.
ot,l
Succeed at Scale Up
ailure to properly scale up mixing in
Scale-up
problems in
industrial reactor
F batch and continuously stirred ves­
sels remains a persistent problem in
the process industries. Numerous
causes of difficulty exist, but a pattern is
evident: A lack of understanding of the pro­
mixing can be
cess undermines many efforts. Mixing prob­ be achieved more easily in small equip­
lems are seldom recognized, in part because
costly, but are
they are not well understood, but also Contrast those with applications that are
all too common.
because they are not examined as quantita­ less sensitive to the needs of uniform mix­
tively as other unit operations.
Here's a proven
Correcting errors in scaling mixing • heat transfer:
procedure that
operations is costly and sometimes impos­ • blending of miscible fluids:
sible. Errors can cause losses of productivi­
avoids them.
ty, quality, and profit, and they also can reactions;
lead to safety problems such as reactive­
) chemical incidents. Although technical
problems cause most failures, nontechnical
reasons also contribute to difficulties.
Scale up of mixing can be easy or com­
plex. Most difficulties arise when potential
problems have not been well thought out.
Hardest of all are multiphase processes in
which the chemistry depends on condition
Douglas E. Leng, of the phases.
The Dow Chemical Co. Good quantitative tools and measures of
Jal performance are required to solve such
ihaif problems. (See the accompanying article
on­ by Tatterson for an examination of these
needs.) My 25 years of experience with
·'er ­ industrial mixing and scale-up problems
lac has led me to identify some general trou­
~ion blespots and to develop a procedure for
eeds, successful scale up.
First of all, the engineer" must clearly
understand the role of the mixing. Is rapid
attainment of uniformity critical to process
success? The following are typical chemi­
cal processes that depend on rapid attain­
ment of uniformity:
• chemical reactors/polymerizers in
which reaction kinetics are equal to or
faster than the ratc of mixing:
• competing chemical reactions where
i' )
poor mixing affects yields;
• crystallizers thai depend on uniform
mixing to promote the growth of large uni­
form crystals; and
• reactions dependent on mass transport.
such as coalescing and redispersing of liq­
uid-liquid and gas-liquid mixtures.
For such processes. desired results can
ment than in large equipment.
ing. These include:
• reactors inyolved with slow chemical
• suspension of solids.
These foul can be considered noncritical
applications, i.e.. they can usually be scaled
up with few difficulties.
Many engineers are most familiar with
the latter, noncritical applications.
Unfortunately. they get the impression that
mixing is simple and can be treated casual­
ly. Thus. it is not surprising that so many
scale-up problems occur.
Avoiding problems
For successful scaleup of mixing in
industrial processes, a designer should fol­
low six distinct steps:
1. define the process need;
2. identify all of the operational
parameters;
3. review the process history:
4. select the imponant process
parameters;
S. choose an initial equipment design
vessel design, impellers. impeller location.
bal'fles. and points of feed and exit
~treams: and
6. test the design relative to the process
needs and assumptions and then fine tUlle it
to meet the needs of the most important
variables.
Many scale-up failures can he traced
directly to the omission of one or more of
CHEMICAL ENGINEERING PROGRESS • JUNE 1991 • 23
 MIXING
I
I!1
thesl! six steps. We will consider
each of the steps in turn and provide
ex:ampJes of problems.
Defining the .process need
. The design/~cale-up. process
should start with a thorough exami­
nation of all process needs.
Requirements are often straightfor­
ward. Sometimes. however. they
may he complex and even contlict­
ing: For example. it might be neces­
sary to exceed minimum shear to sat- .
isfy dem;)nds for flow and
uniformity.
Typical process needs
include:
• supplying a uniform slurry
to feed another processing
step;
• facilitating a controlled
chemical reaction;
385·hp Drive
Feed from
• providing for mass or heat Second
transfer: Stage
Reactor
• dispersing liquid drops for
a suspension polymerization
or extraction;
• assuring continuous mixing
of added reactants or Isopar Vapor
monomers. from
Petrochem
Avoid the temptation to Superheater
quickly accept the obvious
without evaluating Jess obvi-
ous needs. For instance,
solids must be kept in sus­
pension. but sometimes that • Figure 1. Sparged, lOO,OOO-gallon cofltinuously-stirred­
may not be enough, as tank reactor containing 45% solids.
shown in the following
example.
A complex, three-phase, continu­
ous-stirred-tank-reactor system was
being scaled up from test data
derived in 3,SOO-gal vessels. The
reaction was an equilibrium dimer­
ization, described by:
2 A (solid) ~ (2 A) (solid) + 2 NH.
(gas) .'
The reactor was the last stage of a
three-stage train. see Figure I, and
contained reacting solids suspended
in a light hydrocarbon. Melt from the
second stage entered the 100,000-gal
l stirred reactor and snliditled immedi­
ately to form a fasl-:-;ettling slurry
containing 4S% solids. Agitation was
\
' provided by a single. four-blade, 4So
I
1i -pi lched-blade turhine 16 ft in diam­
eler operated at 26 rpm and driven
by a 38S-hp motor. A large, bell­
shaped distributor \\as located under
24 • JUNE 1991 • CHEMICAL ENGINEERING PROGRESS
1111
the impeller 10 distrihute the S,.uper­
heated hydrocarhon vapor. The
impeller was supposed. to disperse
the vapor into buhhles to· prtwide
mass transfer for the liberation of
ammonia. driving the reaction ·(0 the
right to form the dimer (2 Al.On
start-up, however, solids accumulat­
ed at the base of the vessel. causing
the plant to shut down. The scale up
had been based on invalid criteria,
which led to inadequate mixing for
suspension of the solid.
