Chemical Engineering Science, Vol. 48, No. 10, pp. 1785-1791, 1993. lXK%2XI!J/93 S6.00 + 0.

00
Printed in Great Brimin. 0 1993 Pngamon Press Ltd

LIQUID MIXING IN A BUBBLE COLUMN UNDER PRESSURE

PETER M. WILKINSON, HERMAN HARINGA and FRANS P. A. STOKMAN

Department of Chemical Engineering,University of Groningen, 9747 AG Groningen, The Netherlands

and

LAURENT L. VAN DIERENDONCK

DSM Research, PO Box 18, 6160 MD Gelccn, The Netherlands

(Received 15 January 1992, accepted for publication 11 November 1992)

Abstrati-The liquid axial-dispersion coefficient and gas hold-up arc measured in a batch-type bubble
column of 0.158 m diameter for the system water-nitrogen at pressures between 0.1 and 1.5 MPa. It is
determined that pressure has a marked influence on gas hold-up (in accordance with the results in previous
articles), whereas for the same conditions the influence of pressure on the liquid axial-dispersion coefficient
is relatively small. Furthermore, it is noted that the influence of pressure on liquid mixing is opposite to
what is predicted by theoretical equations for liquid mixing. On the basis of simple mechanistic arguments,
these discrepancies are explained. Finally, it is also demonstrated that empirical equations based on
atmospheric data can be used (with some adjustment) to estimate the liquid dispersion coefficient at higher
pressures.

INTRODUCTION
The literature on the liquid axial-dispersion coeffi-
&nt for bubble columns is extensive. Especially, for
the air-water system at atmospheric condition, many
measurements have been done, and both theoretical
(Joshi, 1980; Field and Davidson, 1980; Riquarts,
1981; Walter and Blanch, 1983; Kawase and MOO-
Young, 1986) and empirical (Deckwer et al., 1974;
Hikita and Kikukawa, 1974) equations have been
developed to predict the axial-dispersion coefficient.
Measurements showing how these equations and
theories hold for high pressures are, however, very
scarce. This, together with the fact that the value of
the gas density has a significant influence on the gas
hold-up in a bubble column (Idogawa et al., 1987;
Wilkinson and van Dierendonck, 1990; Tarmy et aZ_,
1984), leads to the conclusion that liquid mixing is
also likely to be influenced by gas density (and, thus,
pressure).
The aim of the present study is, therefore, to deter-
mine experimentally the liquid axial-dispersion coef-
ficient (and the gas hold-up) as a function of pressure.
EXPERIMENTAL APPARATUS AND PROCEDURES
For the present study the axial dispersion was de-
termined by injecting approximately 30 ml of a 4 M
NaCl solution at the bottom of a bubble column filled
with deionized water, while subsequently measuring
the change in conductivity at a distance above the
tracer inlet equal to 0.8 times the column height (as
recommended by Deckwer, 1985). In order to inject
this (NaCl) tracer into the bubble column at a high
pressure (up to 1.5 MPa), a small holding vessel was
1785
filled with the tracer, after which the pressure in this
vessel was raised 1.5 MPa in excess of the bubble
column pressure. The tracer was then injected by
opening a magnetic valve that connected the tracer-
holding vessel with the bubble column for maximally
0.3 s. From preliminary experiments, it was deter-
mined that the conductivity cell (which was intro-
duced from the top of the column on a 1 cm diameter
tube) must be. shielded from direct contact with
bubbles, because they cause a significant fluctuation
of the conductivity signal. A small alteration of the
conductivity cell was, therefore, made: underneath the
conductivity cell, a small shield was mounted which
reduced the direct contact between the rising bubbles
and the conductivity cell. The diameter of the (per-
fectly vertically aligned) bubble column was 0.158 m
and the gas-liquid dispersion height was 1.50 m for all
experiments. The alignment of the column was
checked because deviations from vertical alignment
influence the dispersion rate (Tinge and Drinkenburg,
1986). The sparger used for the experiments was a ring
with 37 holes of 2 mm. In addition to determining the
response of the tracer, the gas hold-up was also deter-
mined. For these gas hold-up experiments, the column
was first filled with liquid to a height of 1.5 m, then gas
was introduced and liquid was withdrawn from the
column until a (gas-)liquid height of 1.5 m was re-
gained. The volume of liquid withdrawn from the
bubble column was then used to calculate the gas
hold-up.
INTERPRETATION OF RESULTS WITH
ONEDIMENSIONAL AXIAL-DISPERSION MODEL
Liquid mixing in a bubble column is usually de-
scribed on the basis of the one-dimensional axial
1786 PETER M. WILKINSON et al.

