Ind. Eng. Chem. Res.

1996, 35, 4559-4565 4559

Hydrodynamics and Mass Transfer in a Liquid-Impelled Loop

Reactor

D. M. R. Mateus, M. M. R. Fonseca, and S. S. Alves*,

Secc a o de Biotecnologia and Secc a o de Feno menos de Transfere ncia, Departamento de Engenharia Qumica,
Instituto Superior Te cnico, 1096-Lisboa-Codex, Portugal

The liquid-impelled loop reactor was studied with respect to hydrodynamics and liquid-liquid
mass transfer. The system involved a continuous aqueous phase, a dispersed organic phase
(n-dodecane), and sometimes a solid phase (gel beads). Indole was the transferred solute. Drop
size, dispersed phase holdup, and continuous phase circulation rate were measured. Experi-
mental overall volumetric mass transfer coefficients of indole were taken from an earlier paper.
In the absence of gel phase or up to about 10% gel concentration, circulation and holdup could
be reasonably well predicted from standard expressions for pressure balance and single-phase
friction pressure loss. This was best achieved by a widely used correlation proposed by
Richardson and Zaki. Use of the Zuber and Findlay two-phase drift-flux model was also
successful, with an adjusted parameter. Experimental mass transfer coefficients were compared
with calculations from existing correlations. The best agreement was obtained with correlations
for circulating drops, as expected by the range of drop Reynolds numbers covered in the
experiments.

1. Introduction n-dodecane and water. In neither of these studies was

The liquid-impelled loop reactor, or LLR, is a rela-
tively novel type of bioreactor (Tramper et al., 1987),
analogous to the airlift in its hydrodynamics; the main
difference is that continuous liquid phase circulation,
rather than being driven by air dispersed in the riser,
is driven by a second immiscible liquid phase with a
different density (Figure 1). This kind of reactor may
be advantageous if, for some reason, a second liquid
phase is necessary or convenient in the bioreactor, e.g.,
when one of the reagents or products has low solubility
in the aqueous phase, where the reaction takes place.
Another major advantage over stirred reactors is the
avoidance of high-shear regions. Examples of applica-
tions include the bioconversion of benzene to cis-
benzenoglycol (van den Tweel et al., 1987), the produc-
comparison between experimental data and available
correlations attempted.
In this work mass transfer is linked with hydrody-
namics to see how well available correlations perform
in predicting measured overall volumetric mass transfer
coefficients.
2. Theory and Modelling
Drop Size. The mechanism of drop formation at an
orifice depends on the regime (Clift et al., 1978). At low
flow rates, there is individual drop formation, whereas
at high flow rates, a jet is formed and drops break up
from this jet. The single-drop regime occurs if (Meister
and Scheele, 1969)

[ ( DN
)]
tion of antraquinones by plant cell cultures (Buitelaar 1/2

et al., 1990), the growing of bacteria in tetralin (Vermue vN e 1.73 1- (1)
FdDN d
and Tramper, 1990), and the biosynthesis of L-tryp-
tophan from indole and L-serine (Mateus, 1994). where vN is the average dispersed phase velocity through
Hydrodynamics of the LLR has, to the authors the orifice, d is the drop diameter as calculated for the
knowledge, been studied only by van Sonsbeek et al. single-drop regime, is the interfacial tension, Fd is the
(1990), who modeled it using the Zuber and Findlay two- density of the dispersed phase, and DN is the orifice
phase drift-flux model and a friction coefficient derived diameter.
from one-phase flow theory. The effect of adding a third To estimate drop size in the jet regime, Scheele and
solid phase, important when an immobilized biocatalyst Meister (1968) proposed
is at play, was not studied. Large solid phase holdups
may be necessary in this case to achieve the required d ) (1.5m)1/3DN2/3 (2)
productivity (Mateus et al., 1996).
Liquid-liquid mass transfer in the LLR was inves- where m is the wavelength of the growing disturbance
tigated by van Sonsbeek et al. (1992) and by Mateus et of the jet surface (Meister and Scheele, 1967). In the
al. (1996). The former determined overall oxygen single-drop regime, the following correlation has been
transfer coefficients between tap water and a dispersed proposed (Scheele and Meister, 1968)
phase consisting of an oxygen-enriched perfluorochemi-

