Chemical Engineering and Processing 48 (2009) 10891104

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Chemical Engineering and Processing:
Process Intensication
j our nal homepage: www. el sevi er . com/ l ocat e/ cep
Review
Equipment improvement trends in distillation

Z. Oluji c
a,
, M. Jdecke
b
, A. Shilkin
b
, G. Schuch
b
, B. Kaibel
c
a
Delft University of Technology, Process & Energy Laboratory, Leeghwaterstraat 44, 2628 CA Delft, The Netherlands
b
BASF SE, GCT/C - L540, 67506 Ludwigshafen, Germany
c
Julius Montz GmbH, Hoffstrasse 82, Hilden, Germany
a r t i c l e i n f o
Article history:
Received 6 February 2009
Received in revised form 18 March 2009
Accepted 19 March 2009
Available online 26 March 2009
Keywords:
Distillation
Packed columns
Tray columns
Dividing wall columns
Energy saving
a b s t r a c t
Answering to the challenges imposed by industrial growth, the distillation, which is the most mature
among separations regarding the applications and technology development, still manages to improve
and fromtime to time a technology breakthrough occurs which moves this proven technology to a higher
level of sophistication. The purpose of this presentation is to address the recent distillation equipment
developments, particularly those BASF, Montz, and TU Delft were involved with.
2009 Elsevier B.V. All rights reserved.
Contents
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1089
2. Energy saving column congurations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1090
2.1. Dividing wall column (DWC) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1090
2.2. Internally heat integrated distillation column (HIDiC) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1091
3. Unusual applications . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1092
4. Equipment advances . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1093
4.1. Random and structured packings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1093
4.2. Trays . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1095
4.3. Complex contactors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1096
4.4. Scale of equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1097
5. Equipment modelling advances. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1100
6. Equipment testing facilities/standards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1101
7. Concluding remarks . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1102
Acknowledgements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1103
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1103
1. Introduction
Distillation is the most practical and hence most widely uti-
lized uid separation technology in process industries. However,
it is capital- and energy-intensive and, with decreasing relative
volatility, the size and energy requirements of a column tend to

Extended version of a paper presented jointly by M. Jdecke and

Z. Oluji c at
ProcessNet Annual Meeting, held on 79 October 2008, in Karlsruhe, Germany.

Corresponding author. Tel.: +31 15 278 66 74; fax: +31 15 278 69 75.
E-mail address: z.olujic@tudelft.nl (

Z. Oluji c).
increase, whiletheenergyefciencyof theseparationprocess tends
to decrease [1,2]. Indeed, a weakness of distillation represents its
relatively low energy efciency.
This is a fact, and in answer to globally proclaimed need for a
more sustainable process industry, distillation has become the tar-
get of efciency increasing efforts, by improving the equipment,
or by combining it in an effective way with other separations or
reactions. One should note that under the ag of so-called process
intensication effort, there are some ongoing attempts to arrive
at a more compact equipment by employing external elds, like
centrifugal force, sound or microwaves. There are also some more
radical efforts goingon, i.e. those orientedtowardreplacingexisting
0255-2701/$ see front matter 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.cep.2009.03.004
1090

Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104
Fig. 1. Photograph of a 7-m diameter column during transport at the site.
by a to be invented, much more efcient vapour/liquid contactor
to be used in conjunction with distillation, which however appear
to be fruitless so far.
For a large industrial company, the main reason to implement
innovations into the distillation technology represents its demand
to stay competitive, i.e. to minimize capital expenditures and oper-
ating costs while increasing the productioncapacity. Inthis respect,
the main activities are focused on improving/enhancing perfor-
mance characteristics of vapour/liquidcontactors, i.e. trays, random
and structured packings. The latter are frequently offered by Indian
and Chinese manufactures at substantially lower prices as com-
pared to the established manufacturers in Europe and USA, the
more attractive prices being however counterbalanced by uncer-
tainties regarding their performance characteristics.
Fig. 1 shows a photograph of a 7-m diameter column during
transport to installation location in a BASF plant. Indeed, a large
column. However, present day worldscale plants require frequently
larger diameter columns to be installed. In order to minimize the
investment costs, more accurate designs with less safety margins
are required, realized with the aim of appropriate design tools and
know-how. Distribution of phases becomes again a major concern.
Without a possibility to perform adequate tests there will be a lack
of data necessary to verify the predictive models appropriately. This
and other column size and equipment performance related ques-
tions are somethingpresent daycolumndesigners have todeal with
on daily basis.
The objective of this paper is to give a survey of recent devel-
opments in the eld of distillation equipment and to indicate
challenges in this respect.
2. Energy saving column congurations
2.1. Dividing wall column (DWC)
Interestingly, it took more than 10 years after rst applica-
tion at BASF, in 1985, before other companies have realized and
consequentlyexperiencedthat makingadequateprovisions for sep-
arations of three component feeds into pure products within one
shell, where appropriate, enables saving of both operating and
investment costs [35]. At present there are more than 70 packed
DWC columns operated by BASF worldwide.
Successful implementationof DWCconcept represents anexam-
ple of a recent technology breakthrough in the eld of distillation
with potential for further exciting developments. Namely, upon
successful implementation of unxed wall technology, which
enabled signicant expansion of the application window (see
Fig. 2), the DWC became a very attractive option not only for
the separation of three-component mixtures but also of mixtures
Fig. 2. The number of the dividing wall columns deliveredby J. Montz over the years.
containing larger number of components within a single shell
[6,7].
Fig. 3 shows a photograph of the shell (3.6m internal diameter
and of 34m height) and a drawing illustrating schematically the
internal conguration of a recently build packed DWC for the sep-
aration of a four component mixture into pure substances under
deep vacuum, incorporating various components of process and
mechanical designrelatedproprietaryknowledgeof BASF SEand/or
J. Montz GmbH. Striking is the complexity of the internal design of
this column, containing in total eight wire gauze packing (Montz
A3-500) beds. Several beds of different height and cross-sectional
area are separated by the un-xed dividing walls, some of them
being in an off-centre position. Proprietary reux splitters and liq-
uid distributors are installed to handle properly different, in some
cases extremely low specic liquid loads (about 0.1m
3
/m
2
h).
One should bear in mind that similar to the separation of three
component mixtures, a column for separation of four components
can be designed with a single dividing wall. However, in case of
a sharp separation between two medium boiling components, this
would lead to a formation of additional entropy of mixing and, con-
sequently, to a poor performance with respect to energy saving
potential. To minimize the energy consumption, a more complex
columncongurationis thought, withthreedividingwalls arranged
to create above and bellow the feed sections with three beds in
parallel [7]. Even more complex congurations can be expected
when dealing with ve or more component mixtures, but this is
something not attempted yet in industrial practice.
A specic feature of a packed DWC is that liquid distribution to
separated column sections can be controlled by mechanic means
whereas the vapour distribution is dictated by the pressure drop of
the internals. Being the key designvariable, the pressure drophas to
be ne-tunedto t to the requiredliquidto vapour ratios. The latter,
in turn, requires an accurate prediction of the total pressure drop
at various operating conditions considering the packing and the
contribution of the auxiliary equipment, i.e. liquid collectors and
distributors installed. The pressure drop associated with the use
of most commonly utilized internals, i.e. chevron (vane) type and
chimney type liquid collectors and narrow trough (gravity) liquid
distributors canbe estimated withfair accuracy using a simple, rst
principles based method proposed most recently by Rix and Olujic
[8].
Certainly, a considerable research effort preceded the indus-
trial implementationof the un-xedwall technology. The necessary
knowledge of hydrodynamics of un-xed wall DWC was collected
during air/water and tracer experiments supported by BASF and
carried out in Hilden, Germany jointly by J. Montz and TU Delft
using the test equipment of semi-industrial scale (internal diame-
ter of 0.8m). These experiences helped to develop the full design
and construction know-how that represents nowadays a basis for
the realization of much larger packed columns than those in the

Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104 1091

Fig. 3. A photograph of the shell and a drawing illustrating internal conguration of a DWC for separation of a four component feed into pure products.
verybeginningof DWCapplications (diameters rst well below1m,
now up to 4m, some columns up to 80m tall).
In the meantime J. Montz developed the know-how for imple-
mentation of un-xed wall in conjunction with tray columns [6].
However, experience with the rst industrial DWC equipped with
trays must be collected to prove whether benets similar to those
experienced with packed columns can also be expected. Generally,
DWCs made recently a successful inroad into the renery world
dominated by large tray columns, and this is becoming a fast devel-
oping application eld. The dimensions of largest tray DWCs are
impressive: diameters of around 6m and more than 100m tall
[9,10]. DWCs can be equipped also with random packings, where
appropriate. Constructional and design aspects of DWCs are elabo-
rated in more detail elsewhere [7].
Most recently, a model system based R&D effort has been com-
pleted indicating that further synergetic effects can be obtained
by combining reaction and separation in a DWC [11,12]. Recent
academic research performed at/or in co-operation with Ger-
man universities [1315] has contributed to increase the public
knowledge on operation and control of DWC. Prediction of overall
performance is becoming a routine calculation; however, the pre-
dictive models capable of dimensioning a DWC are still not publicly
available. With increasing academic interest for DWC, this situation
may change soon.
2.2. Internally heat integrated distillation column (HIDiC)
Indeed, a DWC, which is a thermodynamic equivalent of ther-
mally coupled (Petlyuk) columns, reduces the energy requirement
by around 30% compared to that of conventional two-column con-
gurations. However this is a solution for a rather specic class of
distillation applications. In order to achieve substantial energy sav-
ings, the distillation columns used for separation of close boiling
mixtures at largest industrial scale should be targeted rst. In such
applications reboiler duties between 20 and 80MW are common.
Where appropriate (stand-alone columns), the implementation of
heat pump assisted distillation is a most effective, but also a highly
cost-intensive solution.
In this respect, further improvement is expected from the so-
called internally heat integrated distillation column (HIDiC) which
combines direct vapour recompression and diabatic operation, i.e.
allows performing a distillation process at lowest feasible energy
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Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104
Fig. 4. Schematic of congurations of a vapour recompression column (left) and an
internally heat integrated distillation column (HIDiC).
requirement, close to theoretical minimum [16,17]. Fig. 4 shows
a conventional vapour recompression (heat pump) column and a
HIDiC.
However, to enable the transfer of the required amount of heat
from hot rectication to cold stripping section, each stage requires
additional heat exchange area, which needs to be installed above
the active area of a tray preferably in stripping section. Prelimi-
nary pilot scale tests performed at TU Delft have indicated that an
annular sieve tray equipped with heat transfer panels can function
accordingly [18]. Next step is operation of a prototype concentric
column (outer diameter of annular stripping section is 0.8m and
the internal diameter of rectication section is 0.3m) with ve
fully integrated trays. By the aid of this column, further experience
withthefunctionalityof aHIDiC, mechanical designandinstallation
aspects should be collected, providing a solid basis for the design of
an industrial demonstration column. In the meantime, a Japanese
research consortium has already succeeded to demonstrate the
functionalityof aHIDiCinindustrial practice[19]. However, this was
done by placing in a shell a number of unit-size concentric packed
columns in parallel. Therefore, this HIDiC conguration appears to
be industrially unviable, since it implies a linear relation between
capacity and capital investment, while the distillation is a typical
economy of scale technology.
Presently, in addition to the pilot-scale experiments with the
concentric tray column mentioned above, TUDelft is involved with
evaluation of HIDiC as a potential retrot technology for the self-
standing propylene manufacturing plants. The objective of this
work is to see whether the production capacity of these plants can
be increased well beyond that achievable through replacement of
existing trays with high capacity trays. This approach relies on the
idea that the existing shell(s) can be rearranged to obtain two nor-
mally operating parts of the rectication section placed in parallel.
These must be connected with a concentric HIDiC unit with strip-
ping stages integrated with equivalent number of stages from the
upper part of the rectication stages. It is expected that combin-
ing debottlenecking with energy saving in an effective way (saving
energy and capital compared to conventional schemes) will be con-
vincing enough for the industry to support further development
and implementation of HIDiC. Design features of a new HIDiC and
a comparison with a state of the art, heat-pump assisted (direct
vapour recompression) propylenepropane splitter can be found
elsewhere [20].
Another approach to implement the HIDiC concept is based
on the idea of transforming the well-established plate-n heat-
exchangers into a fractionating falling lm type device. This line
of development is pursued by the Energy Centre of the Netherlands
(ECN) and the purpose of the present project is to provide an exper-
imental proof of this principle [21]. The bench scale unit has been
designed and delivered to TU Delft to be evaluated thoroughly as a
joint activity of ECN and TU Delft. In Japan, the plate n approach
has been developed from the beginning of HIDiC implementa-
tion related research activities within a separate project devoted
to improving energy efciency of air distillation process. Now this
fully governmentally supported project carried out by Tayio Nissan
Corporation (former Nissan Sanso or Japan Oxygen Corporation)
has reached the nal, industrial demonstration stage. According to
the latest information [22], a 7t/h HIDiC unit has been built in par-
allel to a standard 85t/h production unit at an industrial site. It is
expected, that after several months of continuous operation and
performance tests, a clear picture can be obtained about indus-
trial viability of HIDiC in this ever growing distillation application
eld.
3. Unusual applications
There are numerous separations technologies available; how-
ever, if an ultra high purity product is required, distillation is
usually preferred over other methods, despite extremely low rel-
ative volatilities and small production capacities. Obtaining and
purication of oxygen-18 (
18
O
2
) is an example of such a highly
demanding, but extremely effective isotope separation process
introduced recently by Taiyo Nissan Corporation [23]. High purity
18
O
2
became a demanding product upon advent and establishment
of Positron Emission Tomography (PET) as a diagnostic method for
detectingcancers. Namely, 18-Oxygenuponhydrogenationis trans-
ferred into oxygen-18 water (H
2
18
O), which serves as basis material
for manufacture of an effective uoro-glucose type cancer-marker
used in conjunction with PET.
Fig. 5. Basic owsheet of distillation based process for production of oxygen-18 water [23].

Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104 1093

Table 1
Isotopic composition of natural oxygen [23].
Oxygen isotope Molecular weight Composition
16
O
2
32 0.99519
16
O
17
O 33 0.00074
16
O
18
O 34 0.00407
17
O
2
34 0.1ppm
17
O
18
O 35 1.5ppm
18
O
2
36 4.2ppm
The basic owsheet of this process is showninFig. 5. The starting
material is commercial grade oxygen stream from air separation,
cryogenic distillation unit, which is treated in a tray column to
obtain the ultra-pure oxygen. The composition of this natural oxy-
gen stream, containing three isotopes is shown in Table 1, and the
differences in boiling temperatures are less than 1K. Also oxygen-
18 is present in this mixture, but in an extremely small quantity
to be extracted. Therefore, the
16
O
18
O isotope has been taken as
source of
18
O. Nine packedcolumns containinga structuredpacking
are used in the
16
O
18
O enrichment section and roughly a 500-
fold enrichment was required to arrive at a satisfying composition
level, prior to entering the specially designed isotope exchange
reactor. In the reactor, roughly 1/4 of the
16
O
18
O is transformed
into
18
O
2
. The reactor efuent enters the
18
O
2
enrichment and
puricationsectioncontaining four packedcolumns equippedwith
specially designed random packing. Pure oxygen-18 is fed to a
hydrogenation reactor generating H
2
18
O. In addition to a reboiler
and a condenser, each of 13 packed distillation columns has a liquid
reservoir to provide for intermediate hold-up needed for start-
up in case of emergency. One should note that the start up time
for this peculiar plant was 6 months, which is much less than 2
years as encountered in H
2
18
O manufacturing plants developed
for unknown purposes in USA and Israel in cold war time. Also
it is interesting to mention that one tray and 13 packed columns
are placed within a 7m3.5m70m cold-box with an operating
temperature of around 90K, maintained by circulating commer-
cial grade nitrogen. The waste nitrogen and oxygen are recycled to
the air separation unit, which makes this plant into a zero-emission
unit. The production capacity of this quite large, continuously oper-
ating, multi-column unit is 100kg/year of high purity H
2
18
O for
medical use, whichrepresents one-thirdof present needs andsome
100kg/year of low purity H
2
18
O for industrial use. Indeed a quite
untypical but highly effective low energy application of distilla-
tion.
Although the cold box is well insulated (perlite), an extremely
low operating temperature results into a rather large inux of heat
which must be accounted for in design calculations. The so-called
Simultaneous Heat and Mass Transfer model, which was origi-
nallydevelopedtodeal withmass transfer incryogenic distillations,
proved to be a powerful design tool in conjunction with character-
istic diffusion coefcients determined experimentally. A detailed
description of this rate-based model can be found in the book by
Koichi Asano [23].
Unfortunately, the sub-chapter describing above mentioned
oxygen-18 separation and purication process does not provide
any information on the type and size of the structured packing
used. However it is well known that structured packings were orig-
inally developed for the heavy water-water distillation, which, due
to a rather low relative volatility (below 1.05) represents a very
demanding separation task. Indeed, Sulzer wire gauze BX pack-
ing, as well as Montz A3, with a specic geometric area of around
500m
2
/m
3
and a corrugation inclination angle of 60

, proved to
be an optimal solution for this, as well as for other numerous ne
chemicals separations under vacuum.
4. Equipment advances
The key to successful implementation of energy and/or invest-
ment costs saving congurations of distillation columns represent
novel, better performing vapourliquid contacting devices suitable
for a particular separation task. Since user companies strive to
increase production with minimuminvestment, retrot of existing
columns is a frequent optionimplying replacement of existing trays
or packings with an effective alternative device. Presently, vacuum
applications are dominatedbystructuredpackings, whereas inhigh
pressure applications (above 5bar), trays are usually employed.
Also randompackings can nd a favourable application in the com-
plete operating range. To cope with the ever growing demand on
capacity, all three families of vapourliquidcontactors were subject
to intensive research and development in recent years.
In the meantime, a number of well established tray and/or pack-
ing manufacturers have been taken over by either Koch or Sulzer.
These two companies grow bigger and cover the largest part of
distillation equipment market. But also smaller companies, like J.
Montz, Raschig and Rauschert, owning to their innovative solutions
manage to keep their share on the market. Finally, many existing
and new small manufacturers around the world offer well proven
trayandpackingdesigns that arenot anymoreprotectedbypatents.
Besides the new products offered by the well known equip-
ment manufacturers, there is an increasing number of commercial
products coming mainly from China. Chinese manufacturers claim
high performance and offer their trays and packings at much
lower prices. However, these high performance claims are not
yet supported by hard experimental evidence thus making the
implementation of such signicantly cheaper products in plants of
American and European companies less probable.
4.1. Random and structured packings
Upon its introduction some 10 years ago, the Raschig Super Ring
(see Fig. 6a), the newest development in the eld of random pack-
ings [24], made an inroad and the number of industrial applications
is steadily growing. Newest evidence conrms the favourable per-
formance characteristics of this superb packing [25].
Similar trend occurred with the introduction of latest genera-
tion of structured packings, so-called high capacity/performance
structured packings (Koch-Glitsch HC, Montz M and MN, and
Sulzer MellapakPlus series) [26]. Thanks to an effective develop-
ment, these new generation packings (see Fig. 6b and c) can be
used to replace the conventional counter-parts allowing a signif-
icant capacity increase, depending on process conditions. Sulzer,
Koch-Glitsch and Montz offer these packings in specic area sizes
matching the specic needs of various industrial applications (see:
www.sulzer.com, www.koch-glitsch.com and www.montz.de).
As mentioned above, new players on column internals market
come from Far East countries, with relatively cheap products that
are announced as being competitive or even better than the most
advanced designs of well established manufacturers. Fig. 7 shows
a photograph of a high performance structured packing (TJH255)
made available throughTianjinCorporationfromPRChina [27]. The
maindistinctive feature of this packing is that inadditionto smooth
bends at both ends of corrugated sheets there is an additional bend
inthe middle of the corrugatedsheets. Therefore, it is not surprising
that this packing that resembles the MellapakPlus 252.Y exhibits a
pressure drop in between conventional and high capacity Mellapak
packings (see Fig. 8).
Indeed, avoiding sharpbends, i.e. anabrupt change of the vapour
owdirectionat the transitionbetweenthe packing elements leads
toa signicant pressure dropreductionincase of commonpackings
with corrugation inclination angle of 45