dispersion model: that the slip velocity at high pressures is smaller than
at low pressures is an indication that fewer large
(1) bubbles occur at high pressures and it indicates that
the liquid circulation velocity is not as high as at lOW
Together with the necessary boundary conditions, pressures.
this equation can be solved to predict the response of On the basis of the energy balance method and the
a tracer injection (Siemes and Weis, 1957): assumption that a multiple number of circulation cells
in axial direction occur (of which the dimensions are
c, - cx.r=o 1+2&os ;x
c,,::,
- c,, ,_ 0 =
n=1 ( > proportional to the column diameter), Joshi (1980)
determined that the liquid circulation velocity in
a bubble column can be calculated with
xexp(-$&r). (2)
U, = 1.31 [gD,(U, - ~,Us)]l’~ (U, N 0.23 m/s).

Due to a linear relationship between the tracer con- (3)

centration (C,,) and the conductivity, the conductiv-
ity response signals were used directly to determine
the axial-dispersion coefficient El [by fitting the meas-
ured response to the result of eq. (2) with x = H,].
RESULTS AND DISCUSSION
The values of the axial-dispersion coefficients, cal-
culated by the above-mentioned procedure, are
shown in Fig. 1. For each axial-dispersion experiment,
the gas hold-up was also measured (Fig. 2), and, from
these gas hold-up values, the slip velocity ( Ug/ag) was
calculated (Fig. 3). The value of the gas hold-up shows
a large increase with increasing pressure [in ac-
cordance with the results of Wilkinson and van
Dierendonck (1990)] and, consequently, the slip velo-
city (Fig. 3) is much higher at low than at high pres-
This equation indicates that the liquid circulation
velocity decreases as U, approaches &@Ub.In other
words, when the slip velocity (U&,) approaches the
rise velocity of a single bubble ( Ub = 0.23), as is the
case at high pressures (Fig. 3), this equation predicts
that the liquid circulation velocity decreases. That
liquid circulation patterns occur in bubble columns,
with the liquid flowing upward in the centre and
(because of continuity) downward near the column
wall, is generally assumed to be (in combination with
liquid turbulence) one of the primary causes of liquid
mixing. This assumption is also reflected in Joshi’s
(1980) theoretical equation for liquid mixing that is

q
sures. In spite of this, the liquid axial-dispersion coef-
ficient is higher at high than at low pressures (Fig. 1). kw P(Wm)

In other words, the mixing time (t, N Hz/E,) de- I 0.1

creases (slightly) with increasing pressure. If these
. 0.0
0 1.0
experimental results are, however, compared with . 1.0

theoretical concepts on liquid mixing (that have been

developed over the past decades) then it appears that
these different theories do not provide an explanation
for the experimental results. First of all, it is generally
assumed that the occurrence of a high slip velocity (as
0.0
0.00 o.oa a.10 a.,. 0.10

is especially the case at low pressures) is an indication

“0 (m/s)
of large bubbles (with high rising velocities) and an
upward liquid velocity at the centre of the column Fig. 2. Gas hold-up in water vs (nitrogen) superticial gas
(where the gas hold-up is maximal). In other words, velocity in bubble column for the same conditions as in
Fig. 1

0..
“0
(mle)
=o

0.00 0.06 0.10 0.1s o.to

“0 (m/s)

