--

fPlt
-fa r gcnt p /"
.

e-t

y.JfrGe

$$fi
Doble Mukesh
GE India Technology Centre Pvt. Ltd

7r'{n'

chemical-reaction step is II ;tr*\; flowsheet for a new procls5 i.':* ii Taking that rsaction from th6,
A

,the

ant is
ard:Iti,'

ncc thc

viabilitv

01'a nurv l)roccss

is e-.tablished at thc gram lcvci

in tlre laboraton,. the

safctl' and hazar4 issues, as '*'cll as the irandling of rnaterials on a large

scale
[61.

proccss undergoes various scaleup steps

before it reaches the manufacturing plant. Because the capital investment required for tran-qforming a raw material to a finiShed product i,s proportir-rnal t0 ther caltacitv of'tiic planl

Keep in mind that there is usually a knowledge gap between bench chemists and process chemists on the one hanC, and chemical engineers and chemical technologists on the other. If

convcrsion, distribution betri'et'n tirt,' main product and byproducts. lrcat ef fects, florv patterns, backnixing. gasliqtrid-solid interaction and rssucs involving process controi.

THE PLANT IS NOT THE LABORATORY

Scveral diflerences exist betu'et'n Liit,, w:lv ?r proccss is developed in tlrc irib,rratorv ar-rd the rr'av it is carrierci r.rr-rt iri thc lrlant. As a sirnple exanrple. ir lerilc-

the scaleup activitY cannot

success-

thi' i) 6 -0.; I)o\\-('r. it r. rlcsu' ebic trl itrrlrl iis lrrllc ii plnnt as is t:ont

rliistil

srst,cnt rr,ith tht- cxpecttrci futrrrc kct fol the product [1]. -st:aler.rll

tlar-

{ull.r' I'rridge L}ris ga;t. t}rc rcsult-" in the ltrli-scalc plant rnay inclucle a reduccd f ield, longer batch c1'clc Limes, great,cr

rs thus a criticai activity

during the development of a chen-rical proccss. This article {bcuse-s main}v on st:alcup of thc rcur:tion stcyt, rvhich
n'pir:ailv represer-rts lhr: ireal't r)f lr ncu' J)r'{)c(rss. Thr: articlc as-st:mblcs a ri'idt rangc of practical rcaction-scaleup guidelincs that previousll' havc been dilfuserd throughout the en$neering

anounls of effluents or undesirable byproducts, unneccssarily hazardous operations, or unduly high consumption ofenergy. Regardless of the typer of proces-s involvcrd, the problems of scaleup are highil' sinrilar. Accordingjy, the information presented in this article
should apply to virtually all of the
chernical process industries, including such seemingly diverse activities as biochemical s'r'ntheses, production of paper pulp, and processing of metal orL's.
Iinori'lccigcnirle rcaction scalcup encr()r'n])asses sevr-:rirl ar-ipects o{- cht't-n-

tion carried out in a rouncl-ltotl onr flask in the research laboralon, ar .r

vcrticai-sided kettle outfitted rr'ith
n

very high speed of agitation might givl entirely different yields in a plant's

slolr'lv revolving mixer. Among thi:

reasons are differences in itatch cvclt: tinic, the degree of agitation. rvall t'ffect-s, and tl-re surface-to-r'olume ratit-r

litr:raturt'. Included are the key elerntnts in developing :r scaleup -slratr,rr'. and ti'rc unknori.ns tirat thc r:ngilrr,r,r nlust atldrcss carlv in thc scaleult
,

of the container. We focus successrvclr' on several such issues.

Batch cycle time

Ti're overall processing time inciuders not onlv the rcaction tinti.i-rrtr st,. lrrrl alsn thc t,inrc nr-.cded frrr foecling tlr, rl*r' nlrl.('r'rals, hcating thr' rll('lrutl>, cooling titc lrrrrcluct,s, rrncl tii:r'irrrl'r. rr.r and clcraning. Thesc time rciluir'()r'n(,nis are generaill' negligrbie in tlrt' laboll lory:. [.tt, nia\' bc on the orcier o{'.*e-r'crir] hours in thc full-scale plant. For cxample, it t1picail1' takc,s aborrl

.l',:,tr',i iillclttio jt is iiivi n il,rrt i: ,;i ir, scalrLtps irrvrrlving lgtllrl iolt tincl

lliring.

b:caus{'

thcr rilLt,r-r

p1'cs('nL

istn'.

cl-icnrrgal t;ngiri,:r'r'ing and flrrirl

:r'rr

cial chlrllcngcs [,']1. Intelirgcnt sr:aleup cntails finrling rind coliating all the infornration and rii'tii r^t:rlr.rirld lbr tlrr: dc'sign. cor-rst.r'trc:i;rin. :inrl siarlr.lp ol lhc nttrv full-srzt: irjrrri'. ii tlu.ii rtlso t;tkr'into lir,:('orrnt
46
3;iII",1ICi..i-

nrcrchnlricrs. I^rsur.s lrrising fronr kinct-

ics, themodvnnnrics and

hi'drodv-

nanric-. alfect lhe sclection of the herst t1'pe of reactor, it.s intc.rnal design anri

x'ill clictatc
JANUARY

its operat.ing rr:gimt:. Thcsc, in turn, reilct,or f icid, dergree of

2OO2

ENGII']iI-RIN'i

V/WVJ CHE

COI/

l
',

TABLE 1. vA[uES OF EXPONENT, FOR THE IMPEILER.SPEED EOUATION, f,, IN SCALEUP BY GEOMETRIC SIMII.ARIW For equol liquid motion or conslont
Froude number, ogiiotor-tip speed, sheor rote or grovitotionolefiects, D
For For equolsolid suspension, equol moss-tronsler rotes or powel

fill a 10-kI vessel via a 5rr-ilia. pipe. Cooling the contents : rr lLil-scaie reactor could require
.1-2 h to