. However, experimental
evidence has demonstrated that the bottom part of corrugations is
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Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104
Fig. 6. Photographs of high performance randompacking and structured packings (a) Raschig super ring, (b) Montz-pak B1M, (c) Mellapak Plus and (d) Raschig Super Packing.
critical with respect to capacity, because the bends in bottom part
are essential for a smooth drainage of the liquid [28,29]. Another
important consideration represents the effect of the ow channel
geometry modications on the packing efciency. First generation
of Montz high capacity packings is characterized by a relatively
long bend in the bottom part of corrugations (B1-M series). Total
reux distillation tests have proved both a considerable pressure
drop reduction and a substantial gain in capacity at the same
packing efciency with respect to conventional design. However
a certain loss in efciency was observed in the preloading region
[30]. This issue has beenaddressedbythe further development and,
after some effort, anoptimized, highperforming congurationwith
reduced length of the bend and slightly changed corrugation incli-
nation angle emerged which is commercially available as B1-MN
series [31]. This exercise was interesting because it indicated that
with ne-tuning of the corrugation geometry further performance
improvements canbe achieved. For instance, the well knownMontz
low pressure drop A3 gauze packing (corrugation inclination angle
of 60

), with a long bend in the bottom part of corrugations does

not bring more capacity but reduces the pressure drop by 20% with
respect to that of original packing, at the same efciency [31]. Sim-
ilar gains can be expected from high performance version of well
know Sulzer BX packing. This small but very effective modication
of the packing geometry is a valuable development, particularly for
deeper vacuum applications, where each millibar of pressure drop
counts. Signicantly cheaper metal sheet counterparts, having the
same specic geometric area as common wire gauze packings (e.
g. B1-500MN and expanded version, i.e. BS-500MN [31]), as well
as MellapakPlus 752.Y [32] perform very well and preserve their
efciency over the whole range of vapour and liquid loads encoun-
tered in typical total reux distillation experiments. However, due
to a smaller corrugation inclination angle (even below 45

) their
pressure drop is too high to be considered suitable for applications
traditionally dominated by BX and A3 packings. In a most recent
paper introducing a new type of wire gauze packing with a spe-
cic geometric area of 900m
2
/m
3
, Luo et al. [33] demonstrate a
relative performance advantage of reducing the corrugation base
to corrugation height ratio from common 2 to below 1. This mod-
ication was evaluated earlier in Delft [28], and it proved to be
favourable withrespect topressure dropandcapacity. Because such
a conguration discourages the owof liquid lmover corrugation
ridges, it was considered to be decient with respect to mass trans-
fer efciency. However, with corrugation ridges rounded, as it is
done in this case, and under low liquid load conditions, this pack-
ing could achieve a good active wetting of the surface. However,
as observed in total reux experiment, it behaves similar to com-
mon gauze packings, exhibiting a strong decline in efciency with
increasing F-factor.
Although there is theoretically still some potential for enhance-
ment of the performance of corrugated sheet structured packings,
it seems that limits for practical improvement of this superb
vapour/liquid contacting device are close. However, according to
preliminary tests, a new design of structured packing, introduced
recently under the name Raschig Super Packing (see Fig. 6d),
looks promising regarding the potential for further performance
improvement [3436].
However, the reduction in pressure drop, mainly due to elim-
ination of sharp bends in the ascending vapour ow at transition
between packing elements (layers) and a shorter, nearly vertical
ow path, could lead to increased sensitivity to maldistribution in
vapour phase. The same may occur withthe liquid, because the new
quite open structure does not encourage lateral transport of liquid

Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104 1095

Fig. 7. Photograph of TJH255 structured packing.
to the extent encountered in beds consisting of corrugated sheet
structured packings. First industrial applications in columns with
diameters well above 1mshould verify this hypothesis. Mechanical
design and installation aspects as well as related cost are another
unknown factor and the overall picture needs to be well balanced
to challenge the market position of established corrugated sheet
structured packings.
Fig. 8. Pressure drop of TJH255 structured packing, compared to that of Mellapak
250.Y and Mellapak 252.Y.
4.2. Trays
Some 20 years ago it became obvious, that structured packings
are not capable of performing accordingly in the separations at
higher operating pressures. This has led to activities towards the
improvement of tray type devices in order to achieve higher capac-
ity at an affordable pressure drop with an acceptable penalty on
separation efciency.
A specic, nowwell established and widely employed advance-
ment in this area represent the so-called xed-valve trays, which
combine in a cost effective way some benets of sieve and
valve trays, operating at comparatively higher vapour load. The
capacity of both conventional and novel trays can further be
increased simply by placing random or structured packing on or
above the active area of the tray. However, such a combination
seems to offer advantages only at low to moderate liquid loads
[37].
The ultimate developments in these respect are centrifugal
devices like Swirltube tray and ConSep tray from Shell and Sulzer
[3841], and Ultra-Frac tray from Koch-Glitsch [42,43]. Swirltube
and UltraFrac combine phase contact and separation, while Con-
Sepcombines a sieve traywitha cyclonic device. ConSeptraydesign
allows operation at the vapour loads above the system limit, lead-
ing to a complete entrainment of the liquid which after a short but
intensive contact is separated from the vapour in a battery of pro-
prietary axial cyclones installed above the active area. Compared to
a VGPlus tray, a ConSep tray allows a capacity increase of impres-
sive 50%, but at lower efciency, which however is large enough to
satisfy the needs of typical applications. It is worth noting, that the
pressure drop associated with the operation of such devices is sub-
stantiallyhigher thanthat of theconventional trays; this aspect may
limit the number of potential applications signicantly. Although
according to Koch-Glitsch [43] the pressure drop of UltraFrac is
signicantly lower than that of ConSep, this claimed advantage
requires a direct experimental conrmation to be accepted.
A promising development in this respect represents a so-called
JCPT-Coow-Tray of Tianjin Corporation [27], shown in Fig. 9. The
drawingaccompanyingthe photographof a test unit made tot into
a 0.5 internal diameter column hydraulics simulator illustrates the
working principle of this device, which employs a structured pack-
ing as a demister. Fig. 10 demonstrates the pressure drop, weeping
and entraining tendency expressed as a function of the gas load fac-
tor at constant liquidload, measuredat BASF usingair-water system
at ambient conditions. Obviously, the pressure drop of the JCTP-
Coow-tray is much lower, nearly one half of that of a MVG-tray at
the same gas load. This indicates that at the same pressure drop, a
JCPT-Coow tray would enable a capacity increase well above 30%.
The question is whether this tray, which weeps at comparatively
higher gas load, will exhibit such a good efciency as experienced
with MVG trays.
Regarding the fact that all these high-capacity trays, by virtue
of their operation cause large pressure drop, one should keep
in mind that for tray column applications where the pressure
drop is critical, employment of UOPs slotted sieve trays could
be considered [44]. These rst-generation high-capacity trays
combine high efciency (large ow path lengths) with low pres-
sure drop and have been improved in the meantime. Todays
optimized tray-deck designs eliminate vapour cross-ow chan-
nelling by preventing hydraulic gradient formation via slots with
variable density and directionality, bubble promoters, and fully
active bubbling areas. With this a uniform froth height is main-
tained and consequently a uniform vapour distribution across
the entire tray ensured. These well proven trays are particularly
suitable for tray columns with extreme diameters, and, impor-
tantly, can be installed with rather low tray spacing, usually
0.30.5m.
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Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104
Fig. 9. Photographof JCPTCoowtray, made tot intoBASF 0.5mcolumnhydraulics
simulator.
4.3. Complex contactors
It is well known that in the loading range, characterized by a
sharp increase in the liquid-holdup, the efciency of both random
and structured packings tends to improve signicantly. However,
this occurs in a relatively narrow range at relatively high vapour
loads in an immediate proximity to the ooding point. Therefore,
to avoid the sudden loss of efciency, the packed columns are
designed to be operated at a safe distance from this point.
However, to realize a rather large potential gain in efciency
within the loading range, an operation under partly ooded con-
ditions achieved in a controlled way inside a column containing
common packings and/or catalytic packings is required. The effort
Fig. 10. Pressure drop, entrainment and weeping characteristics of JCPT CoowTray
compared to that of a MVG (Sulzer) tray.
Fig. 11. An element of sandwich packing consisting of structured packing placed
above a partial ooding generating device.
spent inthis directionat BASF over the years indicates that so-called
sandwich packing that consists of structured packing elements
separated by specially designed ooding promoting devices (see
Fig. 11) canensureastableoperationof apartlyoodedbed[4547].
As showninFig. 12, this is accompaniedby a relatively large specic
pressure drop. However, inapplications where this canbe tolerated,
such a complex conguration, which allows increased efciency
without loss of capacity, could bring economic benets.
Fig. 12. Pressure drop of sandwich packing.

Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104 1097

Fig. 13. Schematic of the structure of KatapakSP packings.
Operation under increased liquid holdup is generally benecial
if reactions are carried out in combination with distillation. For het-
erogeneously catalyzed reactions, the contactor needs to be equally
functional onbothreactionandthe separationside. Sulzer Katapak-
SP series of commercially available catalytic structured packings
is built of packing elements/segments of unit height, which com-
prise catalyst containing pockets separated by corrugated sheets.
The corrugated sheets used in conjunction with Katapak-SP are
those encountered in MellapakPlus 752.Y, a large specic geomet-
ric area, high performance structured packing. A specic feature
of Katapak-SP packing is that it allows a certain degree of exi-
bility with respect to the area/volume occupied by reaction and
separation parts. Fig. 13 shows schematically the structure of two
commercially available versions of this packing, Katapak-SP 11 and
Katapak-SP 12 with respectively one and two corrugated sheets
placed in between catalyst containing elements [48]. However, one
should realize that Katapak-SP 11, Multipak [49] being its predeces-
sor, and Katapak-SP 12 exhibit different uid-dynamic behaviour
and, consequently, different mass transfer efciencies [48,50]. For-
tunately, the effect of Katapak-SP element conguration, including
those containing 3 or more sheets placed in between catalyst con-
taining elements, on hydraulics and mass transfer performance of
the packed bed can be predicted with condence using a parallel-
channel model developed recently at TU Delft [50].
Another point of concern with scale-up and application of these
packings is that a certain liquid load is required to get the catalyst
containing pockets saturated with owing liquid [51], which, how-
ever, is well above the operating one as observed in recent pilot
scale total reux distillation experiments [50]. This means that the
catalyst will not be used fully. On the other hand, if the column liq-
uid load is above the liquid percolation rate through the catalyst,
the excess liquid will bypass the pockets thus avoiding the reaction
zone. This liquid will however mix with the liquid leaving the pock-
ets, both mixing at the transitions between packing elements with
the liquid coming from the corrugated sheets. All these and other
performance affecting factors must be taken into consideration by
the column designers.
A practical solution could be to have catalytic packing sec-
tion partly ooded, as discussed earlier. However, as observed
in air/water hydraulics experiments reported elsewhere [52], if
a section of catalytic packing is placed between two sections of
structured packing in a reactive distillation column with constant
diameter, the transition between the upper structured packing bed
and the catalytic packing is the place of the onset of loading, and
with increased gas load the liquid build-up will progress upwardly
leading to the ooding of the upper bed and, eventually, the whole
column will become hydraulically inoperable.
Althoughtheconventional methods for determinationof theliq-
uid holdup give a fair picture of the uid-dynamic behaviour of
catalyst containing pockets, a more detailed insight, with respect
to spatial distribution of liquid in such structures can be expected
from more sophisticated, non-invasive measurement techniques.
Preliminary data obtained at the University of Liege indicate that
promising results in this respect can be expected from dedicated
tests performed using the state of the art X-ray computed tomog-
raphy [53,54].
4.4. Scale of equipment
Due to mechanical and investment cost related limitations, the
tallest distillation columns do not exceed 110m. If the number of
required trays in conjunction with chosen tray spacing(s) exceeds
the number tting into this height, two column shells are con-
nectedinseries. Typical examples of twoshells inseries arepolymer
grade propylene-propane splitters designed to operate at pres-
sures around 20bar to enable condensation of overhead vapour
using water. The newer design, particularly those in stand-alone
propylene plants are heat pump assisted columns which operate
at pressures around 10bar, which substantially increase the rela-
tive volatility. The latter enables an installation of all required trays
into one shell as well as operation at signicantly reduced reux
ratio.
Although handling large feeds (often larger than 100t/h) in con-
junctionwithhighreux ratios (up to 20) high-pressure distillation
columns rarely exceed 6min diameter. In other words, the column
diameter tends to increase with decreasing operating pressure,
i.e. vapour density. For instance, typical diameters of present days
ethylbenzene/styrene columns, equipped with structured packings
are 89m. The largest column diameter employed at BASF so far is
10m; however, in reneries the vacuum towers can have diame-
ters up to 14m. Even larger diameters will be required to capture
CO
2
from the ue gases of power generation plants. To minimize
capital expenditure, the absorbers with diameters well above 20m
will be necessary, bringing new challenges regarding the column
operation and construction.
On the processing side, large diameters imply dealing with well
know but never sufciently understood problems associated with
a pronounced tendency of both phases to unequal distribution
(maldistribution) if a chance is given, and this tends to increase
with increasing diameter. This is true for both packed and tray
columns. In general, the liquid phase, if distributed unequally over
the column cross-sectional area because of distributor failure or
irregularities in the bed structure caused by poor packing instal-
lation, forces the gas phase to distribute non-uniformly. The same
will occur on large diameter trays with long liquid path, if there
are local differences in the density of froth layer imposed by some
minor designor constructional irregularities. Intall columns, under
strong wind conditions, the top part of a column moves causing
clear liquid thickness to change signicantly, forward and back-
ward, givingthegas phaseanopportunitytoescapethroughregions
with reduced resistance. This and other forms of cross ow chan-
nelling can be reduced or eliminated using such common sense
solutions like compartmentalization in case of splashing liquid or
by installation of ow directing bafes or other means including
proprietary designs of ow pushers [55]. This can be done with
certain degree of simplication using CFD simulations to validate
tray layout quality. Nevertheless, proper experimental evidence
is required to get the necessary design condence. The research
efforts along this line are still going on but there are no reports
on systematic studies with test trays having diameters larger than
that (2.3m) reported in the book by Stichlmair and Fair [2]. Chi-
nese researchers involved with numerical simulation of sieve tray
performance [56], use temperature distribution and ow pattern
data collected by Porter et al. using a test tray with a diameter of
2.44m [57]. However to get necessary design condence it is often
enough to arrange an ad-hoc airwater test to visualize hydraulic
performance of a large diameter tray.
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Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104
Fig. 14. Montz ad-hoc tray hydraulics testing installation (6.8m).
Recently, J. Montz has built a single tray test setup to demon-
strate operability of a nine meter diameter cross ow tunnel tray,
which, due to an extremely long liquid path, has been designed as
a cascade tray to provide sufcient liquid gradient. It was a really
challenging task in view of the very large pump and blower capac-
ities required, and hence, only one half of the tray in actual size,
with a tray below to ensure a uniform gas distribution was built. It
was a relief to observe that tray with such a large cross-sectional
area and long liquid path can operate smoothly. Considering the
trays size, their proper installation represented quite a challenging
task, requiring special constructional provisions to ensure levelness
within the given tolerances (3mm), without an excessive support
structure which can affect the tray hydraulics adversely. Indeed, in
largediameter columns, particularlyintheso-calledheavydutyser-
vices [58], the tray support structure canoccupy signicant fraction
of the cross-sectional area. The effect of the orientation of the sup-
port bars on hydraulic performance of a tray is described elsewhere
[37].
Fig. 14 shows a photograph of another ad hoc installation, i.e. a
6.8-m diameter column section containing three cross ow trays,
with a liquid owpath of around 6m, which was built with utmost
care to allow experimental simulation of the tray hydraulics as
close as possible to the actual situation. The test performed with
this installation indicated that under certain operating conditions
a strange ow pattern disturbance can occur, which however do
not tend to escalate into an inoperable situation.
With the advent of corrugated metal sheet structured packings
at the beginning of the 1980s, large diameter packed columns made
an inroad into distillation plants. After some initial performance
failures it became obvious that a good initial liquid distribution is a
prerequisitefor thepackedcolumns toperformaccordingly. For this
reason, assembling and testing liquid distributor prior to delivery
became a standard practice of packing manufacturers.
Although a lot of attention has been given to the liquid distribu-
tion in packed beds, the experimental evidence obtained at larger
scale is scarce. Most recently, Olujic et al. [59] published a paper
comparing the hydraulic performance of packed beds consisting
of conventional Montzpak B1-250 and its high-capacity counter-
part B1-250M, as measured at ambient conditions using air-water
systemin conjunction with a Perspex column hydraulics simulator
with an internal diameter of 1.4m. Fig. 15 shows the top segment of
this column with a narrow trough distributor containing 149 drip
tubes, which corresponds with approximately 100 drip points per
meter square. The layout of the drip points is shown on the left
hand side of Fig. 16, in parallel to a conguration with each second
Fig. 15. Photo of the large turndown, narrow trough liquid distributor with drip
tubes during installation in the TUD column hydraulics simulator (internal diame-
ter =1.4m).
Fig. 16. Layout of drip points of the narrow trough distributor used in TU Delft
studies: 100 drip points/m
2
(left), and 50 drip points/m
2
(right).
tube closed. The latter was used to reveal the effect of such a strong
reduction in the density of initial distribution.
Fig. 17 shows the drawing of a double wall liquid collection sec-
tion, which was placed immediately below the packing. Special
feature of this device is that it enables determination of the relative
quantity of the liquid leaving the bed via walls. The rods with rect-
angular funnels (50mm50mm) at the end, which were moved
gradually along three equidistantly arranged directions, provided
information on the liquid distribution across the bed.
Fig. 18shows aset of characteristic results, illustratingtheeffects
of initial irrigationdensityonliquiddistributionperformanceof B1-
250 and B1-250M, respectively. The measured proles are shown
for threedifferent liquidcollectingdirections ontheleft handsideof
Fig. 18, as continuous lines. They represent observedlocal owrates
compared to the average liquid load, 10m
3
/m
2
h in present case,
shown as a horizontal line. The numbers shown on the left hand
Fig. 17. Schematic of the double wall liquid collecting section.

Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104 1099

Fig. 18. Typical liquid distribution data/proles as collected during liquid distribution tests using TU Delft column hydraulics simulator.
side indicate corresponding wall ows. On the right hand side, the
corresponding 2D liquid distribution proles are shown, which are
obtained by interpolating measured values per concentric ring cor-
responding to the location of the collecting points. This way, it was
possible todetermine corresponding coefcients of standarddevia-
tionshowninparallel to givenproles. Different velocity ranges are
represented by different colours shown in the accompanying bar,
which however can be seen in greater detail, in colour, in online
(pdf) version of this paper.
Two sets of data are shown for each of compared packings,
B1-250 and B1-250M, respectively, for a standard initial irrigation
density of 100 drip points per meter square, and one congura-
tion with less drip points. It is worth noting that the beds under
comparison had the same structure consisting of layers compris-
ing three (manhole size) segments of packing. As shown in Fig. 18,
and elaborated in detail elsewhere [59], B1-250M packing exhib-
ited somewhat better quality of distribution in the bulk of the bed,
but this appeared to be at the cost of increased wall ow. It is read-
ily seen in the observed proles for the standard irrigation density,
yielding the standard deviations of around 22 and 18% for B1-250
and B1-250M, respectively. This means that the best distribution in
abedconsistingof apackingwithaspecic areaof about 250m
2
/m
3
lies in the range of 20% deviation from the mean value. One should
note that this is well above the average deviation in the individ-
ual drip points of the state of the art liquid distributors, which is
below 5%. Exhibited liquid distribution quality is an intrinsic char-
acteristic of this type and size of corrugated sheet packing, and it
can be hardly expected that a better quality can be achieved by
increasing the initial irrigation density. Indeed, still unpublished
data indicated that doubling the initial irrigation density will not
result into any improvement inthe liquid distributioninthe packed
bed. Fig. 18 indicates that a reduction of the number of drip points
by factor two has almost no effect as well. Such a result has long
been anticipated and the presented large scale experimental data
explicitly show that this is true.
Although airwater data cannot be carried over directly to
organic systems [60], it may demonstrate tendencies which can be
expected regarding the relative magnitude of wall ow. It should
be noted that the wall ow can be detrimental to efciency even
in columns with large diameters. Especially when dividing wall
columns are considered, in which the relative amount of wall area
is much larger than that in conventional columns and, particularly,
when high product purities are required, the effect of the wall ow
canbesubstantial. Toavoidthepossibledetrimental effects of liquid
and/or vapour bypassing, wall wipers need to be designed, placed,
and installed properly.
Among the experimental data obtained from the comprehen-
sive liquid distribution study with B1-250M packing performed at
TUDelft, the best results were achieved at the initial irrigation den-
sity of 90 drip points/m
2
. At this conguration, 10% of available drip
tubes located in the centre were closed thus leading to a simple
but highly effective change in the layout of drip points. This indi-
cates a high potential towards the further improvements of packed
bed performance, by paying attention to details in design of liquid
(re)distributors.
A practical problem associated with the liquid distribution in
large diameter packed columns, not recognized widely so far, lies
inthe fact that additional columnheight (very expensive) is needed
to accommodate one or two predistribution stages. This increases
sensitivity to column malperformance. The reason is that a failure
of the liquid predistribution manifold to feed equally all sections
of the very accurate last distribution stage, being usually a narrow
trough distributor with at least 50% open area for ascending gas
ow, will result into highly irregular initial prole. Such an initial
maldistribution cannot be restored to the health by intrinsic redis-
tribution properties of the structured packing. In other words, with
present high standard quality of liquid distributors, the predistri-
bution manifold design becomes a main concern.
Although beds of structured packing can be found in daring
heights or depths (up to 10m or even more), it is a general prac-
tice to limit them, at least during conceptual design, to bed heights
corresponding to approximately 15 equilibrium stages (theoretical
plates or trays). This implies the need for frequent liquid redistribu-
tion in separations requiring a large number of stages. As shown in
Fig. 19, a typical liquid redistributionsectionconsists of a liquid col-
lector placed above a liquid distributor, with the height required for
installation tending to increase with increasing column diameter.
These installations are designed to ensure best conditions for effec-
tive collection, mixing and redistribution of liquid. Where pressure
drop is a concern, liquid collectors are usually of the chevron or
vane-type. The latter are designed to avoid excessive interaction
of phases, which eventually amounts to the fact that these devices
act as a kind of promoter for the gas maldistribution [61]. The 2D
prole, shown in Fig. 20, on bottom side of the left hand picture,
1100

Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104
Fig. 19. Schematic of a typical liquid redistribution section as installed in a packed
vacuum column.
has been measured using earlier mentioned 1.4m facilities at TU
Delft. The dark (blue in colour representation) kidney-like prole
indicates a region with effectively zero gas velocity, while the peak
velocities at the periphery are around6m/s. Fortunately, as demon-
strated elsewhere [62], such a pronounced, but quite symmetrical
gas maldistribution can be restored to health within two or three
packing layers. This is the reason why the gas maldistribution is not
consideredtobea bigthreat tocolumnperformance. However, with
the tendency to employ high capacity packings, at lower pressure
drop, one should bear in mind that available pressure drop in a bed
in this case may be not enough to smooth out the velocity prole.
Thus, the maldistribution can penetrate deeper into the bed before
the redistribution work is accomplished properly.
From Fig. 20, one can see that CFD simulations resemble
observed proles, which implies that commercial packages (Flu-
ent) can be employed with condence for the simulation of the gas
ow through the column internals. The proles shown in Fig. 21
represent a ow eld image as obtained by a simulation of an
improved, streamlined design of the conventional vane-type col-
lector [61]. Striking is that a much better gas distribution prole is
obtainedaccompaniedby a 30%reductioninpressure drop. The lat-
ter was achievedmainly by reversing the cover of the central trough
accordingly.
One should note that contrary to the situation with the liquid
distributors, for the gas inlet distributors there is no possibility to
test their functionality experimentally prior the installation. There-
fore, a CFD-assisted design of column internals regarding the gas
ow simulation will become increasingly important in the near
future. Now CFD is widely employed at Sulzer for the purposes of
layout of inlet gas (vapour) distributors [63]. But also in the design
of complex large diameter liquid distributors CFD can be a very
helpful tool to speed up the layout process [64].
5. Equipment modelling advances
Although the advances made in commercial CFD tools towards
the description of single phase ows to reveal the effects imposed
by geometry of various column internals are encouraging, this
highly sophisticated technique is still far away fromthe point to be
capable to describe even simplest forms of gasliquid interaction
encountered in industrial columns in a physically sound way. This
means that there is still a long way ahead and many obstacles to be
overcome, on hardware and software side, to create computational
capabilities to move from the empirical to a more fundamentally
founded column design, which can eventually culminate to the
development of the rst methodof scientic design. This is some-
thing Porter pleaded for some time ago trying to motivate academic
community to organize a devoted research effort in this direc-
tion [65]. Indeed, the key for the success in this area is a better
understanding of interactions between the heat and mass trans-
fer phenomena and underlying uid dynamics. The latter strongly
depends on the type of gasliquid contactor employed.
For structured packing columns, the plug ow based 1D
approachprovides a means for estimating ideal performance. How-
ever, a more detailed approach is required to account properly
for the liquid and gas maldistribution effects. As elaborated in
greater detail elsewhere [66], this implies adopting a certain level
of subdivision of the packed bed, with discrete cells ranging in
their dimensions from the largest, corresponding to the packing
element/layer height, to the smallest, corresponding to the require-
ments of CFD approach. The ability of the commercial CFD tools to
capture the anisotropic characteristics of single-phase gas ow in
structured packings, as well as to predict the pressure drop based
on such discrete cell approach has been demonstrated in a num-
ber of papers published recently [6769]. CFD advancements are
also addressed by Taylor in his recent state of the art review on
distillation modelling [70].
Certainly, the model accuracy is expected to increase with the
decreasing dimensions of a discrete cell. However, this is accom-
panied by a correspondingly increased computational complexity,
impractical run time, and uncertainties regarding the attainable
accuracy. However there are even more ambitious efforts going
on, pushing toward ultimate exactness in this respect. In a multi-
partner research project in USA supported by US Department of
Energy, including a national laboratory with their exceptional com-

Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104 1101

Fig. 20. CFD snapshot of a side cut of a dry gas owthrough the liquid distribution section as shown in Fig. 19, with a comparison of measured and predicted gas distribution
prole entering the bed above.
putational facilities, Separations ResearchProgramat theUniversity
of Texas at Austin providing for experimental validation of the
model under development, and a number of industrial partners, an
attempt is made to simulate the uid-dynamics inside structured
packings using direct CFD simulations [71].
No doubt, the combination of empirical models with CFD tech-
niques can improve the structured packing column design practice
substantially. Although the structured packings with their ordered
structure provide more regularity with respect to the nature of
gasliquid interface than random packings and trays, an exact
localization of the interface, prediction of its form and quantity
represents anextremely difcult task eveninthe preloading region.
With this in mind, Shilkin et al. [72] and Shilkin and Kenig [73] have
shown that an alternative modelling approach, based on replace-
ment of the actual complex hydrodynamics by a combination of
geometrically simpler ow patterns, in which the transport phe-
nomena can be described in a rigorous way, can lead to surprisingly
good results when applied to corrugated sheet structured pack-
ings. According to Kenig, the driving force behind this most recent
development, theso-calledhydrodynamic analogy(HA) approach
lls the gap between the rigorous CFD and empirical rate-based
approaches [74]. This is illustrated graphically in the plot shown in
Fig. 22, indicatingthat complexuid-dynamic situations as encoun-
tered in packed and tray distillation columns, are best approached
using the least rigour, one-dimensional, but empirically well sus-
tained rate-based or equilibrium-stage-based models.
Being fundamentally founded, the rate-based approach is con-
sidered to be more appropriate. However, due to the fact that
the number of required equilibrium stages can be determined for
majority of industrial distillation applications with ultimate rigor,
the stage efciency determination methods are still widely used in
conjunctionwithdesignof bothtrayandpackedcolumns. However,
one should note that in the case when extremely pure products
need to be distilled, the required number of stages is still deter-
mined experimentally using a test column of suitable (pilot-plant)
size.
There is no doubt, in more complex situations, particularly
those including chemical reactions (reactive absorption and dis-
tillation) rate-based modelling enables a closer approach to reality
to the extent depending however on the appropriateness of model
parameters used [7577]. This conrms necessity of adequate
experimental support for the purposes of development and val-
idation of advanced predictive models. As discussed in these
references, incase of advanced (complex) rate based methods there
are also some other (numerical) factors like the degree of lm
discretization that affect both the computational effort and the
accuracy of the model.
The parameters required for the rate-based models to describe
the hydrodynamics and mass transfer in distillation and absorp-
tion columns, with and without chemical reaction, are gas (vapour)
and liquid-side mass transfer coefcients, the interfacial (specic
contact) area, liquid holdup and pressure drop. For practical design
purposes it is also interesting to know the point of onset of loading
and ooding, respectively.
Of particular importancearecorrelations for predictingthemass
transfer coefcients and the effective (interfacial) area, which are,
for structured packings estimated using some of few established
empirical correlations. These however exhibit large discrepancies
when compared [78], and affect directly the accuracy of the predic-
tive model [79].
Adetailed classication of the rate-based modelling approaches
depending on complexity of the ow conditions along with their
relative advantages, limitations and interactions are discussed in
the above mentioned, most recently published paper by Kenig [74].
Moreover, this paper introduces the authors concept of compli-
mentary modelling of uid separation processes, i.e. nding the
best solution for a given task by a reasonable and effective combi-
nation of different modelling approaches. This is in agreement with
an old quote saying that the essence of the engineering is to be
only as complicated as you have to be, but you must also be able to
get as complicated as the problem demands [80]. To comply with
this requirement, chemical engineering curricula should include a
sound combination of fundamental and practical uid dynamics
related knowledge.
6. Equipment testing facilities/standards
Traditionally, FRI (Fractionation Research Inc.) is considered as
a standard for testing commercially available packings and trays.
Prototype testing is performed mainly at SRP (Separations Research
1102

Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104
Fig. 21. CFD snapshot of a side cut of the dry gas ow through the liquid redis-
tribution section equipped with a streamlined chevron type collector, and the
cross-sectional gas distribution prole as delivered to the bed above.
Program) at the University of Texas at Austin. However, this is usu-
ally done on proprietary basis, using equipment of a smaller but
large enough diameter of 0.43m to be considered useful. Similar
installation was used during the last 10 years at TUDelft, to test the
prototypes of J. Montz M and MN series packings, as well as Sulzer
MellapakPlus 752.Y [32] and Katapak SP series catalytic packings
[48,50]. Most recently, Bayer TS has commissioned a state of the
art, total reux distillation unit (internal column diameter 0.6m)
for such purposes. The tests results with the new generation of J.
Montz packings have been partly published [31].
The experimental evidence is the only proper mean to support
development and to validate properly predictive models to be used
for design purposes. Unfortunately, the test data on performance
of novel equipment, available publicly, are scarce and difcult to
verify. This increases the risk associated with the need to arrive
at tight enough designs. With this in mind, BASF SE encouraged
and supported TU Delft to make a critical evaluation of the test
facilities and procedures. The results of this comprehensive study
Fig. 22. Classication of the kinetics-based modelling approaches according to the
Kenigs complimentary modelling approach [74].
concerned with structured packings are made available as an open
access document [81]. It contains a standardization proposal to dis-
tillationcommunityworldwide, openfor the discussionandfurther
improvements. It is our hope that this will lead to a rst standard
in this respect, which could easily be extended to randompackings
and trays, similar to that recommended by AIChE for performance
evaluation of operating industrial columns [82].
7. Concluding remarks
Reducing the energy requirement of distillation columns and
systems and related reduction of CO
2
emissions are becoming a
part of globally proclaimed efforts toward more sustainability in
process industries, whereas the goal must be achieved without an
excessive capital investment.
Dividing wall column, which is nowwell established as a packed
columnandexpands slowlyintothe applications dominatedbytray
columns, is themost prominent exampleof adistillationtechnology
breakthrough. As proven in more than hundred applications with
separation of three component feeds so far, the energy saving is
accompanied by a capital saving compared to conventional two-
columns congurations. Introduction of the unxed wall was a key
for expanding the number of applications, and more importantly, it
open doors for designing highly cost and energy effective DWCs for
separation of four or more component mixtures into pure products
withinasingleshell. Oneshouldnotethat intheliteraturetheDWCs
for the separation of four-component mixtures are referred to as
Kaibel column [83], which is a tting tribute to the inventor G.
Kaibel of BASF.
Usability of HIDiC has been demonstrated. Unfortunately, HIDiC
is a capital intensive technology, which, however, can become more
economically attractive if it proves to be suitable for the debot-
tlenecking purposes. At the same time, there are barriers to be
overcome on process and mechanical design side to arrive at an
industrially viable column conguration. This is the main goal of
a devoted research effort undertaken presently by a research con-
sortium supported by Dutch government, with TU Delft and ECN
(Energy Center of the Netherlands) as research institutions and
BASF SE, Bayer TS, and Sulzer as industrial partners. Interesting to
mention is that in the meantime implementation of HIDiC became
a subject of interest of American researchers [84].

Z. Olujic et al. / Chemical Engineering and Processing 48 (2009) 10891104 1103

The distillation equipment related developments addressed in
this publication are encouraging, particularly those related to high
performance packings operating at minimized pressure drop per
stage. However, at very low pressure drop, a packed bed will be
unable to correct any form of initial maldistribution on vapour
side. This means, particularly in conjunction with large column
diameters employed nowadays in world scale process plants, that
provisions have to be made to ensure a uniform initial vapour dis-
tribution. CFD modelling can be useful in design of inlet devices.
On the other hand, high capacity trays operate at high tray pressure
drop, however, here the liquid phase pattern needs to be controlled
byappropriate provisions, and, again, CFDcanbe a useful tool inthis
respect. Although we all strive for it and there are many enthusias-
tic modelling minded people and promising developments around,
we are still far away from having pilot-plant experiments replaced
by computer experiments.
Dedicated research effort is needed to enable further improve-
ments of distillation, to comply with global requirement for a
more sustainable process technology (reduction of energy use and
relatedCO
2
emissions inconjunctionwithreducedcapital expendi-
ture). Thermodynamically, a sustainable distillation column design
implies operating at lowest allowable pressure and lowest pres-
sure drop, which however is not quite compatible with industrial
design practices. Namely, an operation at vapour loads that ensure
capacity increase in existing columns, or more compactness in new
designs, always leads to an increased total column pressure drop,
regardless the type of contactor. Thus, the process intensication
always works against the thermodynamic efciency of distillation
and, insome specic cases the increased pressure drop candiscour-
age implementation of heat pump system. Although being capital
intensive, the latter will gain more attention of process industries
in the near future.
Acknowledgements
Authors are thankful to BASF SE, J. Montz GmbH, and TU Delft
for providing information and illustrations used in this paper, as
well as to Koichi Asano, Professor Emeritus of Tokyo Institute of
Technology, for permission to reproduce a gure and a table from
his book (Ref. [23]).
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