[
cal, FC40. A steady state method was used. Mateus
DN 20QDN 4FdQvN
et al. (1996) used a dynamic method to measure overall vd ) F
gF 3gF
+ 2 - +
volumetric mass transfer coefficients of indole between d gF

( Q2DN2Fd
)]
1/3
* To whom correspondence should be addressed. Telephone, 4.5 (3)
+351-1-8417188; Fax, +351-1-8499242. (gF)2
Secc
ao de Biotecnologia.
Secc
ao de Fenomenos de Transferencia. vd is the drop volume after break off, F is the Harkins-
S0888-5885(96)00225-4 CCC: $12.00 1996 American Chemical Society
4560 Ind. Eng. Chem. Res., Vol. 35, No. 12, 1996

Figure 1. Liquid-impelled loop reactor: (a) safety valve, (b) and (c) sampling valves, (d) riser, (e) downcomer, (f) organic phase reservoir,
(g) discharge valve, (h) perforated plate (1 mm diameter holes), (i) recirculating pump.

Brown correction factor generally presented as a plot
of F vs DN (F/vd)1/3 (Scheele and Meister, 1968), g is the
acceleration of gravity, is the viscosity of the continu-
ous phase, Q is the volumetric flow rate of the dispersed
phase, and F is the density difference between con-
tinuous and dispersed phases. For both nozzle and
multinozzle distributors, Vedaiyan (1969) proposed an
alternative correlation (in cgs units) to obtain the mean
drop size, d
weight between the riser and downcomer liquid columns
Pdf ) FgH (7)
where  is the dispersed phase holdup in the riser, F
is the difference in densities between the continuous and
the dispersed phases, and H is the height of the two-
phase column (approximately the height of the riser).
The various friction losses may be given, as a first
approximation for low holdups of the dispersed phase,

( )
vN by Darcys equation for single-phase pressure loss

d
(4)
2gDN
1/2
)R

( )
Fg Pi ) KiF
ui2
(8)
2
with R ) 1.592, ) -0.0665, and the following restric-
tion for nozzle size where F is the continuous phase density, ui is the
continuous phase velocity in section i, and Ki is a factor
which in general depends on the Reynolds number and
1 1/2 1/2
( )
2 Fg
< DN <
Fg ( ) (5) on the type of fitting. It may be given by

Holdup and Circulation. Circulation results mainly
from a balance between driving force and drag at the
walls
Pdf ) i Pi
where Pdf is the driving force and Pi are the friction
pressure losses in the various reactor sections and
fittings. Driving force is given by the difference in
Leqi
Ki ) fi(Rei) (9)
Rhi
where fi is the Fanning friction factor for straight pipe,
Rei, Rhi, and Leqi are respectively the Reynolds number,
(6) hydraulic radius, and equivalent length of section or
fitting i.
If large holdups and/or a third phase is present, the
situation becomes more complicated, as friction is now
a function also of the holdup and properties of the
dispersed phase(s). Two types of model may then be
 Ind. Eng. Chem. Res., Vol. 35, No. 12, 1996 4561
Table 1. Continuous Phase Mass Transfer Coefficients in Liquid-Liquid Systems
drop condition expression authors
(i) stagnant Shc ) 2.0 + 0.95Rec0.5Scc0.5 Garner and Suckling (1958)
(ii) stagnant
( ) dg1/3 Hughmark (1967)
0.072
Shc ) 2 + 0.463Rec0.484Scc0.339
Dc2/3
(iii) circulating Shc ) -126 + 1.8Rec0.5Scc0.42 Garner, Foord and Tayeban (1959)
(iv) circulating
[ ( ) ]dg1/3 Hughmark (1967)
0.072
0.484 0.339
Shc ) 2 + 0.463Rec Scc F
Dc2/3
with
F ) 0.281 + 1.615K + 3.73K2 - 1.874K3