= n=
n=

I 314 213 0

per unil volume,

rn the order of 1-2 h. Such exli,nded cooling times may pose

rrroblems :ii't.-chemicais. Heal-transfer is::Ltf:,{ relaled to scaleup are dis,-'us-sed in more detail in the next { f,,ction, as weil as later in the article.
temperature-sensi'i'irr, ratio of surface area to volume de,
S

Forequolsurfocomotion, n
Fot For constont Reynolds number or

equolblend lime, n =

= l12
= 2. =3

scale mixing. For instance, for dis persing a gas into a liquid, the, DuE,sug gested ratio of impelier diameter tr ter to tank diameter is 0.25; for bringinl nglng

for

constont hydrodynomic similority, n For conslont pumping copocity, D

gal, fuil-scale vessel, then the power

would have to be increased by a factor ' of I25, which is unrealistic. Similarly, if one rvanted to maintain the same agitator tip velocity during scaleup, it would be necessary to raise the agitator power by a factor of 25 [7], which is likewise impractical. So, instead, the elapsed liquid-circulation time in a full-scale vessel is

two liquids into contact (as in liq n liquidJiquid extraction), the figure i .rre is 0.4; and for blending of low-viscos iscos'eater ity liquids, it is equal to or greate than 0.6. Similarly, operations that depend on large velocity gradients but low circulation rates, such as gas dispersion, are accomplished at full scale with high-speed small-diameter impeilers. Operations that require high circulation rates are best done with large-diameter, slow-moving impellers.

urface-to-volume ratio

:i,iises as a reactor vessel is scaled r::r For instance, for a spherical ves.,,1. a r.olumetric scaieup factor of
lrt.()00 ri'ould mean a reduction in sur:iicr.-iirea-to-volume ratio by a factor ' r 21.5. Thcrcfore, to input or dissipate the ::i1nro amount of heat, the heat-trans' r i'atc must be increased in propor:r,;n i.r tire. rise in vessel capacity. This ::.er(r{rse can be achieved by providing r'-iriitional heat-transfer area or using : : sher heating-medium temperatures. ll,'rrr'ever, the latter tactic can lead to ,;,,'rcased ski.n temperature and local:

usually longer than

in a small one.

The question arises as to whether the longer mixing period affects the reaction process. A good test for the sensi-

As an approximation relevant for low-viscosity (waterlike) iiquids, it can be said that a mixer-power input of 0.5 to t hp per 1,000 gal of liquid gives "mild" agitation, 2 to 3 hp per
1,000 gal gives "vigorous" agitation, and 4 to 10 hp per 1,000 gal gives "intense' agitation (as might be needed during emulsification, for instance). These figures refer to the power that is actually delivered to the iiquid and do not include friction and gear losses.

tivity of the reaction to the

elapsed bulk mixing time is to perform the reaction in a geometrically scaled down model of the full-scale vessel, with the

.t.t:d overheating, which may raise

-;,ii.rv hazards or lead to the formation ; tar-n' or otheru'ise polymeric ''',;u'oducts. Another approach is to dei.,aS(1 the reaction rate so as to nratch 'l''r nraximum possible available heat:r.i or" cooling rate, but this option .r,,ids ro a longer processing time.

agitation speed the same as in the full-scale one. The results obtained at

these conditions are a good indication of the fuil-scale performance. Here is another example regarding the difference between small-scale and full-scale agitation. In the laboratory, one sometimes agitates the flask (or other vessel) itself, rather than inserting a mixer per se. In fermentation ,\gitation and mixing studies, for instance, most screenings ii aleup of mixing operations involves are done in "shake-flasks" mounted on ,r x"rdr: rang'e of issues. First, rve set rotational, shaking or rocking devices. ,:.,. ..tage ivith some basic points. There is no relationship between the in the first place, agitation must, as "pumping" capacities and shear rates ,; i)nlctlcal matter, differ rvith reactor achieved within these flasks and the , ;rlr, For instance, if we instead in- corresponding capacities and rates ex-ir,,cl on maintaining the same perienced in a fuil-scale fermenter out,.r,1rsr.d crrculation time in the fullfitted with a conventional agitator. , :r jt: \'.:SSl as rve have in a srnaller In short, it is unrealistic or impossir r. \\'i. r','ould liave to have highcr vebie to make all the mixing parameters rr ri,s. because the liquid n'ouid have of the full-scale vessel equal to the in', travei a greater distance. Accord- dividual fluid-mixing and fluid-me; Ii1. f irr\\'e r requ irctnt,nt 1_rel unit .. i chanics variabie in a small-scale tank. :un,,ol.r the fuil scale g'ould have to The eng:neer responsible for scaleup 'rl; in prcportion to the square of must accept this as a fact of life, which ril;rnrcter of the tank. is to be kept in tnind when appiying

Scaleup rules: At least three different kinds of scaleup rules for mixing have been published. Summar)' descriptions of them are as follorvs, rvitir more details available from the references cited:

Scaleup based an similarity concept [8]: In this approach, geometric similarity fixes the ratio of various lengths within the system. These lengths include impeller diameter D, tank diameter T, blade width b and liquid level

H. During scaleup (for instance. in

scaling up Diameter D 1 to D) under' this concept, the lengths are chosen such that the "before and after" ratio, R, is the same for each pair of lengths:
D2/D

t = Tz/T t = bzlb t = HzlH t = R The impeller rotational speeds,

ly';,

of the large vessel and the small vessel are related as foliolvs:

I'z = l{,'( llR)n

Based on theoretical and empirical analyses, suggested values of the exponent, n, for different types of agitation situations appear in Table 1.
Scaleup based. on friction latu of corre-

'

ir,rrt -satisfi'ing

that requirenrent

is

lhe purely mathematical scaleup relatronships presented below.