Vapor to
Condenser
!
I,~\
45' psr Impeller
I
Vapor Distributor
The major mistake was thinking
that adequate suspension of solids
was sufficient to produce desired
production rates. The suspension
problem was solved by doubling the
power per unit volume, as suggested
in tests, but that necessitated trans­ tants, chain terminators, initiators.
ferring the original drive to a stand­ and reflux return.
by SO,OOO-gal reactor. As the
revised plant got back in production,
tests revealed good solids suspen­
sion was provided in all regions of
the smaller SO.OOO-gal reaclor. The
productivity, however, was only
about 2S% of the projected rate for
that size of vessel. The reaction rate threefold, tip speed by 70%, and th\.'
was an important problem that had
not heen solved, Further tests also
revealed that sparging the superheat­
ed hydrm.:arhon was not effective in
removing the ammonia, although
~H.'ceptahlc reaction rates had heen
achieved by sparging gas into a
3,SOO-gal pilot-plant reactor.
Finally. it was shown 'that condi­
tions had been different in the pilot­
plant vessel. Sparging was accom­
plished by pas~ing nitrogen into the
slurry of suspended solids in miner­
ai oil. Nitrogen bubbles had provid­
ed the mass transfer needed to
remove the ammonia in the small
reactor, but, in the plant reactor, cal­
culations ot heat transfer from the
buobles to the surrounding fluid
indicated tpat all bubbles had
collapsed due to condensa­
tion. The liberated heat from
condensation was transported
to the surface by convection.
where it caused the top layer
to boil. Mixing, therefore,
also had to rapidly circulate
reacting solids through the
boiling surface layer to
remove ammonia. Many
mixing designs were pro­
posed. several were tested
and pro\'ided improvements,
but none was sufficiently
effective to permit continu­
ing to operate the plant.
Fortunately, problems of
such magnitude occur
infrequently.
Identifying all of the
operational parameters
List and then prioritize the
reasons for mixing. These
may include requirements for mixing
time (blending). micromixing, heat
transfer, shear. solids suspension.
mass transfer (including liquid-liq­
uid, liquid-solid. and gas-liquid 1.
introduction of gas into liquid, reac­
Textbooks on mixing note that
these operational parameters do not
scale up equally. Oldshue (I) illus­
trates this for scale up from a :::O-gal
to a 2,SOO-gal \essel: If the power
per unit volume (PlY) is held con­
stant, circulation lime increases
impeller Reynolds number by a fac­
tor of 8.S. I f processes reqUire both
constant PlY and shear to be main­
lained, condition;. of geomelric simi­
larity need to he n:laxeJ.
In miniplanh. nonsill1ilar geol11\.'­

try is used to simulate mix­
if'!!. in a large-scale reaclor:
), example, when blend
tIme i, critical. miniplant
.;tudies can be done in a
reactor having a smaller
impeller diameterltank diam­
eter (OIT) ratio.
Identifying all of the key
parameters is, admittedly, not
turbine installation. which
always easy, but the prob­
lems that can be caused by
skimping on the analysis can
be tougher. For instance,
incomplete parameter identi­
this scale and were unman­
fication led to the following
problem:
lation of large in-line filters.
Production of a fine
chemical was' being scaled
up from a miniplant to a
3,500-gal reactor. Agitation
was believed to be needed ill Figure 2. Schematic oj local relative turbulence
for solids movement equiva­ intensities.
lent to the just-suspended
state. In reality, the reaction rates
depended on several factors, per­
haps the most important of which
was mass transfer between the two
coalescing liquid phases. The pro­
iuction facility was sized according
,~ reaction rates observed in mini­
plant vessels. Production rates
determined after plant start-up were
found to be more than an order of
magnitude less than expected.
At small scale, high shear and
rapid circulation led to a dispersion­
controlled environment and small
drops with a large interfacial area.
At the large scale, shear rates were
lower and circulation was slower,
with both factors contributing to
conditions classified as coalescence
controlling. This led to large drops
and much less interfacial area.
Because the kinetics were controlled
by mass transfer, the change from
dispersion dominance to coalescence
dominance explained the unexpected
behavior on scale up.
The scale-up problem might have
been anticipated if the agitator had
been stopped during early laborato­
ry work so that very rapid coales­
cence could have been seen. The
problem was greatly eased by
adding a second impeller, which
):ncreased the overall circulation
rates and provided an additional
region ror drop dispersion.
Input Intensity=1.0
Intensity=20
Intensity=5
J!
Intensity=1
Intensity=O.2
Reviewing the process history
A process is often scaled up in
incremental stages to meet growing
product-development needs. This
provides an opportunity to observe
the development of problems due to
scale up and can help minimize risk.
Problems can be subtle, as seen in
the following example:
A nonaqueous dispersion was
being developed from laboratory
through a mini plant, pilot plant,
semiworks plant, and, finally, fuIl­
scale production. The product was to
contain a certain fraction of solids in
the form of micron-sized polymer
particles. The procedure developed
was to continuously feed initiated
monomers into a vigorously agitated
hot fluid to rapidly disperse the
monomers and provide uniformity
and heat transfer. The rate of poly­
merization was governed by the rate
of the addition of monomer, which
contained free-radical initiators with
a half-life of less than a second at the
temperatures in the reactor.
