengonline.com/66434-10 Phone number Reader Service #
Consulting . . . . . . . . . . . . . . 61
Equipment, New & Used . . . 61
EST Group, Curtiss-Wright .....45 Engineering Software ............. 61
adlinks.chemengonline.com/66434-11
Software . . . . . . . . . . . . . . . 61
1-301-919-9670
adlinks.chemengonline.com/66434-242
Flexim GmbH .........................57
adlinks.chemengonline.com/66434-02 Genck International ................ 61 Advertiser Page number
Phone number Reader Service #
1-708-748-7200
Fluid Components adlinks.chemengonline.com/66434-243 Visimix .................................... 61
International ...........................37 +972 52 383 4174
adlinks.chemengonline.com/66434-12 Indeck Power adlinks.chemengonline.com/66434-246
Equipment Company ............. 61
Load Controls ........................53 1-800-446-3325
1-888-600-3247
Wabash Power
adlinks.chemengonline.com/66434-244 Equipment Co ........................ 61
adlinks.chemengonline.com/66434-14
1-800-704-2002
Neuhaus Neotec ....................60 adlinks.chemengonline.com/66434-247
Magnetrol.............................. C4 adlinks.chemengonline.com/66434-201
1-800-624-8765
adlinks.chemengonline.com/66434-15
Xchanger, Inc. ........................ 61
Ross, Charles & Son Co......... 61 1-952-933-2559
1-800-243-ROSS
adlinks.chemengonline.com/66434-248
adlinks.chemengonline.com/66434-241

* International Edition Vesconite Bearings ................ 61

1-866-635-7596
See bottom of opposite page adlinks.chemengonline.com/66434-245
for advertising
sales representatives'
contact information Diane Burleson
Send Advertisements Chemical Engineering, 11000 Richmond Ave, Houston, TX 77042
and Box replies to: E-mail: dburleson@che.com Tel: 512-337-7890

FOR ADDITIONAL NEWS AS IT DEVELOPS, PLEASE VISIT WWW.CHEMENGONLINE.COM

November 2017; VOL. 124; NO. 11
Chemical Engineering copyright @ 2017 (ISSN 0009-2460) is published monthly by Access Intelligence, LLC, 9211 Corporate Blvd, 4th Floor, Rockville, MD, 20850. Chemical Engineering Executive, Editorial, Advertising and Publication Offices: 40 Wall
Street , 50th floor, New York, NY 10005; Phone: 212-621-4674, Fax: 212-621-4694. Subscription rates: $149.97 U.S. and U.S. possessions, $166.97 Canada, and $292 International. $20.00 Back issue & Single copy sales. Periodicals postage
paid at Rockville, MD and additional mailing offices. Postmaster: Send address changes to Chemical Engineering, Fulfillment Manager, P.O. Box 3588, Northbrook, IL 60065-3588. Phone: 847-564-9290, Fax: 847-564-9453, email: chemeng@omeda.
com. Change of address, two to eight week notice requested. For information regarding article reprints, please contact Wrights Media, 1-877-652-5295, sales@wrightsmedia.com. Contents may not be reproduced in any form without written permission.
Canada Post 40612608. Return undeliverable Canadian Addresses to: IMEX Global Solutions, P.O. BOX 25542, LONDON, ON N6C 6B2

CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017 63

 Economic Indicators
2015 2016 2017

Download the CEPCI two weeks sooner at www.chemengonline.com/pci

CHEMICAL ENGINEERING PLANT COST INDEX (CEPCI)

625

(1957-59 = 100) Aug. '17 July '17 Aug. '16 Annual Index:
Prelim. Final Final
2009 = 521.9 600
CE Index ______________________________________________ 571.9 569.6 544.0
Equipment ____________________________________________ 690.6 686.7 649.2 2010 = 550.8
Heat exchangers & tanks _________________________________ 605.8 603.6 558.4
2011 = 585.7 575
Process machinery _____________________________________ 684.8 685.9 653.8
Pipe, valves & fittings ____________________________________ 892.7 876.6 817.4 2012 = 584.6
Process instruments ____________________________________ 406.0 403.9 391.2 2013 = 567.3 550
Pumps & compressors ___________________________________ 984.7 984.7 966.0
Electrical equipment ____________________________________ 521.7 520.8 511.6 2014 = 576.1
Structural supports & misc. ________________________________ 741.4 739.9 708.5 2015 = 556.8 525
Construction labor _______________________________________ 329.4 330.4 328.0
Buildings _____________________________________________ 562.6 561.7 548.5 2016 = 541.7
Engineering & supervision _________________________________ 311.0 313.3 314.3 500
J F M A M J J A S O N D
Starting with the April 2007 Final numbers, several of the data series for labor and compressors have been converted to
accommodate series IDs that were discontinued by the U.S. Bureau of Labor Statistics

