.

ot,l

Succeed at Scale Up

ailure to properly scale up mixing in mixing to promote the growth of large uni­
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
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
mixing can be
cess undermines many efforts. Mixing prob­ be achieved more easily in small equip­
lems are seldom recognized, in part because ment than in large equipment.
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. ing. These include:
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 • reactors inyolved with slow chemical
avoids them.
ty, quality, and profit, and they also can reactions;
lead to safety problems such as reactive­ • suspension of solids.
) chemical incidents. Although technical These foul can be considered noncritical
problems cause most failures, nontechnical applications, i.e.. they can usually be scaled
reasons also contribute to difficulties. up with few difficulties.
Scale up of mixing can be easy or com­ Many engineers are most familiar with
plex. Most difficulties arise when potential the latter, noncritical applications.
problems have not been well thought out. Unfortunately. they get the impression that
Hardest of all are multiphase processes in mixing is simple and can be treated casual­
which the chemistry depends on condition ly. Thus. it is not surprising that so many
Douglas E. Leng, of the phases. scale-up problems occur.
The Dow Chemical Co. Good quantitative tools and measures of
Jal performance are required to solve such Avoiding problems
ihaif problems. (See the accompanying article For successful scaleup of mixing in
on­ by Tatterson for an examination of these industrial processes, a designer should fol­
needs.) My 25 years of experience with low six distinct steps:
·'er ­ industrial mixing and scale-up problems 1. define the process need;
lac has led me to identify some general trou­ 2. identify all of the operational
~ion blespots and to develop a procedure for parameters;
eeds, successful scale up. 3. review the process history:
First of all, the engineer" must clearly 4. select the imponant process
understand the role of the mixing. Is rapid parameters;
attainment of uniformity critical to process S. choose an initial equipment design
success? The following are typical chemi­ vessel design, impellers. impeller location.
cal processes that depend on rapid attain­ bal'fles. and points of feed and exit
ment of uniformity: ~treams: and
• chemical reactors/polymerizers in 6. test the design relative to the process
which reaction kinetics are equal to or needs and assumptions and then fine tUlle it
faster than the ratc of mixing: to meet the needs of the most important
• competing chemical reactions where variables.
i' )
poor mixing affects yields; Many scale-up failures can he traced
• crystallizers thai depend on uniform 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
the impeller 10 distrihute the S,.uper­
heated hydrocarhon vapor. The
achieved by sparging gas into a
3,SOO-gal pilot-plant reactor.
ex:ampJes of problems. impeller was supposed. to disperse Finally. it was shown 'that condi­
the vapor into buhhles to· prtwide tions had been different in the pilot­
Defining the .process need mass transfer for the liberation of plant vessel. Sparging was accom­
. The design/~cale-up. process ammonia. driving the reaction ·(0 the plished by pas~ing nitrogen into the
should start with a thorough exami­ right to form the dimer (2 Al.On slurry of suspended solids in miner­
nation of all process needs. start-up, however, solids accumulat­ ai oil. Nitrogen bubbles had provid­
Requirements are often straightfor­ ed at the base of the vessel. causing ed the mass transfer needed to
ward. Sometimes. however. they the plant to shut down. The scale up remove the ammonia in the small
may he complex and even contlict­ had been based on invalid criteria, reactor, but, in the plant reactor, cal­
ing: For example. it might be neces­ which led to inadequate mixing for culations ot heat transfer from the
sary to exceed minimum shear to sat- . suspension of the solid. buobles to the surrounding fluid
isfy dem;)nds for flow and indicated tpat all bubbles had
uniformity. Vapor to
collapsed due to condensa­
Typical process needs Condenser tion. The liberated heat from
include: condensation was transported
• supplying a uniform slurry
to feed another processing
step;
• facilitating a controlled
chemical reaction;
!
385·hp Drive
to the surface by convection.
where it caused the top layer
to boil. Mixing, therefore,
also had to rapidly circulate
reacting solids through the
Feed from
• providing for mass or heat Second boiling surface layer to
transfer: Stage remove ammonia. Many

I,~\
Reactor
• dispersing liquid drops for mixing designs were pro­
a suspension polymerization posed. several were tested
45' psr Impeller
or extraction; and pro\'ided improvements,
• assuring continuous mixing but none was sufficiently
of added reactants or Isopar Vapor effective to permit continu­
monomers. from ing to operate the plant.
Petrochem
Avoid the temptation to Superheater Fortunately, problems of