' lrnr.rrilr not feasjblt. economically. ,:' r,siilrpi. iithc po\\'er per unit vol':'r

Certain practical guidelines have

becomc common as regards relative

kept COnSlant befrveen ;,-;:ril pilot plant vessel and a 625r,\\'r.rl'{:, tO }tr:

impeller and tank diameters in full-

sponding states I9l: Under this theory,

CHEMICAL ENGINEERING WWW.CHE.COM JANUARY

2OO2 47

all mixing situations in the laminar regime are characterized in such a

rvay that the power number (a dimensionless variable that relates impeller power to other process variables, such
as N,

tional to AFD2; for laminar conditions, it is proportional to N2. I Accordingly, if the power per unit
volume is to be held constant during a scaleup, then N2 equals N/D1lD)a3 under turbulent conditions. And under laminar conditions, N2 equals N7.

where do is the particle diameter, and the power required per unit volume of the liquid is proportional 16 p-{.55. Liquid-liquid emulsion In scaling

D and liquid density

p) remains

inversely proportional to the Reynolds number. (Under turbulent conditions,

up Iiquid-liquid-emulsion systems, keep in mind that the shear-rate parameters (viscosity and surface tension)

the power number is instead

con-

stant.) The relevant Reynolds number is Duplpt,, where z is the tip velocity (equal to AD) and pr is the iiquid viscositl'. All the scaleup transitions are characterized rvith reference to this
reference rel adionship.

In applyrng this analysis, the flow

regin're is held fixed, whereas the val-

Scaleup u:ith gas-liquid mixing: In specifying rnixing equipment, a major principle is that. the impeller blade must be two or three times larger than the largest bubble, particle or fluid "clump" that is of significance to the process. So, when scaling up gas-liquid systems, be aware that a large vessel tends to have a wider bubblesize distribution than a smaller vessel

'affect emulsioir formation. Both the

blend time and the standard deviation of the circulation times for the individual droplets influence the size of the emulsion droplets. The average emui-

sion droplet size is proportional to N-2.56D4.17?1.88, and to achieve uni_ form dispersion U3l, N should be proportional
1o

2-2'15.

ues of N, D, and the power input, P,

are determined simultaneously.

maintain flou' similarity

To (or the same

[,l/]. Another consideration is that the size of the bubbles should not exceed
one-half to one-third of the vertical height of the impeiler blade. In the presence of gas bubbles, the
required blend time for the continuous phase increases. Accordingly, the percentage of gas holdup is an important factor in scaleup. The linear superficial gas velocity increases on scaleup, and there is usually a greater volume

degree of ,nixing), rvith a given impeller geometr.v, the parameters are related as fojiows:
.^y'

The position of the agitator plavs a crucial role in the formation of liquidliquid emulsions. To disperse higherdensity liquid into a iower-density liquid the agitator has to be located in the latter, and vice-versa, Blending: If two or more liquids witir

varies as U(D|T)2 P varies as Nv2 and I/(D/T) PIQ varies as I|(D/T)2

reiatively low viscosity are

being

n'here A represents the flowrate

t}'rrough the impeller. St:aleup basecl ort agitati.on intensitt, l/01. Thc nrore intense the agitation of the contents of a vessel, the faster

t]'rose contents become turned over. The vessel turnover rate, which is defined as QN rvhere V is the vessel volume. can therefore serve as a criterion

of gas hold-up in big tanks than in small tanks. So the larger-scale system entails longer blend times. The impeller rotational speecl, N, required for completely dispersing a gas in a flat-blade turbine assembly
can be found from the relationship

blended, so that the process is not affected by liquid shear rates, the difference in blend time and circulation between small and large tank is usuallv the only scaleup factor involved. Hou'ever, if there are large differences in density or surface tension between the

for tire intcnsit-"- of agitation. This approach en-rploys an agitation number, rV7. rvhich i-s scaled between 1 to 10 for rlverage btrlk-fluid velocities of 6 to 60 It/min (in other rvords, mild to violent
agitation ), respectively. For s1'stems that are geometrically

= QeTgo.tp.2D4

rvhere Q, is the gas florvrate and

g is

the acceleration due to gravity. This equation indicates that the rotational
speed required is directly proportional

liquids, then extra shear forces (and. thus, more input power to the mixer-) are required to achieve the ultimat,e levei of uniformity. During blending, there is a relative increase in Reynolds number ri'ith scaleup, regardless of the relative

magnitudes

lhe

sirnilar. the impeller tip speed, ND, of

scaled-up vessel

equals

to the square root of the gas flowrate and tank diameter, and inversely proportional to the square of the agitator diameter. Of course, the power redecreases with the increased presence of gas. Solid suspension.. In a suspended-

of the incoming-fluid properties. The time needed for blending, l, is proportional Lo TH|ND2. And
in
geometrically similar tanks. proportional to 1/l/.

is

the torque per unil volume is constant if A'iDl = ItzD,:. Accordinglr', torque per unit volume equals 3.27 Nppl'{ fllg,(HlT)1,
3.S:r2lrttl(DlT\1.5, and

quirement

for agitation

Agitation plus heat transfer In the scaiing-up of manv homogeneous, stirred systems, the rate of
heat transfer controls the design of the heat-transfer equipment. In such
systems, h is proportional
16 Jrnrlnr-1.

where Np is the power number and g. is the conventional conversion factor betu'een force uni[s. And the vesse]

solids system in which the solids account for up to about 30Vc of the total

rveigl'rt, scaleup
keeps the solids

of the mixer

that

rvhere

turnover rate. Q^', equals i0.8

.\'//l fr,'.t, I] {f P.:'.r1. . Pou'er requirements: For a scaledup reactor, tiie po\\'er requirement per tinit volurne, PN, can be determrned from the agitator speed. For

suspension poses no problem 1121. On the other hand, concentrated slurries start behaving likc viscous pseudo-plastic material, rvhich complicates the scaleup task.

in

/i is a heiit-tlansfer

cor,l'fl

cient, u is the fluid circulation velocit1',.d is the characteristic dintcnsirrn of bhe system (for instance. the agitrrtor diameter) and m is an entpiri-

ttrrbulent conditions, PN is propor48

The minimum impeller rotational speed required for suspending solids, Nrp^, is proportional to d00.2 1D0.85,

cally or experimentally deterniineC

scaleup exponent whose value is generally around 0.67.