()( )
c c ur
1/4 1/6
K ) Rec1/8
d g

used to estimate pressure drops (Holland and Bragg,
1995): homogeneous flow models and models for sepa-
rated flow such as the Lockhart and Martinelli model
(Lockhart and Martinelli, 1949). In the present case,
where most of the pressure drop occurs in vertical pipes
with no apparent stratification of phases, simpler
homogeneous flow models are likely to be applicable.
Equations 6-9 relate the continuous phase velocity
to physical properties, geometric and operational vari-
ables, and the holdup of the dispersed phase. This may
be independently related with the slip velocity, us, and
the superficial velocities of the two phases in the riser,
overall mass transfer coefficient, while kd and kc are the
film coefficients for the dispersed and continuous phases,
respectively.
In the general case where both phases control mass
transfer, the dispersed phase coefficient kd depends on
the magnitude of the continuous phase coefficient, kc,
which may be estimated using the empirical correlations
in Table 1.
To calculate the dispersed phase coefficient, kd, for
the general case where both phases control mass
transfer, Jakob (1949) derived the following expression
for stagnant drops

[ ( )]
uc for the continuous and ud for the dispersed, through
the theoretically derivable formula 4Ddt
d
kd ) -
6t
ln 6 Cn exp -n2 (15)
ud uc n)1 d2
us ) (10)
1-
-

where Dd is the solute diffusivity in the dispersed phase
For many two-phase systems, it has been found that and t is the contact time.
the slip velocity is related to the terminal velocity, ut, For circulating drops, Elzinga and Banchero (1959)
by (Richardson and Zaki, 1954) suggested that the correlation proposed by Kronig and
Brink (1950) for the case in which mass transfer is
us ) ut(1 - )n-1 (11) controlled in the dispersed phase alone be adapted to
the general situation where both phases control. The
where n is an empirical quantity, found to be around 2 Kronig and Brink equation is as follows