I
Vapor Distributor
quickly accept the obvious such magnitude occur
without evaluating Jess obvi- infrequently.
ous needs. For instance,
solids must be kept in sus­ Identifying all of the
pension. but sometimes that • Figure 1. Sparged, lOO,OOO-gallon cofltinuously-stirred­ operational parameters
may not be enough, as tank reactor containing 45% solids. List and then prioritize the
shown in the following reasons for mixing. These
example. The major mistake was thinking may include requirements for mixing
A complex, three-phase, continu­ that adequate suspension of solids time (blending). micromixing, heat
ous-stirred-tank-reactor system was was sufficient to produce desired transfer, shear. solids suspension.
being scaled up from test data production rates. The suspension mass transfer (including liquid-liq­
derived in 3,SOO-gal vessels. The problem was solved by doubling the uid, liquid-solid. and gas-liquid 1.
reaction was an equilibrium dimer­ power per unit volume, as suggested introduction of gas into liquid, reac­
ization, described by: in tests, but that necessitated trans­ tants, chain terminators, initiators.
2 A (solid) ~ (2 A) (solid) + 2 NH. ferring the original drive to a stand­ and reflux return.
(gas) .' by SO,OOO-gal reactor. As the Textbooks on mixing note that
The reactor was the last stage of a revised plant got back in production, these operational parameters do not
three-stage train. see Figure I, and tests revealed good solids suspen­ scale up equally. Oldshue (I) illus­
contained reacting solids suspended sion was provided in all regions of trates this for scale up from a :::O-gal
in a light hydrocarbon. Melt from the the smaller SO.OOO-gal reaclor. The to a 2,SOO-gal \essel: If the power
second stage entered the 100,000-gal productivity, however, was only per unit volume (PlY) is held con­
l stirred reactor and snliditled immedi­ about 2S% of the projected rate for stant, circulation lime increases
ately to form a fasl-:-;ettling slurry that size of vessel. The reaction rate threefold, tip speed by 70%, and th\.'
containing 4S% solids. Agitation was was an important problem that had impeller Reynolds number by a fac­
\
' provided by a single. four-blade, 4So not heen solved, Further tests also tor of 8.S. I f processes reqUire both

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
revealed that sparging the superheat­
ed hydrm.:arhon was not effective in
removing the ammonia, although
constant PlY and shear to be main­
lained, condition;. of geomelric simi­
larity need to he n:laxeJ.
shaped distributor \\as located under ~H.'ceptahlc reaction rates had heen In miniplanh. nonsill1ilar geol11\.'­

24 • JUNE 1991 • CHEMICAL ENGINEERING PROGRESS

1111
 II

try is used to simulate mix­ 2.0()()-gal semiworb plant.