scaleup based

on holding the

CHEI'"4ICAL ENGINEERING WWW.CHE.COM JANUARY 2OO2

I
TABLE 2. EXAMPLES OF INNOVATIVE REACTOR DESIGN FOR SCAtE.UPS
Process lssues

Smoll scole Scoled up version setup

U-tube converter
Petd dish

. Highly exothermic of benzene lo moleic onhydride . Needs efficienl heol removol . Mold growth smolhers orgonism 2. Pencillin by fermentotion . Need conirolled surfqce growth

i. Cotolylic oxidotion

Methyl lerl-butyl ether from isobulene ond melhonol wilh ion-exchonge cololysl 4. TAX (l -ocetylhexohydro-3,5 dinilro- 1 ,3,5 triozine)

.Exothermic

'Cololysl deoclivotion obove .Swelling of cololyst

. Exothermic . Eosily delonoble

I '10"C

Stined
vessel Fixed bed Slirred vessel Stined vessel

Chombered multi-tube reoctor with cooling iockei (l9J Submerged fermenlotion lechnology, lor mold lo grow submerged in the liquid food source (l9J Fluidized-bed reoclor to overcome hot spots ond occounl for swelling
ta anl

Low-dio. tubulor reoctor with cooling

moleriol

iockel (fost heol removol, ond omoun

of delonoble moteriol is smoll) (21) Plug-flow reoclor wilh cooling iocket, slightly lilled upwords from horizontql to ollow gos escope f2lJ Slotic mixer reoclor (21)

5. Sevofluorone (non-explosive, inholing onoeslhetic) from h e x of luoroisoproponol, HCHO, onhydrous HF, oleum 5 Sullolion ol mixed lollowderived olkonolomides with
chlorosulfonic ocid (a phormoceulicol product)

Exothermic

Detonoble Low volotility ol producl ond qos releose

.

.Gos releose

Highly viscous

.Connol use onlifooming ogents .Cololysi ottrition due lo ogilotion .Gos leok ol ihe glonds due to
high pressure

Stirred vessel

7. Hydoxyl ommonium
phosphole from
N

CSTR

Continuous, spqrged bubble column

(see moin

(2t)

HaNOr+H3PO6+Pd+H2

texl)
Gossporged Pocked column {or gqs-liquid

Aulo-oxidotion ol corene with . Exothermic . Low gos-fo-liquid moss tronsfer homogeneous cololyst
'?. Suspension polymerizoiion
. Lumps

formed by feeding inilioled rnonomers (micron-sized polymer dispersion formed !n non-oqueous medium) 3. Suspension polymerizotion

of polymers formed, needing inline product filler in lorger scole

conloct ond exlernol heot exchonger stirred vessel in lhe recirculolion loop. (22'j Semi-bolch Locote monomer feed slirred inlet pipes directly ol the impeller reoclor zone to improve ogilotion (23)
Semi botch

Trcnseslerficotion ol fotty

ccid ond sorbilol, lo

produce surfoclonl

lmproper ogitolor design leoding lo lormotion of woter droplets in monomer (insteod of monomer in woter), cousing o decreose in heot trqnsfer coefficienl form 50 lo 2 Btu/(h)(fiz)('F) Reduced yield Formotion of oleic ocid droplets in sorbilol, insteod of sorbilol in oleic ocid os desired

siined

Second impeller in the upper woler loyer (2j)

reocior

Stirred

botch reoctor

Roising ihe impeller lo locole il in lhe oleic ocid phose

:i rIirlrsii,r ctielficient c0nstant is rlr i,lt in cascs rvhere pilot plant

:

; ii,.- inclic:rle that tiic heat-triinsfcr

r-t;itt,',, ilt, tt'ltst's ::l()\\'l\' {)\'cf il '. ilr:r 1rr. lirl instlncr'. thc firruta: rri lltrlr lttcrtc or lat'rv dcPosiLs ::.l t.hr heat lran,sler are:r. (Onc - -.i'i, ruLrsc of' snch dcposits is a rii/,r';liulo sr.lnsilir-itl in the mater'l'l.,rt-'. 1i,r lLrt agitatcrl svsl:cnt.

it is olten considered essenrial to assurc that lhe same rabe of hcat transfer is maintained in tl'rc lalgt:-sc:rlo urijt. t,c, avoiil r-nirtct'itrl
material,
dt:gr:rclation. l'rtr Lhrrsc cascs, lr2l/r1 rtrtrsl eqrlal D2lD j, rv[ic]r me:rrts Lhat,

Scaleup can instead be baserd on mainlaining a const,ant imptrller-tip slrt:cd irr thc agitated vessel. In lhet
/r,/h 7 cqual-" (DelD t)"r-t .1'his a1rproach n'ray be rclcvant wl'ren bubble breakagc is an issue.
casr-'.

for geometrically similar

m
.

vessels,

Maintaining dr.namic sjrnilaritl

tlnd(')' tulhulettt flrlu rcqrtir,,s c,'n-qtant, values ol the Retrrold,q nunrircr' at Lire inrpcllel ttp. Sut:h sintrlalitr'.
.,vlriclr i-..

Nc/.ly'7 equals (D clD rlr2'2nttt

' .
,1.,i

D-i

l), 'r I rr' '/'r

.. ,j t.,:l) .1 i !
;.,.1\\'t,r

"

"i
a

I)i,r unit voluntt tn Strcrlt r',1 rvrii.s;1ll Lrit rrs lollorvs;

, [',ii,-: . D,l'-.trt.t!!t] f I) -. tt:l-'1tn\itrl

fiervevcr, this latter relatior.rship indicates thiit the inrpcllcr rotational specd in the largcr r-init should bc ,.qtu'l to {rl {r('.ttcr- tltar tliat rt thr' srniil.I-st:l l': urr rt i clcpr:ncli n g ulton thr: i alrrt' oi lt ). J'huL stipulirtron is conlrarl' lo nornral practice gcnt:rallv, irgita tol s peecl ciecrreases rvi t.h st:aIeup. Furt,irermore, such a scaleup principle is not vr:n' practical (even u'hcrr con-

ibr rnst,ancc. usclirl rr-it lr n()n-\\-\\'Ioniill] flLrid-.. gu.rriitit(,r.: -.inrilur nrappirlg-q (fron small to
scirlcd-u1l vc-sselsi of lht: r'atios rrl local to averagc rate-q olencrg-'- clissiJration. As a rtrstrlL, A-.2/AIi ttquals \,D ti Dri-.