for Re > 500.
An alternative is the two-phase drift-flux theory of
Zuber and Findlay (1965), who proposed the following
expression
ub ) c0(uc + ud) + ut
where c0 may be taken as an empirically adjustable
parameter and ub is the drop rise velocity. An ap-
proximate relationship between ub and the slip velocity
has been proposed by Ayazi Shamlou et al. (1994)
ub ) us(1 - )
Equations 6-10 may be solved together with either
eq 11 or eqs 12 and 13 to give both the velocity of the
continuous phase, uc, and the holdup, , for any given
value of the dispersed phase flow rate, as long as the
drop terminal velocity is known. This may be calculated
using, for example, the graphical correlation given by
Hu and Kintner (1955).
Mass Transfer Coefficient. The overall mass trans-
fer coefficient is given in terms of the partial mass
transfer coefficients of the two phases by
1 1 m
K d kd kc
) +
where m is the equilibrium coefficient and Kd is the
[ ( )]
d 3 t
kd ) -
6t
ln Bn2 exp -64nDd
8n)1
(16)
d2
Coefficients Bn, Cn, n, and n in eqs 15 and 16 are given,
(12) for the general situation where both phases control, in
Elzinga and Banchero (1959) as a function of kc.
The referred equations for film coefficients have been
deduced for clean systems. Impurities, and particularly
tensioactive substances, may significantly increase or
decrease the overall mass transfer kinetics. The phe-
nomena involved are complex, and to date, there is no
(13) general treatment of the problem.
3. Experimental Section
Reactor. The liquid-impelled loop reactor (LLR) is
shown in Figure 1. It consists basically of two glass
pipes (riser and downcomer) connected at the top and
bottom. It is operated in a way similar to an airlift
reactor, except that the dispersed phase is a liquid
instead of a gas. In the present case, an organic solvent
(n-dodecane), with density lower than water, is continu-
ously dispersed into the aqueous phase through the
perforated plate at the bottom of the riser. The dis-
persed organic phase coalesces at the top of the reactor
(14)
and is recirculated. A sheet of polyurethane foam at
the disengagement section of the LLR helps coalescence
and avoids the formation of emulsions (Fonseca et al.,
4562 Ind. Eng. Chem. Res., Vol. 35, No. 12, 1996
Table 2. Physical Properties of the Two Liquid Phases
Mutually Saturated with Indole at 37 C
interfacial tension
density viscosity
(mN m- 1)
(kg m- 3) (kg m- 1 s- 1)
n-dodecane 735 0.00163 44a
phosphate buffer 1006 0.00075
(0.1 M, pH 8.0)
a Between 0 and 4 s. b For t f .
1994). The density difference between the riser and
downcomer induces the desired circulation of the con-
tinuous phase, which may include a solid third phase.
More details of the LLR and its operation can be found
in Mateus et al. (1994).
Physical Properties. Measured physical properties
of the two liquids relevant to this work are presented
in Table 2. The liquids were mutually saturated by
mixing and settling, prior to measurement. Viscosities
were determined with a Schott-Gerate micro-Ostwald
viscometer, densities were obtained using a pycnometer,
and interfacial tension was measured by the Harkins-
Brown drop volume technique.
Drop Size. Drop diameters were measured using the
photographic method. To avoid lens effect, photos were
taken through a water-filled transparent cubic chamber
with an engraved scale, which enveloped a section of
the riser. Sauter mean diameters were calculated from
3-4 photos for each experimental condition, each photo
containing 100-200 drop images, depending on operat-
ing conditions. The dispersed phase was dyed with red
oil to improve contrast. This dye is appropriate, since
it has a minimal effect on interfacial tension (Hu and
Kintner, 1955), as was experimentally confirmed.
Holdup and Circulation. To determine the con-
tinuous phase velocity, a flow-follower technique was
used. The time a colored gel bead takes to cover a fixed
distance in the downcomer was measured. This mea-
surement was repeated at least 15 times to take into
account any deviation from a flat velocity profile. The
continuous phase velocity was taken as the difference
between the average bead velocity and the experimental
bead terminal velocity.
Holdup was determined by an unconventional tracer
injection technique, as follows. At some point in time,
the dispersed phase is suddenly dyed. From the time
the dyed front takes to reach the top of the riser, the
known dispersed phase flow rate, and the riser volume,
the holdup can be easily calculated, as long as plug flow
is assumed. A similar pulse experiment was enough to
show that the effect of axial dispersion was indeed
negligible for this determination.
4. Results and Discussion
Drop Size and Terminal Velocity. Both visual
observation and the threshold estimated by eq 1 indi-
cated that the prevailing regime was single drop.
Figure 2 compares the prediction of drop size using eqs
3 and 4 with experimental measurements. The result
is reasonable without parameter adjustment. Adjust-
ment of parameters in Vedaiyans equation, (eq 4), gives
R ) 1.753 and ) -0.0787 and very good agreement
with experiment. Thus, for the remainder of the work,
where experimental measurement of drop size was not
carried out, Vedaiyans equation with adjusted param-
eters was used instead.
Figure 3 presents the terminal rise velocity of n-
dodecane drops in 0.1 M phosphate buffer, pH 8.0,
38b
Figure 2. Drop diameter as a function of flow rate of the dispersed
phase: 9 experimental values; s predicted drop diameter using
Scheele and Meister eq 3 for the single-drop regime; - predicted
drop diameter using Scheele and Meister eq 2 for the jet regime;
0 predicted drop diameter using Vedayian eq 4 without adjusted
parameters; - - - predicted drop diameter using Vedayian eq 4 with
adjusted parameters.
Figure 3. Terminal rise velocity of n-dodecane drops in phosphate
buffer (mutually saturated in indole), given by the Hu and Kintner
correlation (1955).
mutually saturated in indole, as a function of drop
diameter using the correlation of Hu and Kintner (1955).
Friction Pressure Loss Calculation. In order that
holdup and circulation rate may be calculated, the
various friction losses must be accounted for (eqs 6, 8,
and 9). Two situations were considered: with and
without a third, solid phase, consisting of gel beads.
Without solid phase, all pressure losses except those
in the riser are single phase. Even for the riser, since
the organic phase holdup never exceeded 6%, pressure
losses could be calculated assuming single phase; two-
phase homogeneous flow calculation gives very similar
results. Six terms are considered in eq 6: two sections
of straight pipe (riser and downcomer), two 90 elbows,
and two cross-sectional changes. Values of Ki for vari-
ous fittings may be found, e.g., in Perry and Chilton
(1973), while straight pipe friction factors for smooth
pipe were obtained using the Blasius equation
0.0781
f) (17)
Re1/4
With the gel phase present, on the other hand, the
situation becomes more complicated. Three phases are
now at play, the continuous aqueous phase and two
dispersed phases, the organic and gel phases. The
organic phase, while being the driving phase due to its
density, has little effect on friction losses owing to its
small holdup. The gel phase, on the other hand, while
not contributing to the circulation driving force, because
its density is that of water, does affect friction losses
due to its large holdup. The contribution of gel holdup
to friction losses is difficult to calculate, because of the
complex reactor geometry; hence, experimental values