CURRENT BUSINESS INDICATORS LATEST PREVIOUS YEAR AGO

CPI output index (2012 = 100) ____________________________________________________ Sept. '17 = 100.0 Aug. '17 = 100.8 Jul. '17 = 101.8 Sept. '16 = 99.6
CPI value of output, $ billions _____________________________________________________ Aug. '17 = 1,823.5 Jul. '17 = 1,810.7 Jun. '17 = 1,800.5 Aug. '16 = 1,705.8
CPI operating rate, % __________________________________________________________ Sept. '17 = 74.9 Aug. '17 = 75.6 Jul. '17 = 76.3 Sept. '16 = 75.1
Producer prices, industrial chemicals (1982 = 100) ____________________________________ Sept. '17 = 249.3 Aug. '17 = 249.9 Jul. '17 = 244.0 Sept. '16 = 229.7
Industrial Production in Manufacturing (2012=100)* ____________________________________ Sept. '17 = 103.0 Aug. '17 = 102.9 Jul. '17 = 103.2 Sept. '16 = 102.0
Hourly earnings index, chemical & allied products (1992 = 100) ____________________________ Sept. '17 = 180.3 Aug. '17 = 177.3 Jul. '17 = 179.8 Sept. '16 = 169.8
Productivity index, chemicals & allied products (1992 = 100) ______________________________ Sept. '17 = 98.6 Aug. '17 = 101.0 Jul. '17 = 102.9 Sept. '16 = 101.4

CPI OUTPUT INDEX (2000 = 100) CPI OUTPUT VALUE ($ BILLIONS) CPI OPERATING RATE (%)
110 2300 80

105
2200 78
100
2100
95 76
2000
90
74
1900
85
72
80 1800

75 1700 70
J F M A M J J A S O N D J F M A M J J A S O N D J F M A M J J A S O N D

*Due to discontinuance, the Index of Industrial Activity has been replaced by the Industrial Production in Manufacturing index from the U.S. Federal Reserve Board.
For the current months CPI output index values, the base year was changed from 2000 to 2012
Current business indicators provided by Global Insight, Inc., Lexington, Mass.

CURRENT TRENDS

T he preliminary value for the August CE

Plant Cost Index (CEPCI; top; most
EXCLUSIVE AD SPACE AVAILABLE! recent available) increased compared to
the previous months value. The increase
Feature your marketing message alongside this popular editorial department
was driven by rising values for several (but
Each issue includes editorial departments that feature the current industry trends and not all) equipment subindices, including
the Plant Cost Index. As one of the most valued sections in the magazine, your ad is Pipes, Valves and Fittings and Process In-
guaranteed to reach decision makers each month. Ad runs opposite Cover 3 within struments. While the August value for the
Equipment subindex was up as a whole,
the Economic Indicators department.
the subindices for two of the major subin-
Contact your sales representative for more information: dices (Construction Labor and Engineer-
ing & Supervision) were down from the
previous months values. The preliminary
JASON BULLOCK TERRY DAVIS PETRA TRAUTES overall monthly CEPCI value for August
jbullock@chemengonline.com tdavis@chemengonline.com ptrautes@accessintel.com 2017 stands at 5.1% higher than the
713-974-0911 404-634-5123 +49 69 58604760 corresponding value from August 2016.
27206
Meanwhile, the latest Current Business In-
dicators (CBI; middle) saw a small decline
in the CPI Output Index for September.
64 CHEMICAL ENGINEERING WWW.CHEMENGONLINE.COM NOVEMBER 2017
CHEMICAL ENGINEERING For details visit adlinks.chemengonline.com/66434-04
WWW.CHEMENGONLINE.COM NOVEMBER 2017 3
break through
the

NOISE

Better Signal-to-Noise Ratio Means

Better Level Control Performance
While transmit pulse amplitude (signal size) has helped to make
guided wave radar technology the standard for accurate, reliable level
4.40 measurement, the fact is signal-to-noise ratio (SNR) represents a far
Model 706
more critical indicator of level control performance. For superior SNR
Higher SNR
in all process conditions, no other GWR device beats the Eclipse
1.57 Model 706 transmitter from Magnetrol.
Competitor
SNR To learn more about the breakthrough ECLIPSE Model 706 GWR
transmitter visit radar.magnetrol.com or contact your
The ECLIPSE Model 706 transmitter has a
signal-to-noise ratio nearly 3 times higher MAGNETROL representative today.
than competitors.

magnetrol.com 800-624-8765 eclipse.magnetrol.com 2017 Magnetrol International, Incorporated

For details visit adlinks.chemengonline.com/66434-15