'' ";.; '. ', t'til.'l','rr'''l pt't'rttiil , i,,,r,,,111'. :(.irlr,(l LII) ilt ltrrllti'r 'ii, .,:r{'llttltl l.r,r'.\'r.l' (ll tirt irgi'i:,rt-'r,1,
l

lltc grc:rlcr' 1)l' r'riirtl lr)tirti,)lral spt'r,d irr thc, sclrlt,rl'up vlssr,l, along * itir thr,
sidclt:ri esscntial
). ber:ausr:

PUTTING THE PRINCIPLES TO WORK

il,.':, iclt's l pplr-r n g r.l rc grlrrrrr l r',.1 r t ir,n .lr t 1t. .j' 151 ri rscrrssr-'1. I irc cr rgrrr,'t.r' tlr r'n'ing orrt a -scaleulr must. aiscr kcep in rnind a varict.v of'l.rractical considera-

' i,:;1 '. i' rnf,'r'.rlrtt0-:, tlsilirr'

r.lltlr agitet,;r riiarrrr:tcr. lcads to n0tablv high po\r'er costs.

::i

CHEMICAL ENGINEERII.IG WWW.CHE.COM JANUARY

2OC2 49

tions. Many pertain to specific reac-

tors (see below). Others are more

widely applicable:

. Botch uersus continuous operafron: Although the laboratory rvork may have taken place on a batch
scale, a continuous reactor (such as a

simple one. And when series or complex reactions are carried out, the product distributions for the two op-

Fluidized-bed reactors
Because the circulation of the catalyst

tions differ.

If a tubular

particles minimizes the temperature

reactor is

chosen, its diameter affects the radial and axial temperature gradients, which can introduce heat-

and concentration gradients,

the

choice of a fluidized-bed reactor sidesteps the problems, just discussed,

stirred-tank design) is iikely to

scale processing, especially

be

superior for high-throughout full-

transfer and
challenges

flow-distribution

that are inherent in the scaleup of packed-bed reactors. On the othe'r

hand, the effect of the carrier-fluid velocity, and of the physical properties of the catalyst, upon bed activity, bed ex-

in

cases

invoiving a single reaction step and requiring only a short residence time
o

Scaling up frxed-bed reactors

For the scaleup of a fixed-bed catalytic reactor in which a first-order reaction is taking place under isothermal conditions, proper scalcup demands that catalyst particle size and bed depth (or height) be kept constant while the cross-section is multiplied by the scaleup factor. In the laboratory and pilot plant, fixed-bed reactors operate under plug-

Temperatures, concentrations,
residence tim-es: Temperaturc and conccntration gradients, as rveli as residence-time distributions, will not necessarily be the same on a larger scale. The differences may adversely affect the yield and product purity. Such considerations may

pansion and catalyst attrition must first be studied thoroughly. When one scales up a fluidized-bed reactor, it is not suf{icient solely to understand the effect of increasing the vessel size _- the interaction of the

solid catalyst with the fluid

also changes. A ruie of hydrodynamic simi-

. Prouision for heat transfer: The

engineer must decide between using jacketing or a coil for the heat addi-

lead to the selection of rsothermal operation for the scaled-up plant

larity for a scaie change in fluidized

beds has been developed, based on the

flow conditions (ust as stirred-tank reactors operate under weil-mixed isothermai conditions). But it will not be so in the full-scale plant. The temperature and concentration gradients can never be made to be uniform, which leads to a difference in effective heat conductivity. For constant fluid velocity; the reactor throughput increases as the square of diameter of the tube. But with the increase in diameter during scaleup, temperature-distribution effects wiil be more pronounced. With exothermic reactions, the center of the tube will experience the highest temperatures;

governing equations of bubbie and in-

tion or removal. Coils are attractive rvhen a high heat-transfer area or coefficient is important; conversely, coils should be avoided and jackets used rvhen, for instance, the process liquid is highl"v viscous or prone to cause fouling, or contains a high

terstitial gas dynamics []41. In addition to the maintaining of geometric similanty, scaleup of a fluidized bed requires maintaining h1,drodynamic similarity. This latter similarity rule requires that the foiiowing trvo conditions be satisfied:
(U o

- U *l

= mu2(tJ u - U rrii

and

t Reactant purity, and oncethrough uersus recycle: Take care

that in the full-scale plant, the reactants entering the vessel are pure enough to avoid poisoning the catal1,st, or fouling the catalyst bed or
heat-transfer surfaces. In some systems, similar concerns may arise with using recycle rather than oncethrough operation The catalyst: In a full-scale plant, a

percentage of solids

U^f = mu2(U

where Uo is the superficial gas veiocity, U6 is the minimum veiocity re-

^)i

with endothermic reactions, the temperature there will be the lowest. The resulting radial temperature gradients, like hot spots, can cause loss of selectivity, coking or fouling in the catalyst bed, and, sometimes, mnaway conditions that may lead to unsafe situations or destroy the bed. In pilot plants, small catalyst parti-

quired for fluidization, nL

is the scaleup factor, and Subscript i represents the base-case (before scaleup)
condition. The first condition assures
geometric similarity in bubble coalescence; the second assures the geontet-

ric similarity in the flou,field.

These two conditions can be thought

n'ide range of catalyst-handling issue-s can arisc that are not necessarolrvrous at Lirc laboraton' ,sc:tle bnt can afferct the catalv-st activity. lif'e and regenerability. Exarnples include the catal5ust shape and dirnension-s (for heterogeneous catalysis),

of the necessary and sufficient, conditions for hydrodynamic similaritv. F'or scaleup and development probk'nis. it is suggested that both the hydrodr'namic-similarity rule and the identitr' rule, described in the next section, bc applied. Identity rule: The identitl, r'ule dcals only with increasing the diameter of a fluidized bed. It is especiailv useftrl f'or

ilv

cics are generally preferred; for one thing, they minimize mass-transfer
effects when developing the rate equa-

tions. But for full-scale plants, the

usual tendency is to opt for larger particles, to reduce pressure drop across the bed. The engineer must ke'ep in n'rind that the los'cred prc-ssurer drop conles at the cost ofa lou'ered reaction

anil ]ro*' the catalysl is prepared.