if'!!. in a large-scale reaclor: Input Intensity=1.0 howe\cr. agglomerates and
), example, when blend small lumps of polymer
tIme i, critical. miniplant formed. which necessitated
.;tudies can be done in a 'in-line product filtration.
reactor having a smaller Oth~r problems al~() appeared ,.
impeller diameterltank diam­
eter (OIT) ratio.
Identifying all of the key
but were controllable.
The full-scale plant was an
g,OOO-gal multi-pitch-blade
I
parameters is, admittedly, not Intensity=20
turbine installation. which
always easy, but the prob­ included an elaborate recycle 1., ;
lems that can be caused by system through heaters and
Intensity=5
J!
skimping on the analysis can coolers arranged in parallel. I!
be tougher. For instance, Problems greatly increased at 11 '
incomplete parameter identi­ Intensity=1
this scale and were unman­
fication led to the following ageable even with the instal­
problem: Intensity=O.2
lation of large in-line filters.
Production of a fine Calculations showed that
chemical was' being scaled the energy per unit volume , /
up from a miniplant to a was 120 hplLOOO gal at the'7
3,500-gal reactor. Agitation 5-L s,cale and decreased
was believed to be needed ill Figure 2. Schematic oj local relative turbulence almost linearly to 3 hpll,OOO
for solids movement equiva­ intensities. gal in the production reactor.
lent to the just-suspended Meanwhile. product contin­
state. In reality, the reaction rates Reviewing the process history ued to coarsen as larger vessels were
depended on several factors, per­ used. Since the initiator half-life was
haps the most important of which A process is often scaled up in only a fraction of a second, the sizes
was mass transfer between the two incremental stages to meet growing of particles were established virtually
coalescing liquid phases. The pro­ product-development needs. This instantaneously when the monomers
iuction facility was sized according provides an opportunity to observe entered the reactor.. Intense
,~ reaction rates observed in mini­ the development of problems due to micromixing in the small vessel dis­
plant vessels. Production rates scale up and can help minimize risk. persed the monomers much more
determined after plant start-up were Problems can be subtle, as seen in rapidly as polymerization proceeded.
found to be more than an order of the following example:
magnitude less than expected. A nonaqueous dispersion was
At small scale, high shear and being developed from laboratory
rapid circulation led to a dispersion­ through a mini plant, pilot plant, . D. E. lENG is a senior research .
controlled environment and small semiworks plant, and, finally, fuIl­ scientist ill the Central
drops with a large interfacial area. scale production. The product was to Research Engineering
At the large scale, shear rates were contain a certain fraction of solids in laboratory of The Dow
lower and circulation was slower, the form of micron-sized polymer Chemical Co., Midland, MI
with both factors contributing to particles. The procedure developed (517/636-3387; Fax.: 517/638·
conditions classified as coalescence was to continuously feed initiated 9674). He has worked for Dow
controlling. This led to large drops monomers into a vigorously agitated at Midland for 35 years.
and much less interfacial area. hot fluid to rapidly disperse the During the last 25 years, he
Because the kinetics were controlled monomers and provide uniformity has been involved primarily in
by mass transfer, the change from and heat transfer. The rate of poly­ mixing and multiphase
dispersion dominance to coalescence merization was governed by the rate research, applications, prob- ,
dominance explained the unexpected of the addition of monomer, which lem solving, and engineering
behavior on scale up. contained free-radical initiators with administration. He obtained a
The scale-up problem might have a half-life of less than a second at the BSc and an MSc from Queen's
been anticipated if the agitator had temperatures in the reactor. Univ., Kingston, Ont., and a 1
been stopped during early laborato­ Superior product was obtained in PhD from Purdue Univ. A fel- .{
ry work so that very rapid coales­ S-L glass reactors with the desired low of the AIChE and a mem-j
cence could have been seen. The viscosity, particle sizes, and percent­ ber of the American Chemical l
problem was greatly eased by age of solids. The results were not Society, he was the chairman, '.
adding a second impeller, which quite as good in the next size reac­ of the Engineering Foundation A
):ncreased the overall circulation tors, but cerlainly good enough to Conference on Mixing (1981) .. ';.i
rates and provided an additional maintain enthusiastic support from .' "-. '1
;,',?..;,":
region ror drop dispersion. management and customcrs. In the ,tii