Superior product was obtained in
S-L glass reactors with the desired
viscosity, particle sizes, and percent­
age of solids. The results were not
quite as good in the next size reac­
tors, but cerlainly good enough to
maintain enthusiastic support from
management and customcrs. In the
CHEMICAL ENGINEERING PROGRESS • JUNE 1991 •
II
2.0()()-gal semiworb plant.
howe\cr. agglomerates and
small lumps of polymer
formed. which necessitated
'in-line product filtration.
Oth~r problems al~() appeared ,.
but were controllable.
The full-scale plant was an
g,OOO-gal multi-pitch-blade
I
included an elaborate recycle 1., ;
system through heaters and
coolers arranged in parallel. I!
Problems greatly increased at 11 '
ageable even with the instal­
Calculations showed that
the energy per unit volume , /
was 120 hplLOOO gal at the'7
5-L s,cale and decreased
almost linearly to 3 hpll,OOO
gal in the production reactor.
Meanwhile. product contin­
ued to coarsen as larger vessels were
used. Since the initiator half-life was
only a fraction of a second, the sizes
of particles were established virtually
instantaneously when the monomers
entered the reactor.. Intense
micromixing in the small vessel dis­
persed the monomers much more
rapidly as polymerization proceeded.
. D. E. lENG is a senior research .
scientist ill the Central
Research Engineering
laboratory of The Dow
Chemical Co., Midland, MI
(517/636-3387; Fax.: 517/638·
9674). He has worked for Dow
at Midland for 35 years.
During the last 25 years, he
has been involved primarily in
mixing and multiphase
research, applications, prob- ,
lem solving, and engineering
administration. He obtained a
BSc and an MSc from Queen's
Univ., Kingston, Ont., and a 1
PhD from Purdue Univ. A fel- .{
low of the AIChE and a mem-j
ber of the American Chemical l
Society, he was the chairman, '.
of the Engineering Foundation A
Conference on Mixing (1981) .. ';.i
.' "-. '1
;,',?..;,":
,tii
25

MIXING
In larg('r s..:alc vessels. the
mixing intensity was two
orders of magnitude less. so
the dispcr;.ion of the
monomer \\'a~ 'slow relative
to the rat(' of reaction. This
r('sulted in a big difference in
the Damkohler number.
Clearly. increasing the
total power to the level pro­
vided in laboratory-scale
work \\'as not a dable solu­
tion. Instead. attention was
turned to assessing what
could be done to improve
the mixing intensity at the
II monomer inlet without
II
increasing the overall mix­
ing energy. The location of
the monomer inlet was at a
region of low turbulence,
,
and local energy-dissIpation
rates in agitated vessels are
known to be highly nonuniform.
Recently published studies (2,3)
have shown that regions close to
the impeller gave dissipation rates
20 times greater than the average in
the reactor as a whole. Figure 2
shows schematically that regions
near the impeller provide more
intense energy dissipation. Adding
the monomer through a cooled inlet
pipe directly to the impeller dis­
charge stream worked so well at the
production scale that filtration was
obviated.
Thus, careful observation and
analysis gave warning that a prob­
lem, could occur, Fortunately, the
solution was fairly simple to imple­
ment and worked well.
Selecting the important pro­
cess parameters
Textbooks generally treat mixing
as a series of topics that have little in
common. These topics can, however.
lead to an orderly checklist for
selecting parameters that are impor­
tant to the mixing process.
Blending of lIliscihlt! liquids deals
with topics related to design and
I impeller and vessel dimensions, and
~ !
generally ends up with a discussion
about mixing time. 8 m , A process is
seldom scaled up oy holding mixing
time constant because this generally
requires high power commitments.
Processes that d.::pend on rapidly
26 • JUNE 1991 • CHEMICAL ENGINEERING PROGRESS
InterfaciaI
Vortex
Baffles
• Figure 3. Improper geometry for the dispersion of
monomer ill water.
attaining uniformity generally do not
scale up well.
Mixing time was used as a crite­
rion for the scale up of a polymer­
ization process in which a block
copolymer was being produced.
Polymerization rates were fairly
fast, and locally poor mixing gave
inferior results, leading to a product
with a broad distribution of side­
chain lengths. Calculations indicat­
ed what mixing times could be
achieved reasonably in the planned
production reactors, and miniplant
conditions were chosen that would
duplicate these conditions. Tests
were then conducted in the mini­
plant to determine whether the
product quality was sensitive to
agitation rates above and below the
calculated rate based on equal mix­
ing time. In this case. scale up was
successful. due in part to the recog­
nition that mixing time was a criti­
cal fac.tor for product quality.