Also to be considered i-s horv thc catalvst is charged and di-"chargecl Stirred-tanh ler.su.s tubul.ar re-

actor: ])er unit of volrrmc, a fullscale strrred tank is less expensive than a tubular (nominally plug-flor,r') reactor. Horvever, the choice is not a

rate, due to intra-pellet heat- and

sludying chemical reactions; that is, for cases in rvhich the fluidize'd particles consist of catalyst.

ity or effectiveness of larger

must be predicted beforehand.

mass-transfer resistances. The actir'pellets

According to this rule, the catall'stparticle size, bed height and gas ve-

50

CHEI,4ICAL ENGINEERING WWW.CHE.COM JANUARY 2OO2

Process

i. Polybutylene
terephtholote from bulonediol ond cotolyst

2. Bioreoctors in woslewoler lreotment 3. Rodicol-initioted

suspension

polymerizotion of
styrene with butyl

methocrylole

TABLE 3. SOME ISSUES ARISING DURING REACTOR SCAIE.UP Observqlions during scole-up Setup lssues . High heoting role ochlevoble ln smoll . High eslerificotion Stined (polymeizotion) rqte will scole, not in lorge scole, due less heot-lronsfer oreo vessel . Heol buildup in loler stoges per unit of reoctor volume . High ogilolor tip speed in lorge scole leods lo polymer gives more of degroded producl (24) degrodotion . Mixing k1o does not depend on reoctor size but is proportionol Airlifl to U,ro. no* 0.86 (25) reoclor . O2-lronsfer tote lo liquid .lncreosing reoctor size leods to Slined Moleculor weight ond - increose in moleculor weighl ond polydispersion polydispersion vessel - increose in initiotor quontity to mqinloin some Porticle size moleculor weight Auto-occelerqlion - longer time needed to ochieve oulo-occelerotion behqvior
(26)

4. Suspension Stirred polymerizolion tonk of vinyl chloride 5 Finol slep to vitomin 86 Stirred (diozotizotion of nitro lonk to omino compound) ,5 I'Jeutrolizing on ester Slirred prepored in dilule, lonk olkoline, olcoholic
solution using ocid

. Porticle size . Solid suspension . Drop in yield

.
Excess of hydolyzed

. Size vories with rpm -0.e, height-0'I3, ogitotor dio. -0.e . Minimum rpm vories with ogitotor dio. -l.l
(27)

. Lorger liquid surfoce leods lo higher liquid evoporotion rote ond chonge in concentrotion
(28)

side product

. Longel oddition time of ocid leods to reoction between woler ond ester

/ lieutrolizotion

o{ lobile

Slirred

ester using NoOH

lonk

Bose-coiolyzed decomposition of side producl

Longer oddition time of olkoli leods lo decom-

posed product, due io high concenlrolion grodienls Use of No2CO3 os neulrolizing ogent ond increose in ogilolor rpm, to decreose pH grodienls Addition of olkoli to oqueous-rich porfion leods lo

dilution [28)
3. Biochemicol reoction
using onimolcells Slirred

Teoring of bio-orgonism

. Use of shoker

ogitotion poses no problem in smoll

lonk

9. Production of
surfoclonl using oir for oxidotion

Stirred

botch
with oir

bubbting

l0 Gos-phose oxidolion
I

CSTR

I Three-phose
equilibrium reoction
rvith 45% solids

CSTR

12 Fine-chemicol

Stirred-

production with two

rmmiscible liquids
3 Crystollizotion process (suspending solids in

tonk reoclor
Stirred-

tonk

liquid lo ochieve good blending ond ovoid crystol breokoge)

reocior

High tip speed in ogitoted vessels leod to teoring ond breokup of cells a lncreose in viscosity during reoction prevented N2 in Foom oir frorir escoping; use of puie 02 obvioted this prob-lem Excessive heot generotion a Decreose in heol-tronsfer coefficient due to foom lncreosed botch time increosed the bolch lime (5) Use ol diluents con reduce reoction role Heol removol Decreose the process volume Moinloin the low conversion (6) Use of N2 sporging lo drive the gos (2JJ to inodeLow conversion due quole removol of second goseous product, NH3 . Use of second impeller lo oller the regime from lnsutficienl liquid droplet coolescence lo dispersion-controllin g (23) sheoring, leoding lo coolescence ond formolion of lorge droplets . Locote diluent oddition neqr the intoke of Non-uniform, brooder size impeller to ollow crystol growth rother distribution in lorge scole thon nucleoiion to dominote f23l

scole

rr'. nrrrst all be hcld constant dur.';1lr,i1r'r Srr ntrrst the clintensions r l i. ii,rv, -rlistriltLrtion cquipnrent.
r; ;r: ljrr,,rrifjce rlirtnrr;tcrs. and thc

bot.h the small and the largc scale. The ir-rcrease in the capacity of the svstem is purely through the increase in t,he cross-scctional area of t,he {luirliz.r'cl hrrrl
.

other structural parameters are all changcd in the sarnc proporlion:

tn =

' rJ'rii {it)r)tl llt'i,il oll titl h:rst.

Ol

H,/II, = 7.,/7, = prlp, = d rlcl, ri'ltt'rt, tiit' Srrlrst'r'rpts s ;rntl i t'r,i)r'('s('n1 1ltr, slrr;ril- rrrrrl lru'rlr'-srlrlr, ','r,:-st'ls. r-cs1u:ct ivclr i''or lttirining 1hc gconrt.tricaIlv sirniiar {luiciiz.ing conditron bct,n'r'on ll,-,ds of different scaies, the similaritv nrle also reqrrircs t.hat both the fluidizing.