CHEMICAL ENGINEERING PROGRESS • JUNE 1991 • 25

 -
MIXING

In larg('r s..:alc vessels. the kl.' rthe mass transfer coeffi­

mixing intensity was two cient). it is the interfacial
orders of magnitude less. so area. a"that is atTected in k1u
the dispcr;.ion of the measurements, Hen(;c kl.a is
monomer \\'a~ 'slow relative a function of the superfi(;i:l
to the rat(' of reaction. This gas velocity and PIV. the
r('sulted in a big difference in InterfaciaI power per unit volume,
the Damkohler number. Vortex For example. consider the
Clearly. increasing the scaleup of a microbial fer­
total power to the level pro­ mentation. The role of mix­
vided in laboratory-scale ing was to provide gas dis· ,
work \\'as not a dable solu­ persion, supply nutrient
tion. Instead. attention was Baffles blending, keep solids in
turned to assessing what suspension. and maintai'l
could be done to improve reI ati ve \y low shear. Th:
the mixing intensity at the broth became rheologically
II monomer inlet without more non-Newtonian with
II
increasing the overall mix­ time. The scale up was to
ing energy. The location of provide correlations for 80­
the monomer inlet was at a m 3 vessels in which the
region of low turbulence, • Figure 3. Improper geometry for the dispersion of desired dissolved oxygen
,
and local energy-dissIpation monomer ill water. could be maintained by a
rates in agitated vessels are combination of impeller
known to be highly nonuniform. attaining uniformity generally do not speed and gas rate. The criticn
Recently published studies (2,3) scale up well. scale-up variable was selected to be
have shown that regions close to Mixing time was used as a crite­ the kLa, so that equivalence in kLa
the impeller gave dissipation rates rion for the scale up of a polymer­ could provide similar dissolved
20 times greater than the average in ization process in which a block oxygen levels at corresponding
the reactor as a whole. Figure 2 copolymer was being produced. stages in the fermentation.
shows schematically that regions Polymerization rates were fairly Studies were conducted in 30-L
near the impeller provide more fast, and locally poor mixing gave and 2S0-L laboratory vessels. The
intense energy dissipation. Adding inferior results, leading to a product kLa measurements were made by the
the monomer through a cooled inlet with a broad distribution of side­ steady-state method: oxygen con­
pipe directly to the impeller dis­ chain lengths. Calculations indicat­ sumption was determined from the
charge stream worked so well at the ed what mixing times could be difference between the inlet and out­
production scale that filtration was achieved reasonably in the planned let oxygen concentrations and the
obviated. production reactors, and miniplant airflow rate. Probes measured the
Thus, careful observation and conditions were chosen that would dissolved oxygen in the liquid phase.
analysis gave warning that a prob­ duplicate these conditions. Tests The relationship between the two
lem, could occur, Fortunately, the were then conducted in the mini­ sizes of fennenters suggested a cor­
solution was fairly simple to imple­ plant to determine whether the relation of the fonn:
ment and worked well. product quality was sensitive to k aa.(PAl: 14(S )oAfi(lI)
L r~'
agitation rates above and below the where S~ is the superficial gas veloci­
Selecting the important pro­ calculated rate based on equal mix­ ty. It was necessary to correlate kL
cess parameters ing time. In this case. scale up was from a determination of the zero
Textbooks generally treat mixing successful. due in part to the recog­ shear viscosity (11) of broth sampled
as a series of topics that have little in nition that mixing time was a criti­ from the fermenter. The correlation
common. These topics can, however. cal fac.tor for product quality. proved to be accurate, provided
lead to an orderly checklist for Ga.~-liquid mixing usually impeIler flo\\' was sufficient to
selecting parameters that are impor­ relates to phenomena su(;h as gas entrain gas buhbles to the regions
tant to the mixing process. holdup, interfacial area (kiP, the below the impeller,
Blending of lIliscihlt! liquids deals mass-transfer coefficient and inter· Many published studies on
with topics related to design and facial area). and the ratio of power gas-liquid mixing have been done ;11
I impeller and vessel dimensions, and while gassing to power for the low gassing rates. conditions under
~ !
generally ends up with a discussion ungassed state (P /PIf~)' The latter is which mixing is fairly straightfor­
about mixing time. 8 m , A process is expressed as a ru'netion of the aera­ ward. Gas rates. however. arc usually
seldom scaled up oy holding mixing tion number QIND\ where Q is the much highcr in industrial mixing ­
time constant because this generally gassing rate, N is the impeller often I to 3 \'olumcs of gas per vol­
requires high power commitments. speed. and D is the impeller diame­ ume of liquid pcr minute - and can
Processes that d.::pend on rapidly ter. Sin(;e mixing has lillie effect on lead to impclkr cavitation. Wh~'n