Ga.~-liquid mixing usually
relates to phenomena su(;h as gas
holdup, interfacial area (kiP, the
mass-transfer coefficient and inter·
facial area). and the ratio of power
while gassing to power for the
ungassed state (P /PIf~)' The latter is which mixing is fairly straightfor­
expressed as a ru'netion of the aera­
tion number QIND\ where Q is the
gassing rate, N is the impeller
speed. and D is the impeller diame­
ter. Sin(;e mixing has lillie effect on lead to impclkr cavitation. Wh~'n
-
kl.' rthe mass transfer coeffi­
cient). it is the interfacial
area. a"that is atTected in k1u
measurements, Hen(;c kl.a is
a function of the superfi(;i:l
gas velocity and PIV. the
power per unit volume,
For example. consider the
scaleup of a microbial fer­
mentation. The role of mix­
ing was to provide gas dis· ,
persion, supply nutrient
blending, keep solids in
suspension. and maintai'l
reI ati ve \y low shear. Th:
broth became rheologically
more non-Newtonian with
time. The scale up was to
provide correlations for 80­
m 3 vessels in which the
desired dissolved oxygen
could be maintained by a
combination of impeller
speed and gas rate. The criticn
scale-up variable was selected to be
the kLa, so that equivalence in kLa
could provide similar dissolved
oxygen levels at corresponding
stages in the fermentation.
Studies were conducted in 30-L
and 2S0-L laboratory vessels. The
kLa measurements were made by the
steady-state method: oxygen con­
sumption was determined from the
difference between the inlet and out­
let oxygen concentrations and the
airflow rate. Probes measured the
dissolved oxygen in the liquid phase.
The relationship between the two
sizes of fennenters suggested a cor­
relation of the fonn:
k aa.(PAl: 14(S )oAfi(lI)
L r~'
where S~ is the superficial gas veloci­
ty. It was necessary to correlate kL
from a determination of the zero
shear viscosity (11) of broth sampled
from the fermenter. The correlation
proved to be accurate, provided
impeIler flo\\' was sufficient to
entrain gas buhbles to the regions
below the impeller,
Many published studies on
gas-liquid mixing have been done ;11
low gassing rates. conditions under
ward. Gas rates. however. arc usually
much highcr in industrial mixing ­
often I to 3 \'olumcs of gas per vol­
ume of liquid pcr minute - and can
 that happens. impeller discharge
)lWS diminish and the dist·ribution
,)j" ga~ in the vessel can change dra­
matically from fairly uniform to
poor. .-\5 discharge rates decrease.
impeller flow can no longer entrain
gas and carry it to all regions. The
region below the impeller near the
tank bottom is usually the first to
become void of bubbles. Under
flooded conditions. the impeller can
often only distribute gas radially to
regions above it. The ratio PIPIt~
falls to less than 0.5 under these
conditions.
Liqllid-liquid dispersiolls are
commonly associated with drop dis­
persion and the generation of inter­
facial area. Various mechanisms
have been proposed for drop disper­
sion. usually relating fluid forces
(laminar or turbulent shear) to drop
surface forces. The fluid forces can
arise from impact at the walls. or
rotational, dilational or turbulent
shear. Resistance forces are com­
monly those due to interfacial ten­
sion or surface viscosity. The drop
, breaks when fluid forces exceed
cohesi\e forces.
The process of forming the dis­
persion is also important. but it has
recehed little attention. Consider
two separated liquid phases. A and B.
of diiferent density with A on top
and B below. To create a dispersion
of B in A, an impeller must be placed
in A. For the reverse. the impeller
must be placed in B. This sounds
simple and logical. but its impor­
tance was learned the hard way:
A suspension polymerization was
being scaled up from 3,500-gal to
lO.OnO-gal size. All factors about the
vessel geometry were similar, The
process technology had been estab­
lished for many years in the smaller
reactor. Therefore. a prototype
10.OOO-gal vessel was to be tested
first: if it was successful, the remain­
ing pl)lymerizers would be installed.
Agitation at both scales was provid­
ed by a single. three-blade. retreat­
cuneo glussed-steel impeller located
at the bottom of the reactor. The
polymerizers had two finger baffles
placed 1800 apart.
)
The polymerizer had to sequen­
tially mix the phm;es (waler with sus­
pl'nding agl'nt. and monomers with
catalYSt). form a suspension of
monomer drops in water. heat to
polymerize. polymerize. and finally
cool, The monomers were more
dense and initially formed the bot­
tom layer. while water and suspend­
ing agent formed the top layer.
Agitation begun, and heat-transfer
coefficients were calculated online
by the latest instrumentation. As the
polymerizer began its first run. the
heat-transfer coefficient feli from 50
to less than 2 Btu/h/ftC/oF. reactor
temperatures went out of control. and
emergency venting to a condenser
was activated to provide evaporative
cooling and avoid serious reactive­
chemicals problems.
The monomer layer, instead of the
water layer, had become the continu­
ous phase. and heating had initiated
polymerization - resulting in a
mess. Similar results were produced
in two further runs. The problem was
solved by placing a second impeller
in the upper. water layer, which
caused monomer to be thrown up
into that layer. Laboratory mixing
tests showed that the single lower
impeller created a large interfacial
vortex that allowed water from the
upper layer to reach the impeller and
become dispersed, as shown in
Figure 3 , The problem was not
apparent in the 3,500-gal vessel, pos­
sibly because relatively lower tan­
gential velocities existed, resulting in
a shallower interfacial vortex that did
not reach the impeller.
Coalescence of drops occurs upon
collisions with other drops, or
between drops and solid surfaces
Log
Drop
Size
.....f - - - - - - _ l _ Dispersion:
Log Impeller Speed
• Fi~llre -I. Dispersioll-suspensio/l relations/ri/ls ill slispensioll poIYllleri:.atio/l.