'li:- Iiir, :: :irit:ii,'tj. iirt 1t;r('ilr)ll

r

Sirrri/rrrilr' r'ttlc:'l'lris rrrlr' nt'r'liitt'ts tcr itltilllurlq gt,onrctlicitilv stntilat' flLridiz.ing cortclitions betq'ccn lteds of dif:

; !' f ,],,.t .lr.\'(rI(JI)i n

r

:' :r',:

'v' jil iltrrittr' 1()r olh('r qtar:ttttetr:r i,, ilrr', loncituclinnl clistribtr',1' :
i:

g an rl tltt-

il

\'(\rti

g,-(l

{'crt:nt scirles.'lhe fltridizing condiliort

in a geom-etrically similar rnodel nt

tinres larger than the base ntodel assumes that the bcd ircight H, the colirnrn di;inrt'1et' Z, the clistrilltrtion-ori{lr'<' rliantcit'r' r/. tht' oriflce pilch pr and

itr, l,rrirhle'sI can l-loLh hc kept

'

rr)rrir.lr- cortstirnt. ;tnrl llrcrt:'::,, lri.rrtr,:rl rr';rc'tion lrt'hltvirtr 1,, ,,r'i;,.,'ii,tj 1l lrr. irl,'ltiir:;rl ()n

gils vr:locitv ilncl thc minirnunr fluicliz.ation vt locitr, lte variccl prclpor'tionatclv rl'ith thc sq\lelc root of thc
2OC2 51

CHEMICAI- ENGINEERING WWW CHE CON4 .JANIJAFY

scale ratio.

A consequence of this is that the sintilaritv rule does not reqtrire geometrical similarity for the
particies themselves.

resistance. The modifying effect depends on reactor type and size. There-

solids. Based on
N Dru
12

fore, transport resistances are critical

laser-Doppler anemometry studies U2l, it has been found that

I (bU
4

in the scaleup.
Three-phase contact is achieved in either a stirred slurry reactor, where mixing and solids suspension are

d pu

6) =constan r

Stirred-tank reactors For scaleup of a continuous stirredtank reactor (CSTR) with multiple impeilers and a large height-to-diameter ratio. studies have shown that the ratio r of the internal circuiation rate to the vessel throughput q should be

achieved through agitation,

or

kept constant [15, /6]. The internal

circulation rate for geometrically sim-

trickle-bed reactor, where the catalyst is held firm in a packed bed while the liquid trickles down the column slowly and the gas rises from the bottom. The slurry option is the more popular.

In general, when geometric similarity is maintained, lower stirrer speeds are needed for suspending solids in larger tanks. However, small difference in the exponent on b lead to large

The fundamental assumption

in

ilar svstems is assumed to be equal to

the impeller pumping capacity Q,
so

r=Qlq
Q is proportional to l/D3. The ratio of pou'er in sniail and large scales for geometricaily similar systems (that is, D is proportional to T).and equal den-

slurry reactor is that the solid is homogeneously dispersed in the liquid. In developing and scaling up this type of ieactor, the most critical elements are understanding the hydrodynamic issues, the liquid circulation pattern and the slip between the
solid and the liquid. The size of the gas bubbles depends on the dynamic equilibrium between

differences in the power consumption per unit volume. For given impellersize ratio and clearance ratio, the cntical speed is almost the same for turbine and flat-paddle impellers but

the turbine version draws twice

complete suspension of solids.

as

much power as the paddle (and 15 to 20 times as much as a propeller) for

sily on both scales will be as follows:

P(.I P" = (?., and
.s

lT,)4 (qrl qr)3

scale

s'here Subscript c is for large

the bubble coaiescence and breakup

throughout the column. The specifics of those two processes in a given case depend on the physical properties, operating conditions and localized hydrodynamic behavior of the system.
The presence of solids affects the coalescence and the breakup of bubbles.

Biotechnology-process scaleup Scaleup of agitated-vessel processes that use animal cells poses special problems. For one thing, the tips of larger agitator blades tear at increased shear rates. Conditioning the cells to withstand the required sirear,

for sn'rall scale. Also, for geomet-

rically similar systems and equal mean residence times in both the
scales, the vessels throughput

will

be

related as,

i'q1q)r/3 = TJT,
These trvo equations lead to P,JP. = (T,J'l r\L =
(q

or encapsulating the cell organism in or on micro-scale particles, are trvo of many strategies being tried to sidestep that problem. Both the shear rate and the circula-

The bigger the particle, the more the

rlq.)5/3

Accordingly, a tenfold scaleup of the tank diameter means an increase in power requirement of about 105 for

bubble breakup is promoted. The holdup of solids-free gas increases with increasing reactor diameter, and liquid holdup correspondingly decreases. The liquid holdup governs the

tion rate affect the solid-liquid mass

transfer rate. Larger particles tend to siip behind the liquid motion, whereas smalier particles tend to follow the flow pattern. In aerobic biochemical processes, the living organism should have access to dissolved oxygen

the same process result, which is unrt:asonablc to achieve.

Successful scaleup

has

liquid residence time, which is the principal scaleup parameter for predicting product yield. The bubble
shape and prevalence, and the resultant rise velocities, are also important fbr reactor performance.

throughout the tank. Top-to-bottom

blending to meet that need is especially important in fermentation reactors having height-t,o-diamerer (.1'Il'ft ratios of about 2:1 or greilt,er. F-ernrenters withHlT greater tiran 1.5 require dual impellers: the lorver can provide the shear for air bubbles, rvitir the higher providing axial and btrlk mixing tl8l. scaleup of aerobic fermenters is based on the criterion that the oxygen-transfer rate rnust l.r(' gleater than the pcruk ox1'gr-'r'r-u1ltakt, rate of the organism. Sdccess stories Tabie 2 lists examples of reactor clcsigns that have been adopted rvhile moving from bench to larger scale of operation. The laboratory-scale de-

been

achievr.d for the continuous biending of loiv-viscrisitv fluids using the criferir.rn t,hat q/Q is held consLanL 1171. This crirerion rs similar to the one discussed earlier in this section. The relationship PJPr= (?"/?r)5 has Lreen found to be valid for a continuous

stirred-tank reactor by other authors, for rrierrtical reaction yields and mixlr){ lr lnts iilld t'ortstitnt, turrtovcr tintt,

lt

iroth small and large scale.