26 • JUNE 1991 • CHEMICAL ENGINEERING PROGRESS

 that happens. impeller discharge catalYSt). form a suspension of such' as baffles. vessel \\alls. and
)lWS diminish and the dist·ribution monomer drops in water. heat to impellers. Conditions of shear lead to
,)j" ga~ in the vessel can change dra­ polymerize. polymerize. and finally drop collisions, High local shear
matically from fairly uniform to cool, The monomers were more rutes also leud to drop di'persion. In
poor. .-\5 discharge rates decrease. dense and initially formed the bot­ a coalescing and dispersing system.
impeller flow can no longer entrain tom layer. while water and suspend­ coalescence occurs principally in
gas and carry it to all regions. The ing agent formed the top layer. regions of low shear. v.hile disper­
region below the impeller near the Agitation begun, and heat-transfer sion occurs in regions of high shear
tank bottom is usually the first to coefficients were calculated online near the impeller. An agitated disper­
become void of bubbles. Under by the latest instrumentation. As the sion is both dynamic and periodic,
flooded conditions. the impeller can polymerizer began its first run. the Large-scale eddies appear. disappear,
often only distribute gas radially to heat-transfer coefficient feli from 50 and reappear from time to time. sug­
regions above it. The ratio PIPIt~ to less than 2 Btu/h/ftC/oF. reactor gesting highly transient behavior.
falls to less than 0.5 under these temperatures went out of control. and Colliding pairs of drops coalesce if
conditions. emergency venting to a condenser the forces pressing them together
Liqllid-liquid dispersiolls are was activated to provide evaporative endure long enough for drainage and
commonly associated with drop dis­ cooling and avoid serious reactive­ thinning of the continuous phase to
persion and the generation of inter­ chemicals problems. occur between them. If insufficient
facial area. Various mechanisms The monomer layer, instead of the drainage occurs. the drop pair will
have been proposed for drop disper­ water layer, had become the continu­ separate as fluid forces diminish.
sion. usually relating fluid forces ous phase. and heating had initiated Other factors. such as the mobility of
(laminar or turbulent shear) to drop polymerization - resulting in a the liquid-liquid interface. the defor­
surface forces. The fluid forces can mess. Similar results were produced mation of the drops upon impact, and
arise from impact at the walls. or in two further runs. The problem was foreign matter collected at the sur­
rotational, dilational or turbulent solved by placing a second impeller face. also playa role in the drainage.
shear. Resistance forces are com­ in the upper. water layer, which Our current ability to scale up liq­
monly those due to interfacial ten­ caused monomer to be thrown up uid-liquid dispersions depends on
sion or surface viscosity. The drop into that layer. Laboratory mixing whether the system is coalescing or
, breaks when fluid forces exceed tests showed that the single lower noncoalescing. Coalescing systems
cohesi\e forces. impeller created a large interfacial are extremely difficult to scale up if
The process of forming the dis­ vortex that allowed water from the equal interfacial area or drop-size
persion is also important. but it has upper layer to reach the impeller and distribution must be maintained.
recehed little attention. Consider become dispersed, as shown in NOllcoalescillg systems often
two separated liquid phases. A and B. Figure 3 , The problem was not involve suspension-polymerization
of diiferent density with A on top apparent in the 3,500-gal vessel, pos­ processes employing a water-soluble
and B below. To create a dispersion sibly because relatively lower tan­ protective polymer that collects at
of B in A, an impeller must be placed gential velocities existed, resulting in the drop surfaces and prevents coa­
in A. For the reverse. the impeller a shallower interfacial vortex that did lescence. Mixin'g for these systems ~)
must be placed in B. This sounds not reach the impeller. need only provide for dispersion and !
simple and logical. but its impor­ Coalescence of drops occurs upon suspension because coalescence is I"~
tance was learned the hard way: collisions with other drops, or virtually absent. Figure -+ shows that
A suspension polymerization was between drops and solid surfaces mean drop sizes become smaller and
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 suspension
reactor. Therefore. a prototype line, drops
10.OOO-gal vessel was to be tested are suspended
first: if it was successful, the remain­ Log
ing pl)lymerizers would be installed. Drop
Agitation at both scales was provid­ Size
ed by a single. three-blade. retreat­
.....f - - - - - - _ l _ Dispersion:
cuneo glussed-steel impeller located drops above

the dispersion
at the bottom of the reactor. The
line are
polymerizers had two finger baffles dispersed.
placed 1800 apart.
)
The polymerizer had to sequen­ Log Impeller Speed
tially mix the phm;es (waler with sus­
pl'nding agl'nt. and monomers with • Fi~llre -I. Dispersioll-suspensio/l relations/ri/ls ill slispensioll poIYllleri:.atio/l.