CHEMICAL ENGINEERING PROGRESS • JUNE 1991 •
such' as baffles. vessel \\alls. and
impellers. Conditions of shear lead to
drop collisions, High local shear
rutes also leud to drop di'persion. In
a coalescing and dispersing system.
coalescence occurs principally in
regions of low shear. v.hile disper­
sion occurs in regions of high shear
near the impeller. An agitated disper­
sion is both dynamic and periodic,
Large-scale eddies appear. disappear,
and reappear from time to time. sug­
gesting highly transient behavior.
Colliding pairs of drops coalesce if
the forces pressing them together
endure long enough for drainage and
thinning of the continuous phase to
occur between them. If insufficient
drainage occurs. the drop pair will
separate as fluid forces diminish.
Other factors. such as the mobility of
the liquid-liquid interface. the defor­
mation of the drops upon impact, and
foreign matter collected at the sur­
face. also playa role in the drainage.
Our current ability to scale up liq­
uid-liquid dispersions depends on
whether the system is coalescing or
noncoalescing. Coalescing systems
are extremely difficult to scale up if
equal interfacial area or drop-size
distribution must be maintained.
NOllcoalescillg systems often
involve suspension-polymerization
processes employing a water-soluble
protective polymer that collects at
the drop surfaces and prevents coa­
lescence. Mixin'g for these systems ~)
need only provide for dispersion and !
suspension because coalescence is I"~
virtually absent. Figure -+ shows that
mean drop sizes become smaller and
suspension
line, drops
are suspended
drops above
the dispersion
line are
dispersed.
27
 MIXING
------.---~~--------------------------~~~---------------------------
drops arc hetter slispenued as
impeller speed" increase. Decreasing
the agilalor spe\.:d uo\.:s the opposite,
The drop sile eorn.:sponciing. to the
inter.scctipn Ill' the dispersion and
suspension line" is the largest mean
drop size that can he produced under
those specific conditions. The aver­
age size of drops depends on either
turbulent or laminar shear. while
suspension depends on drop sizes.
density differences. and agitation
parameters (-J.).
Another factor to consider is that
the time to reach a completely dis­
persed condition is short in small
equipment but long in large equip­
ment. A light-transmission apparatus
for measuring interfacial area was
placed on a I.OOO-gal suspension
polymerizer to measure the time
required for complete dispersion. The
noneoalescing drops were still being
dispersed after 24 h of agitation.
Table 1. Rules for scaling-up similar vessels under
turbulent conditions
NDX =Constant
Value of X Rules
Constant tip speed,
constant torque/volume
0.85 Solids suspension
i·
I easily suspended solids
0.75 Solids suspension
0.S7 Power/volume
.. 0.5 Constant Reynolds
number
0.0 Constant speed
Note: Using these rules for scale-up requires a Reynolds number greater than 10',
and geometry of similar proportions.
28 • JUNE 1991 • CHEMICAL ENGINEERING PROGRESS
Becaus.e proUllCliol1 schedules
usually do no! allow for allain111ent
of "complete" dispersion. scale up
becomes more complicated. One
ends up comparing completely dis­
perscd drops made in sillall equip­
ment with partly dispersed drops
produced in large polymerizers.
Therefore. agilation speed has to be
increased in the large vessel to pro­
duce drop size:.. equivalent to those
made in the miniplant polymerizer.
Coalescing systems are, by com­
parison. complicated to scale up
for a number of reasons. Rates of
chemical reactions often depend on
the interfacial area, which in turn
hinges on two dynamic factors:
coalescence and dispersion. Other
important points for these systems
are as follows:
1. Dispersion is localized near
the impeller in regions of high
shear; practically no dispersion
~ kinematic viscosit,·. m 2/sec; d is the
~' mean particle size, m; D "is tht
Processes
Same maximum shear,
simple blending
Used in Zweitering
equation for Nis, for
Scale-up of average solids
suspensions
Suspension of fast-settling
slurries, turbulent
dispersion, gas-liquid
operations where kLa's
must be scaled,
refctions requiring
micromixing
Similar heat transfer,
equal viscous/inertial
forces
Equal mixing time, fast
reactions
occurs elsewhere. except initiallv.
. 2. Coalescence occurs e,ery­
where drop colli~ions can OCCllr.
3. Circulation times increase
greatly in large '·e,sels.
The net effect of these three f~\Ctr)r\
is that dispersion dominates in sma! l
scale equipment and coalescem:c
dominates in large-scale. commer­
cial equipment. .
Solid-liquid dispersiolls com­
monly involve the suspension of
solids' that are more dense than the
suspending phase. A reliable way to
predict how much agitation is need­
ed to suspend solids is provided b:
the Zweitering equation (5;:
i.;N = [5 VO• I d ~.: (g/).nlpp4~ X<),I3] I
- p p ~
.-DO.X5 "Iiu
where: N., represents revolutions per
5
second; isa constant that depends
on the selected impeller, its diameter
ratio. and bottom clearance: v is the
impeller diameter. m; X is the per­
centage of solids: (gt::.plp) is the
gravitational constant times the den­
sity difference di\ided by the liquid
density. mlsec:::'
The just-suspended criterion is
good for dissolving solids. but it is
inadequate if homogeneity is
required; see Table 1 for recommen­
dations for homogeneous suspension.