Figure 4. Overall friction coefficient as a function of gel holdup
(volume of gel/volume of aqueous phase).
Figure 5. Continuous phase velocity (9 experimental, s model)
and dispersed phase holdup in the riser (0 experimental, s model)
as a function of dispersed phase flow rate. Model predictions were
made using eqs 6-10 plus the Richardson and Zaki eq 11.
Figure 6. Continuous phase velocity (9 experimental) and
dispersed phase holdup in the riser (0 experimental) as a function
of dispersed phase flow rate. Model predictions were made using
eqs 6-10 plus the Zuber and Findlay model eqs 12 and 13: s
model predictions using c0 ) 0.5; - - - model predictions using c0
) 1.
were obtained for an overall K h , on the basis of continu-
ous phase velocity in the riser, defined as (from eqs 6-8)
2FgH
K
h ) (18)
Fucriser2
Figure 4 shows the effect of gel phase holdup on K h.
As expected, the presence of gel beads increases friction,
thus decreasing circulation. Each individual point was
obtained by linear regression of experimental values of
 vs Fucriser2/(2FgH), assuming Kh to be approximately
constant for the range of organic flow rates used. The
curve in Figure 4 results from fitting the experimental
points.
Holdup and Circulation. Figures 5 and 6 compare
calculated continuous phase velocities and dispersed
Ind. Eng. Chem. Res., Vol. 35, No. 12, 1996 4563
Figure 7. Experimental vs calculated volumetric mass transfer
coefficients as a function of dispersed phase flow rate. 9 experi-
mental; - kd from eq 15, kc from eq i in Table 1; s kd from eq
15, kc from eq ii in Table 1; kd from eq 16, kc from eq iii in Table
1; - - - kd from eq 16, kc from eq iv in Table 1.
phase holdups with experimental values, for low gel
loads. The use of the two-phase drift-flux model of
Zuber and Findlay (1965), eqs 12 and 13, together with
eqs 6-10 only gives acceptable results for low values of
the adjusted parameter, i.e., c0 ) 0.5 (Figure 5). This
parameter has to do with the continuous phase velocity
profile: it is shown to be equal to 1 for a flat velocity
profile and increases as the velocity profile approaches
a parabola, in which case c0 ) 1.6. However, in the
literature, c0 has taken values as high as 5.0 or as low
as 0.7, being considered more an empirically adjustable
parameter than a theoretical one (Ayazi Shamlou et al.,
1994).
Good agreement, on the other hand, without any
adjusted parameter is found when the slip velocity
required for the solution of eqs 6-10 is calculated using
Richardson and Zaki eq 11, as an alternative to the
Zuber and Findlay model (Figure 6).
Mass Transfer. Figure 7 compares experimental
and calculated overall volumetric liquid-liquid mass
transfer coefficients, Kda, referred to the dispersed
phase, a being the interfacial specific area. Experimen-
tal values are from Mateus et al. (1996), obtained in the
absence of gel phase.
Calculated values were obtained using eq 4 with
adjusted parameters for drop size calculation and eqs
6-11 for hydrodynamics calculations ( and uc). Specific
area a was calculated assuming spherical drops, hence