CHEMICAL ENGINEERING PROGRESS • JUNE 1991 • 27

 MIXING
------.---~~--------------------------~~~---------------------------

drops arc hetter slispenued as Becaus.e proUllCliol1 schedules occurs elsewhere. except initiallv.
impeller speed" increase. Decreasing usually do no! allow for allain111ent . 2. Coalescence occurs e,ery­
the agilalor spe\.:d uo\.:s the opposite, of "complete" dispersion. scale up where drop colli~ions can OCCllr.
The drop sile eorn.:sponciing. to the becomes more complicated. One 3. Circulation times increase
inter.scctipn Ill' the dispersion and ends up comparing completely dis­ greatly in large '·e,sels.
suspension line" is the largest mean perscd drops made in sillall equip­ The net effect of these three f~\Ctr)r\
drop size that can he produced under ment with partly dispersed drops is that dispersion dominates in sma! l
those specific conditions. The aver­ produced in large polymerizers. scale equipment and coalescem:c
age size of drops depends on either Therefore. agilation speed has to be dominates in large-scale. commer­
turbulent or laminar shear. while increased in the large vessel to pro­ cial equipment. .
suspension depends on drop sizes. duce drop size:.. equivalent to those Solid-liquid dispersiolls com­
density differences. and agitation made in the miniplant polymerizer. monly involve the suspension of
parameters (-J.). Coalescing systems are, by com­ solids' that are more dense than the
Another factor to consider is that parison. complicated to scale up suspending phase. A reliable way to
the time to reach a completely dis­ for a number of reasons. Rates of predict how much agitation is need­
persed condition is short in small chemical reactions often depend on ed to suspend solids is provided b:
equipment but long in large equip­ the interfacial area, which in turn the Zweitering equation (5;:
ment. A light-transmission apparatus hinges on two dynamic factors: i.;N = [5 VO• I d ~.: (g/).nlpp4~ X<),I3] I
- p p ~
for measuring interfacial area was coalescence and dispersion. Other
placed on a I.OOO-gal suspension important points for these systems .-DO.X5 "Iiu
polymerizer to measure the time are as follows: where: N., represents revolutions per
required for complete dispersion. The 1. Dispersion is localized near 5
second; isa constant that depends
noneoalescing drops were still being the impeller in regions of high on the selected impeller, its diameter
dispersed after 24 h of agitation. shear; practically no dispersion ratio. and bottom clearance: v is the
~ kinematic viscosit,·. m 2/sec; d is the
~' mean particle size, m; D "is tht
Table 1. Rules for scaling-up similar vessels under impeller diameter. m; X is the per­
centage of solids: (gt::.plp) is the
turbulent conditions gravitational constant times the den­
sity difference di\ided by the liquid
NDX =Constant density. mlsec:::'
Value of X Rules Processes The just-suspended criterion is
good for dissolving solids. but it is
Constant tip speed, Same maximum shear, inadequate if homogeneity is
constant torque/volume simple blending required; see Table 1 for recommen­
dations for homogeneous suspension.
0.85 Solids suspension Used in Zweitering A more difficult. and less studied.
i· equation for Nis, for problem is the one of predicting the
I easily suspended solids N for solids less dense than the sus­
pgnding fluid. In this case, the free
0.75 Solids suspension Scale-up of average solids surface does not provide efficient
suspensions geometry for flow reversal compared
to the curved bottom of a tank. An
0.S7 Power/volume Suspension of fast-settling effective solution for the case of
slurries, turbulent floating solids is to place a second
dispersion, gas-liquid impeller close to the free surface to
operations where kLa's help disperse tloating solids. This ini­
must be scaled, tiates suspension. and the second
refctions requiring impeller provides needed unifonnity.
micromixing An example for !loating solids is
.. 0.5 Constant Reynolds Similar heat transfer,
a process to produce foaming-in­
place beads. The process involved
number equal viscous/inertial adding cylindri,'ai thermoplastic
forces polymer granules ll1 hOI water con­
taining an antil'oagulanl. A foaming
0.0 Constant speed Equal mixing time, fast or blowing agent was added. and the
reactions contents were heated to above the
glass-transition temperature. The
Note: Using these rules for scale-up requires a Reynolds number greater than 10', granules changed from cylindrical to
and geometry of similar proportions. spherical particlc~ during the heating

28 • JUNE 1991 • CHEMICAL ENGINEERING PROGRESS

 :'1
:I

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

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

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

~--------------------~----~~
Big Eddies Vortex
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 A 8 c
from the surface. • Figure 7. Typical surface conditiolls: (A) Turbulellt large eddies promote good
The selection of the ratio of the surface mixi/lg; (B) Laminar conditiolls with large ce1ltral vortex - good for addi­
impeller diameter to diameter of the tion; (C) Flat surface, IlOt recommended for chemical additions.
tank (Din is also important. In·
industrial applications. ratios from higher viscosities, particularly where stall such problems. it generally is
0.25 to 0.65 are used for common heat transfer is a problem, special preferable to add feed streams close
impellers, while larger ratios are impellers - including anchor, gate. to the impeller inlet. Feed can some­ i
used for anchors, gates. and helical nelical. and double-helical types times be added to the bottom of the
types of impellers. If the process should be used. In cases where peri­ reactor where an impeller is usually
requires flow rather than turbulence, odic sweeping by blades of vessel located. In continuous processing.

\ DfT ratios of 0.4 to 0.6 are chosen.