A more difficult. and less studied.
problem is the one of predicting the
N for solids less dense than the sus­
pgnding fluid. In this case, the free
surface does not provide efficient
geometry for flow reversal compared
to the curved bottom of a tank. An
effective solution for the case of
floating solids is to place a second
impeller close to the free surface to
help disperse tloating solids. This ini­
tiates suspension. and the second
impeller provides needed unifonnity.
An example for !loating solids is
a process to produce foaming-in­
place beads. The process involved
adding cylindri,'ai thermoplastic
polymer granules ll1 hOI water con­
taining an antil'oagulanl. A foaming
or blowing agent was added. and the
contents were heated to above the
glass-transition temperature. The
granules changed from cylindrical to
spherical particlc~ during the heating
 :'1
:I

en'le. Batches were cooled to ambi­
C;ll tcmperatures. vented to remove
C " , ; flammable blowing agen!.
;lIll. ,11en inspected prior to being
!ran~ferred out of the rolymerizeL
I j
In~pcction~ provided a rough quality
l'heck. Suspension conditions in the
reactor were never ideal. as evi­
denced by c~usting on the walls. baf­
tle. impeller. and shaft.
On one occasion. conditions at the
Coagulated the entry point for diluent addition.
layer of beads If diluenh are intniduccd near the
j intake of the impeller. uniformity
'\ can often be reachl.'d in time, ,hort
enou!!h to allow crystal !.!rowth to
-- , domi~ate over nucl~ati(ln~ Because
one of the biggest unknowns is
V shear and its effect on cry~tah. vari­
able-speed drives are commonly
V
~ '­ -,"
...,J used for tank crystallizers.

end of the cycle were different. and Choosing an initial equipment

the beads were stickier than usual.
As the operator began his customary
inspection. he was greeted with a
surge of water, beads. and blowing
agent coming out of the manway. A
spark of unknown origin ignited the
tlammable mixture. and the entire
plant was engulfed in flames.
Fortunately. no one was hun. but the
process was never operated again.
A suspension failure had
occurred. causing massive agglomer­
ation to take place. This agglomerat­
ed material formed a solid layer
bridging the top surface of the liquid.
as shown in Figure 5. Venting had
only reduced pressure in the head
<-'tee above the crust layer, not
bw it. As the crust layer broke,
pressure from below forced the con­
tents out through the opening.
Agitation had failed to provide ade­
quate surface movement to assist in
stabilization of the panicles. The
impeller and baffle designs were
inadequate for this application.
Research showed that beads near
the top surface needed to be kept in
motion. to constantly wet and renew
the suspending agen!. When stag­
nant conditions existed. water
drainage and agent suspension
occurred and led to interbead adhe­
sion. In this prolonged plasticized
condition. the integrity of the beads
was lost. and a continuous polymer
i axial tlow and develop a more order­
• Figure 5. Conditioll of suspellsion
failure caused by poor surface mixing.
ing to minimize concentration and
temperature gradients. Process
needs are specific to the system.
The usual objective in scale up of
tank crystallizers is to produce
large. uniform crystals that can be
easily separated and washed.
Conditions of uniformity are more
difficult to attain in large vessels,
which tend to produce a broader,
finer population of crystals. This
makes subsequent processing more
difficult. If nonsolvents are used {O
"salt out" the crystals. the same
mixing phenomena are encountered.
There is one important difference ­
the rate of approach to uniformity
can be influenced by the location of
45° PST
,/
design
Approximately 75% of all new­
installations use contoured or hydro­
foil impellers because they produce
ly circulation pattern. create low
shear. and require less power than
traditional impellers. The effects on
flow pattern produced by these
hydrofoils are ,shown in Figure 6.
Most processes require these fea-,
tures. Installations needing high~
shear mixing often couple a high­
shear· turbine with a hydrofoil
impeller. thereby maintaining good
circulation while providing high
shear/turbulence.
The position of the impellers is
important. in part because the total
volume of liquid may change (usual­
ly increase) during many processes.
More than one impeller can be used,
even for normally shaped vessels,
i.e.. where the ratio of tank height to
tank diameter (HIT) is 1.2. In partic­
ular, paired hydrofoils offer advan­
I

u0
bridge was formed across the sur­
face of the contents. The level of liq­
uid above the impeller is very criti­
cal in marginal cases of floating \ / j.
t, ,j
I . I
suspensions. and it may have been
the cause of the failure. although this
is not certain.
Agitation requirements in crystal­
lization processes involve suspend­
'g solids in liquids, providing low
~
J

FOil/"
Guv J

lear (so as not to fral..'llIre the crys­ • Figllre 6. Dijlerences ill ol'em/lfloll' pallerlls hetweell a ./5°_
tals). and supplying sufficient blend- pitclted-blade turbi/le al/{I a 1t,I'dmflJiI.

CHEMICAL ENGINEERING PROGRESS • JUNE 1991 • 29

,,­ I
MIXING·
tages - their di~charge pallerns
match rather than conflict. as in other
designs. A second impeller is helpful
for solids suspension to provide mix­
ing even while draining the contents
of the vessel. The upper impeller of a
dual-impeller systel11 ,hould be posi­
tioned at a diswnce of about half an
impeller diameter (Dl from the liquid
surface while introducing solids, and
even for entraining gas into the sys­
tem. Normally. the upper turbine is
placed about one impeller diameter
from the surface.