a)6 (19)
d
The slope of the equilibrium curve, m, required in eq
14 for the calculation of the overall mass transfer
coefficient, kd, was taken as an average from experi-
mental equilibrium data in Mateus et al. (1996). The
dispersed phase film coefficient, kd, was calculated for
two different situations, rigid drops and circulating
drops, using eqs 15 and 16, respectively. The continu-
ous phase film coefficient, kc, was also calculated for
rigid and circulating drops, using two expressions for
each regime (equations in Table 2).
Comparison between calculated and experimental
overall mass transfer coefficients (Figure 7) shows that
rigid drop correlations give values somewhat lower than
experimental, as would be expected, since drop Reynolds
numbers were in the range 120-200, for which circula-
tion usually occurs inside drops. The best agreement
between calculation and experiment was obtained as-
suming circulating drops, using eq 16 for the determi-
4564 Ind. Eng. Chem. Res., Vol. 35, No. 12, 1996
nation of kd and Hughmarks correlation (eq iv in Table
2) for kc. The correlation of Garner et al. (1959) for kc
in the circulating regime (eq iii in Table 2), on the other
hand, gives much too high estimates, reflecting the
difference in predicted values for the same situation
from available correlations in the literature and the
difficulty of a priori choice of appropriate liquid-liquid
mass transfer correlations.
5. Conclusions
Hydrodynamics and liquid-liquid mass transfer in a
liquid-impelled loop reactor can be described by a model
which integrates expressions and correlations available
in the literature. For low holdups of the dispersed
phase, and in the absence of a third phase, holdup and
circulation can be calculated from standard expressions
for pressure balance and single-phase friction pressure
losses, together with some way of calculating the slip
velocity between the two phases. This is best done by
a widely used correlation proposed by Richardson and
Zaki (1954). The Zuber and Findlay two-phase drift-
flux model can also be used, with an adjusted param-
eter. The presence of a third, solid phase may be
accounted for using an empirical correction to the
friction factor. Mass transfer is well described using
eq 16 for the determination of kd and Hughmarks
correlation (eq iv in Table 2) for kc.
In brief, this integrated model predicts the mass
transfer behavior in the LLR solely from knowledge of
the geometry, physicochemical properties of the system,
and operating conditions (dispersed phase flow rate and
gel load). It thus opens possibilities for optimization of
reactor design and operation.
Acknowledgment
The authors thank Teresa Reis for help with inter-
facial tension measurements. The fellowship awarded
to D.M.R.M. by the CIENCIA/PRAXIS XXI programme
(B.D. 2827) is also gratefully acknowledged.
Nomenclature
a ) interfacial specific area, m-1
Bn ) coefficients in eq 16
c0 ) parameter in eq 12
Cn ) coefficients in eq 15
d ) drop diameter, m
Dd ) solute diffusivity in the dispersed phase, m2 s-1
DN ) orifice diameter, m
f ) Fanning friction factor for straight pipe
g ) acceleration of gravity, m s-2
H ) height of the two-phase column, m
K
h ) total number of velocity heads lost by friction based
on continuous phase velocity in the riser
kc ) mass transfer film coefficient for the continuous phase,
m s-1
kd ) mass transfer film coefficient for the dispersed phase,
m s-1
Kd ) overall mass transfer coefficient for the dispersed
phase, m s-1
Ki ) number of velocity heads lost by friction in section or
fitting i
Kda ) overall volumetric oxygen transfer coefficient, s-1
Leqi ) equivalent length of section or fitting i, m
m ) equilibrium coefficient
Pdf ) pressure driving force for circulation
Pi ) friction pressure losses in section or fitting i, N m-2
Q ) volumetric flow rate of the dispersed phase, cm s-1
Re ) Reynolds number
Rei ) Reynolds number in section i
Rhi ) hydraulic radius, m
t ) contact time, s
ub ) drop rise velocity, m s-1
uc ) superficial velocity of the continuous phase in the
riser, m s-1
ud ) superficial velocity of the dispersed phase in riser, m
s-1
ui ) superficial velocity of the continuous phase in section
i, m s-1
us ) slip velocity, m s-1
ut ) drop terminal velocity, m s-1
Va ) volume of aqueous phase
vd ) drop volume after break off, m3
vN ) average dispersed phase velocity through the orifice,
m s-1
Vs ) volume of gel phase
R ) parameter in eq 4
) parameter in eq 4
 ) dispersed phase holdup in the riser
m ) wavelength of the growing disturbance of the jet
surface, m
n ) coefficients in eq 16
) viscosity of the continuous phase, kg m-1 s-1
F ) density of the continuous phase, kg m-3
F ) difference in densities between the continuous and
the dispersed phases, kg m-3
Fd ) density of the dispersed phase, kg m-3
) interfacial tension, N m-1
n ) coefficients in eq 15
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Received for review April 16, 1996
Revised manuscript received September 29, 1996
Accepted September 26, 1996X
IE960225B
X
Abstract published in Advance ACS Abstracts, November
1, 1996.