G a s/Ii q ui d/s o I i d:re a cto rs 'llhe conver-sion, selectivity and stabilrt-v of catall'zed reactions in fluid-solid reactors can be significantly modified l.r',' the iniluence of physical transport

speed, N, required for lifting the solids in a siurry rector is inversely proportional to the impeller diameter, D, raised to the 0.67-0.85 power. But to obtain a satisfactory degree of hornogcneity, the particles must not only be lifted {r'orn the bottom buL also carried throughou[ the volume of'the vcssel in sufficient quantities. A relevant relationship is:

The minirnum impeller rotational

NDzlde = constant
The stirrer-blade thickness, b, also
has an effect on the suspension of the
2OO2

52

CI]EI\,4iCAL ENGINTERING WWW.CHE

COM JANIJARY

:',.(i \'(.sscl. ]ras successfrillr.

t :l{1ni. g0norall}' carriecl out in a lrecn

' i:r'rAtor heat-transfer

,rrr,ilt,rl into. ibr instancc, tubtrliir, :,, r j-r'olLrntn, -qtatic-mixer, bLrbble, rr n or {luidized-bcd reactors.

';is ilre satisfied through the use

require-

r-(.cvc'le loop-", cooling jackets r':l i hr: ir:ngth of tl"rc reactor tube, ,,i l'ir.r nlc,a.ns. And 'n'arious impellcr -:rn-( irave been used to improve
\.

tie-q, gas, liquid and solid holdups and h1'clroclynamic regimes, have to bc rneasurcd at the larger scale. Arriving at a mathernatical modcl that describes the process reasonably well in the large scale is important for designing large commercial pro-

'.,lirrn vfficiencr,. -,, iltstructive, by supplemcnting , r-1t(,1r,'-r g(It(lral guidclincs, is a -. :1 |;irl11'rrlar issues tliat can arise ' :.,, :ciilc,ults of spccific proccsses =.',tiii;0ns. F-or i:itl arraV of thenr

cessing units. This is feasible only rvith a correct model and good estirnates of the constants. I Edited by Nicholas p. Chopey

Author
f)oblc Illukesh is a proggam lcadcr in the Chcmical Engat the John F. Wclch Technoi og'y Ccntre' ol GFI India 'l'ech-

neering and l\{odcling Gryrup nologl' (lcntrc,

#

, :l,l,.li

in

. ,: r- scrrlc.lrlt r,,ffort.
.'l ir

rrl thoughts . rr('c('ss of any' commcrcial opera' i, ;,,'r'rcl. ,rn rrnderstanding the ef' :i.ri,,irp orr thc process. Unlil re: -. .,'r,t'\' litt.lt attention was paid ,,, ,:ir is an intcrclisciltlinan.sci-

Pvt Ltd. (Sv l52, F,xpnrt I,romoliolr Irttlrrstri;rl I'rrrk I'lr:rsr' 2, Iloodi ViIlrrgr,. \\,hitcfi('ld Roird. Ilangllorc 560066, India; Phonc: +91-80-U412050; cmail: Mukesh.doblc @gcind.ge.com) Previously, he u,orked for l6 in the ICI India R&1'Centrc. His areas of' .r,ears cxpt-.rtisc afe in modeling and simulation,
procc-ss dr:vclopntent,

rt'i'r rnconlpilssos

ginecring, N{ukesh has prrbiisherl ncarlr,g0 tcchrtical ltapcrs, as rvlll as six jourp:rl liticl,-s 61 1l&D rlnnag(-'nl{'lit. irnrl is co-iirrl}rot. ol't.hc lrook. "lIorlr'g,,rr,_'orrs ('atal-r.sis: Nlcclrrrrrisln irn<l In-

catalyiis ancl reaction en-

scveral

'l:, s ol scitncc- irnci engine cring.

ilu(, krnctics anci tl-ri:rrnodl', r)ril"erneter,s are estirnated in

,.

drrstrral Applicntions" (\\'iler' IrrtetrScicncc, !000i. In 1{){.16, lic rcct,ir.od t}tr. Inclian Ir.rstitut,c ol'Chcnrical lingrnccrs' ilcrdillia An,3;11, frrr cxcclL-.ncc

i,,,1'11lon'. rr'hile hJ'drod,l'nantic t:'rr;rs1i,r plrrameters, such as

"

ir,,,-Iint(r distribution. r,cloci-

in basic r.csc:rrch. [ie holds i].J'cch. and Nl. Tech degrces in chenrical enrinccrins from IIT, Madras, and a Ph.D. in that"ficld fr6m thc l-lniversity of A-qton in Birmingham, U.K. He has carricd out post-d-octoral research itt Cambridge Univcrsit.l' in thc U.K., a-s '"vell as aL Tcxas A&-li{ l]nivcrsitr'. Ilc is a ntcnrbcr of AIChE and of the Indirrn Insl ittrtc of Chcnrical Engincr.rs.

For over 8 years, Liqui-Cel@ Membrane Contactors have been used in a variety of installations for COz and Or removal. They have a track record for removing other gasses as well. To date, membrane contactors contintJe to degas more than 300,000 gpm (68,180 mr/hr) of water. They are proven in the field and offer many advantages over conventional technologies. Liqui-Cel Membrane Contactors
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'I

t.l't'Ilc('s
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l"it' '1',"rr.

l4 llrrrio,
1973.

Nl., others. 146{i. 1986.

N,1.,

AI()hll.i.. \/ol. ;)2, No.

ZB,

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'

1ir. (kilrLstein, A.

. Compactp. 1021,

Chrnt. F)ng. Scl., Vol.

having l0X the surface area compared to

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,

16. Nienoq', 1'.'l:-'l)rig,.\irl.9ir.No.2.p

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Cllt-l'/lCAt [:NGINEERING WWW CHE.COM JANUARY 2002 53