The selection of the ratio of the
impeller diameter to diameter of the
tank (Din is also important. In·
industrial applications. ratios from
0.25 to 0.65 are used for common
impellers, while larger ratios are
used for anchors, gates. and helical
types of impellers. If the process
requires flow rather than turbulence,
\ DfT ratios of 0.4 to 0.6 are chosen.
For micromixing and processes
requiring turbulence. DfT ratios of
0.25 to 0.35 would be selected and
impellers would be operated at high­
er speeds than when flow is required.
The trend in solids suspension has
been to use smaller. higher speed
hydrofoil impellers. These produce a'1
coherent jet of liquid that impinges (
on the bottom of the tank. resulting
in effective suspension of solids and
resuspension of settled solids.
Although the Rushton turbine is
commonly referred to in publica­
tions, it is rarely used now for new
industrial gas-liquid installations.
An improved design is the concave
disk, which resembles a Rushton but
has six concave, semicylindrical
blades facing the direcliun of move­
ment. This provides excellent gas
dispersion. can handle much more
gas before flooding. and lIses less
power than the Rushton turbine. A
new hydrofoil with three wide blades
is also useful. It disperses gas effec­
tively and has little tendency to
flood. even at high gas tllnv rales.
The four-blade, 45 c -pilch-blade
turbine is still used for systems of
moderately high viscosity. e.g .. those
up to 40.000 cPo It pnnides more
local shear than the ncw wide-blade
J hydrofoil designs: the latll..' 1'. howev­
er. supply more flow and a beller
pattern and u~c less energy. At sti 11
30 • JUNE 1991 • CHEMICAL ENGINEERING PROGRESS
~--------------------~----~~
Big Eddies Vortex
A 8
• Figure 7. Typical surface conditiolls: (A) Turbulellt large eddies promote good
surface mixi/lg; (B) Laminar conditiolls with large ce1ltral vortex - good for addi­
tion; (C) Flat surface, IlOt recommended for chemical additions.
higher viscosities, particularly where
heat transfer is a problem, special
impellers - including anchor, gate.
nelical. and double-helical types
should be used. In cases where peri­
odic sweeping by blades of vessel
walls facilitates heat transfer, these
impellers can be designed to come
very close to the walls (or, in some
cases. to actually scrape the walls).
Some detail is given by Ulbrecht and
Patterson (6).
Fluids up to 3,000-4,000 cP
require some degree of baffling. The "
standard configuration calls for four ~
baffles 90° apart with a width of
J Til 0 or Til 2 and located T172 from
the tank wall. This arrangement
works well unless the presence of
solids or non-Newtonian behavior
leads to regions of stagnation.
Baffles placed midway between the
impeller tip and the vessel wall help
to eliminate problems of stagnation.
particularly for thixotropic slurries. ~
Full-length baffles sometimes lead to
problems because they create a rela­
tively quiet. vortex-free surface- (
making it more difficult to entrain
solids, liquids, and even gases.
Baffles placed below the surface
allow the fOf-mation of a free vortex. ~
which assists the transfer of materi- :)
als into the vessel.
Careful consideration must be
given to locations or the entries and
exits in stirred vessels. Materials
arc often added directly to the free
surface to avoid using dip pipes.
whit.:h can beconle plugged. Ir the
reaction is fast, the free surface
must be turhulent to adequately
cope with reaction kinetics. To fore­
c
stall such problems. it generally is
preferable to add feed streams close
to the impeller inlet. Feed can some­ i
times be added to the bottom of the
reactor where an impeller is usually
located. In continuous processing.
avoid placing the feed and exit
points near each other because this
leads to bypassing and distorts the
residence-time distribution.
Designs often make use of steady
bearings to help a\'oid mechanical
problems associated with the use of
long, thin shafts. If steady bearings
cannot be tolerated, however. an
alternative is to U$e a shorter. thicker
shaft and place the drive at the bot­
tom of the vessel. Using bottom
drives eliminates clutter at the top of
the vessel and allo\\s more options.
Motionless (or in-line) mixers
should be considered as an alterna­
tive to stirred vessel designs for cer­
tain types of applications. Fast chem­
ical reactions often are ideal
applications for motionless mixers.
Also. such mixers excel for applica­
tions in which competing reactions I.
take place and backmixing must be
avoided. In-line mixers are also used
to improve heat transfer to exchang­
ers and pipe walls. Simple distribu­
tive mixing depends on the length of
the mixer and the number of ele­
ments. Dispersive mixing. such as
drop sizing. depends not only on the
number of elements but also the
pressure drop and !low rate, which
rclate to energy dissipation.
An advantage of motionless mix­
ing over stirred-\·essel mixing is the
elimination of bypassing. All Iluids
pass through regions of uni form
radial and axial mixing. whereas
lr " in stirred vessels is random.
l~;i,,~'I'l11nOW can lead to a problem
. the process requires the intense
,;[xing found only in regions near
.he impeller. These differences
rn)hubly account for why in-line
mhers invariably scale up success­
fulh. unlike stirred vessels, which
are ~)ften fraught with problems.
),lotionless mixers come in a
\'ariety of designs and are usually
made to fit inside standard pipe
,iZe5. Systems can be designed for
~ither laminar or turbulent mixing
applications.
Designs for in-line mixers are
based on the degree of nonmixing in
the feed and the desired degree of
mixing required for the product.