For micromixing and processes
requiring turbulence. DfT ratios of
walls facilitates heat transfer, these
impellers can be designed to come
very close to the walls (or, in some
avoid placing the feed and exit
points near each other because this
leads to bypassing and distorts the
0.25 to 0.35 would be selected and cases. to actually scrape the walls). residence-time distribution.
impellers would be operated at high­ Some detail is given by Ulbrecht and Designs often make use of steady
er speeds than when flow is required. Patterson (6). bearings to help a\'oid mechanical
The trend in solids suspension has Fluids up to 3,000-4,000 cP problems associated with the use of
been to use smaller. higher speed require some degree of baffling. The " long, thin shafts. If steady bearings
hydrofoil impellers. These produce a'1 standard configuration calls for four ~ cannot be tolerated, however. an
coherent jet of liquid that impinges ( baffles 90° apart with a width of alternative is to U$e a shorter. thicker
on the bottom of the tank. resulting J Til 0 or Til 2 and located T172 from shaft and place the drive at the bot­
in effective suspension of solids and the tank wall. This arrangement tom of the vessel. Using bottom
resuspension of settled solids. works well unless the presence of drives eliminates clutter at the top of
Although the Rushton turbine is solids or non-Newtonian behavior the vessel and allo\\s more options.
commonly referred to in publica­ leads to regions of stagnation. Motionless (or in-line) mixers
tions, it is rarely used now for new Baffles placed midway between the should be considered as an alterna­
industrial gas-liquid installations. impeller tip and the vessel wall help tive to stirred vessel designs for cer­
An improved design is the concave to eliminate problems of stagnation. tain types of applications. Fast chem­
disk, which resembles a Rushton but particularly for thixotropic slurries. ~ ical reactions often are ideal
has six concave, semicylindrical Full-length baffles sometimes lead to applications for motionless mixers.
blades facing the direcliun of move­ problems because they create a rela­ Also. such mixers excel for applica­
ment. This provides excellent gas tively quiet. vortex-free surface- ( tions in which competing reactions I.

dispersion. can handle much more making it more difficult to entrain take place and backmixing must be
gas before flooding. and lIses less solids, liquids, and even gases. avoided. In-line mixers are also used
power than the Rushton turbine. A Baffles placed below the surface to improve heat transfer to exchang­
new hydrofoil with three wide blades allow the fOf-mation of a free vortex. ~ ers and pipe walls. Simple distribu­
is also useful. It disperses gas effec­ which assists the transfer of materi- :) tive mixing depends on the length of
tively and has little tendency to als into the vessel. the mixer and the number of ele­
flood. even at high gas tllnv rales. Careful consideration must be ments. Dispersive mixing. such as
The four-blade, 45 c -pilch-blade given to locations or the entries and drop sizing. depends not only on the
turbine is still used for systems of exits in stirred vessels. Materials number of elements but also the
moderately high viscosity. e.g .. those arc often added directly to the free pressure drop and !low rate, which
up to 40.000 cPo It pnnides more surface to avoid using dip pipes. rclate to energy dissipation.
local shear than the ncw wide-blade whit.:h can beconle plugged. Ir the An advantage of motionless mix­
J hydrofoil designs: the latll..' 1'. howev­ reaction is fast, the free surface ing over stirred-\·essel mixing is the
er. supply more flow and a beller must be turhulent to adequately elimination of bypassing. All Iluids
pattern and u~c less energy. At sti 11 cope with reaction kinetics. To fore­ pass through regions of uni form