The quality of mixing is usually
expressed as the ratio of the stan­
dard deviation (of unmi xedness of
an added species) in the feed to the
average composition. Mixing is
generally considered to be complete
","'hen this ratio is 0.05. This is
equhalent to the "95% mixed" con­
di';(m often referred to in stirred­
\ )1 technology. The length need­
ed for the motionless mixer depends
on the type of mixer selected, the
initial state. and the final uniformity
specified. A comparison of types
can be found in Hamby et af. (5),
along with the design procedure. It
is also important to take pressure
drop into account. Efficient mixers
that appear to require ~port lengths
might also demand an excessive
pressure drop.
Testing the design
It is important to check all of the
process requirements to see how well
each has been met by the proposed
design. The checklist would include
the power to be used. the speed, the
gear box. and the ability to achieve
the required process result. Using
common sense also helps. An
impeller will certainly be inadequate
if it cannot produce sufficient upflow
velocity to overcome the solids set­
tling velocity.
An opportunity exists til the time
('. '\ant st~rt-up to me~sure and doc­
, f.:t performance. 01 course, there
often is a ~lrong desire to begin pro­
duction as Sl)on as possinle. If oper­
aling management can be persuaded
to permit the validation of the
design. however. this will add to the
knowledge base and pay big divi­
dends for future operation and
design. Routine testing is done with
water in the vessel. Speed, vibration.
and power draw (using a wattmeter)
are the first things to check.
An inspection of the liquid sur­
face tells how effective the baffling
is and how easily materials can be
added to the surface of the fluid.
Figures 7A-C show typical surface
conditions. Large-scale. high-energy
eddies, Figure 7A, promote large
surface waves. A large central vortex
is shown in Figure 7B, while static
conditions are shown in Figure 7C.
Conditions in Figures 7A and Bean
be used effectively for adding reac­
tants; faster mixing is achieved by
adding reactants to the impeller
region. Conditions shown in Figure
7C should never be used to add reac­
tants to a vessel. A camcorder can
help to record motion, which can
serve as a valuable future reference.
Mixing times can be measured
by a conductivity probe placed
inside the vessel. The probe is con­
nected to a high-speed recorder to
monitor changes in conductance
(and, hence, concentration). A trac­
er, often salt water, is injected
while the vessel is in operation and
the conductivities are recorded, if
appropriate. Tests can be repeated
at different water levels and agita­
tor speeds.
Draining the vessel is important
to see if mechanical problems occur
as the liquid passes through the
plane of the impeller.
Other pitfalls
Engineers also should guard
against the following common traps
for the unwary in the scale up of
mixing.
1. Reliance on rules:
Preoccupation with scale-up rules ­
e.g.. "constant tip speed." "constant
power per unit volume," or "constant
torque per unit volume" - usually
means the engineer wanls an easy
answer. Depending on rules often
creates problems because rules trun­
cate thinking. Simple mixing (slich
as the blending of nnnrc:li.·ting homo­
CHEMICAL ENGINEERING PROGRESS • JUNE 1991 •
geneous liquids). however. can often
be treated via rules. If truly simple
systems are involved in scale up.
consider the rules given in Table I.
which have proven succe\\ful in
our work.
2. Acceptance (~r eXiSlil1!{ condi­
tions: Energy is often wasted when
scale up is based on undefined needs.
In the case of a fermentation process.
it was found that reducing the original
mixing energy by 60% did not change
the process performance.
3. Undue secrecy: Honest. com­
petent equipment vendors can ,serve
as important resources in helping
you choose the most suitable mixer
design. if they are given adequate
information. Secrecy is important,
but harm can result when only
selected information is provided.
4. Rigidity about flexibilit}·:
System demands sometimes are too
broad for anyone design to handle
well. For instance, a single \es.sel
may have to serve as a blend tank. a
polymerizer, a devolatilizer. and
even a crystallizer. It would be
remarkable if any design could serve
each of those requirements equally
well. Therefore, it is essential to
assess the trade-offs between flexi­
bility and performance.
Occasionally, particularly at small,
remote sites, multi task designs must
be used regardless of consequences.
Mixing is still largely an art. but
it is becoming more scientific. In the
future. quantitative tools such as
computational fluid dynamics
should provide a better link between
design and performance. 8D
Literature Cited. " . ",-,'J
1. Oldshue; J. y.P."Fluid Mixing',
Technology," p.191, .;!,Vt.cGraw-HiIl, Ne~ ~~
York (1983). .,:,:".J . . '.. .,
'2. Cutter, L.
A., AiChllJ.. 12; p. 35~
'(1966). . .:;1\'" .; .' iij
.3. Angst, W., J. R~ Bourne, and P.",'
Dell'ava, Chem. Eng:·.Sci .. 39 p: 335,~
(1984). ~l~;,~.:.. . . . '.• :~
4. Leng, D. E., and G. J~. Quarderer, 'i
Chern. Eng. Commun.,.. ~4, p. 177 (982).:;;
S. Hamby, N., M. F; Edwards, and A•.;:
W. Nienow, "Mixing in the Proces(~
Industries," p. '226. 306. Bulterworths.·~
Woburn. MA (1985). ;i,i , .l'~
.~ ,: Ulbrecht. J. J., a~d G. K. Patterson;'~
'. UMixing of Liquids 'by Mechanical ..;
. Agitation." p. 93, Goro,o", & Breach. New::!
. York (I985)..,.,~" . _ '~'A
31