30 • JUNE 1991 • CHEMICAL ENGINEERING PROGRESS

radial and axial mixing. whereas aling management can be persuaded geneous liquids). however. can often
lr " in stirred vessels is random. to permit the validation of the be treated via rules. If truly simple
l~;i,,~'I'l11nOW can lead to a problem design. however. this will add to the systems are involved in scale up.
. the process requires the intense knowledge base and pay big divi­ consider the rules given in Table I.
,;[xing found only in regions near dends for future operation and which have proven succe\\ful in
.he impeller. These differences design. Routine testing is done with our work.
rn)hubly account for why in-line water in the vessel. Speed, vibration. 2. Acceptance (~r eXiSlil1!{ condi­
mhers invariably scale up success­ and power draw (using a wattmeter) tions: Energy is often wasted when
fulh. unlike stirred vessels, which are the first things to check. scale up is based on undefined needs.
are ~)ften fraught with problems. An inspection of the liquid sur­ In the case of a fermentation process.
),lotionless mixers come in a face tells how effective the baffling it was found that reducing the original
\'ariety of designs and are usually is and how easily materials can be mixing energy by 60% did not change
made to fit inside standard pipe added to the surface of the fluid. the process performance.
,iZe5. Systems can be designed for Figures 7A-C show typical surface 3. Undue secrecy: Honest. com­
~ither laminar or turbulent mixing conditions. Large-scale. high-energy petent equipment vendors can ,serve
applications. eddies, Figure 7A, promote large as important resources in helping
Designs for in-line mixers are surface waves. A large central vortex you choose the most suitable mixer
based on the degree of nonmixing in is shown in Figure 7B, while static design. if they are given adequate
the feed and the desired degree of conditions are shown in Figure 7C. information. Secrecy is important,
mixing required for the product. Conditions in Figures 7A and Bean but harm can result when only
The quality of mixing is usually be used effectively for adding reac­ selected information is provided.
expressed as the ratio of the stan­ tants; faster mixing is achieved by 4. Rigidity about flexibilit}·:
dard deviation (of unmi xedness of adding reactants to the impeller System demands sometimes are too
an added species) in the feed to the region. Conditions shown in Figure broad for anyone design to handle
average composition. Mixing is 7C should never be used to add reac­ well. For instance, a single \es.sel
generally considered to be complete tants to a vessel. A camcorder can may have to serve as a blend tank. a
","'hen this ratio is 0.05. This is help to record motion, which can polymerizer, a devolatilizer. and
equhalent to the "95% mixed" con­ serve as a valuable future reference. even a crystallizer. It would be
di';(m often referred to in stirred­ Mixing times can be measured remarkable if any design could serve
\ )1 technology. The length need­ by a conductivity probe placed each of those requirements equally
ed for the motionless mixer depends inside the vessel. The probe is con­ well. Therefore, it is essential to
on the type of mixer selected, the nected to a high-speed recorder to assess the trade-offs between flexi­
initial state. and the final uniformity monitor changes in conductance bility and performance.
specified. A comparison of types (and, hence, concentration). A trac­ Occasionally, particularly at small,
can be found in Hamby et af. (5), er, often salt water, is injected remote sites, multi task designs must
along with the design procedure. It while the vessel is in operation and be used regardless of consequences.
is also important to take pressure the conductivities are recorded, if Mixing is still largely an art. but
drop into account. Efficient mixers appropriate. Tests can be repeated it is becoming more scientific. In the
that appear to require ~port lengths at different water levels and agita­ future. quantitative tools such as
might also demand an excessive tor speeds. computational fluid dynamics
pressure drop. Draining the vessel is important should provide a better link between
to see if mechanical problems occur design and performance. 8D
Testing the design as the liquid passes through the
It is important to check all of the plane of the impeller.
process requirements to see how well Literature Cited. " . ",-,'J
each has been met by the proposed Other pitfalls 1. Oldshue; J. y.P."Fluid Mixing',
design. The checklist would include Engineers also should guard Technology," p.191, .;!,Vt.cGraw-HiIl, Ne~ ~~
York (1983). .,:,:".J . . '.. .,
against the following common traps
the power to be used. the speed, the '2. Cutter, L.
A., AiChllJ.. 12; p. 35~
gear box. and the ability to achieve for the unwary in the scale up of '(1966). . .:;1\'" .; .' iij
the required process result. Using mixing. .3. Angst, W., J. R~ Bourne, and P.",'
common sense also helps. An 1. Reliance on rules: Dell'ava, Chem. Eng:·.Sci .. 39 p: 335,~
impeller will certainly be inadequate Preoccupation with scale-up rules ­ (1984). ~l~;,~.:.. . . . '.• :~
4. Leng, D. E., and G. J~. Quarderer, 'i
if it cannot produce sufficient upflow e.g.. "constant tip speed." "constant Chern. Eng. Commun.,.. ~4, p. 177 (982).:;;
velocity to overcome the solids set­ power per unit volume," or "constant S. Hamby, N., M. F; Edwards, and A•.;:
tling velocity. torque per unit volume" - usually W. Nienow, "Mixing in the Proces(~
An opportunity exists til the time means the engineer wanls an easy Industries," p. '226. 306. Bulterworths.·~
Woburn. MA (1985). ;i,i , .l'~
('. '\ant st~rt-up to me~sure and doc­ answer. Depending on rules often .~ ,: Ulbrecht. J. J., a~d G. K. Patterson;'~
, f.:t performance. 01 course, there creates problems because rules trun­ '. UMixing of Liquids 'by Mechanical ..;
often is a ~lrong desire to begin pro­ cate thinking. Simple mixing (slich . Agitation." p. 93, Goro,o", & Breach. New::!
duction as Sl)on as possinle. If oper­ as the blending of nnnrc:li.·ting homo­ . York (I985)..,.,~" . _ '~'A

CHEMICAL ENGINEERING PROGRESS • JUNE 1991 • 31