Fig. 1. One-dimensional liquid axial-dispersion coefficient

in water vs (nitrogen) superficial gas velocity in bubble col- Fig. 3. Slip velocity (U&z,) vs (nitrogen)superficialgas velo-
umn as a function of pressure. city in bubble column (based on the data of Fig. 2).
 Liquid mixing in a bubble column under pressure 1787

based on the idea that the axial-dispersion coefficient

is proportional to the product of the mixing length -:K
(L,) and the liquid circulation velocity [U,, eq. (3)]: --t

L, = 0.330,. (4)
E i: T j( E
Combining eqs (3) with (4) leads to
i ut !
E, = U,L, = 0.43D:‘3 [g(Ue - E,U~)]“~. (5) x+dx
This equation [and many other very similar theoret- c,.,t c,., j
X
ical equations-those of Field and Davidson (1980),
u, i j ui
Kawase and Moo-Young (1986)]-thus predicts that
the axial liquid-dispersion coefficient decreases con-
siderably when U, approaches e, Ub (as is the case for
high pressures). Consequently, eq. (5) not only be-
comes increasingly inaccurate at high pressure, also
the trend predicted by eq. (5) is opposite to the experi-
tracer injection
mental result that El is higher at high pressures than
at low pressures. Furthermore, although other
theories on liquid mixing have been developed in the Fig. 4. Schematic representation of liquid circulation and
mixing in a bubble column.
literature, these too cannot be used to explain the
present experimental results: Myers et al. (1987), for
instance, assume that liquid mixing is mainly a result
change liquid. This contribution is represented by the
of liquid entrainment by large fast rising bubbles. The
exchange factor K, while the dispersion (due to liquid
present results, however, indicate that fewer large
entrainment in bubble wakes and due to turbulence)
bubbles (due to a higher pressure) do not lead to
in both the up and the downward flowing section is
a decrease of the liquid mixing rate. Finally, also
represented by E. A mass balance at position x for the
theories that assume that liquid mixing is mainly
upflowing liquid section is given by
caused by liquid turbulence (Baird and Rice, 1975)
cannot account for the lower liquid mixing rate at
atmospheric pressure: by comparing the motion of
bubbles as observed at high pressures and at atmo-
spheric pressure, it can be clearly seen that turbulence
is of much greater significance at atmospheric pres-
sure (for which the churn turbulent regime prevails) (f-5)
than for the homogeneous bubble flow regime that
which can be rearranged to
occurs at high pressures.

LIQUILI CIRCULATION AND ITS INFLUENCE ON LIQUID

MIXING - WC”. x - Cd,xl. (7)
So far, it has been demonstrated that literature A similar equation is obtained for the downflow sec-
theories on liquid mixing usually account for mixing tion:
on the basis of only one mechanism (either entrain-
ment, turbulence or liquid circulation) and it is argued
that each of these separate mechanisms is expected to
Ad(!?$gx +e(2).
=AdE(!.$gx
become of less significance at high pressures, whereas
experimental results show that liquid mixing rate in- + KS(C.. x - cd.,). (‘3)
creases with increasing pressure. If there is much interaction between the upflowing
In order to establish a possible explanation for the and the downflowing liquid (K = large), it can be
experimentally determined influence of pressure, assumed that the difference in tracer concentration
a simple mechanistic model for the bubble column is C - Cd X will be relatively small. In other words,
developed for which it is assumed that liquid mixing is rlzal co&entration differences will then be small.
a result of dispersion and liquid circulation. In Fig. When this assumption is made in combination with
4 a schematic representation is given of a bubble the assumption that A,, = A, = 0.5zDfj4 = 0.5A,
column in which the liquid is flowing upward in the (and, consequently, S = nDJd2) then eqs (7) and (8)
centre and downward near the wall region. Further- can be simplified considerably by addition of eq. (7) to
more, it is assumed that flow reversal occurs only at eq. (8), together with the fact that C, + C. = 2c:
the top and at the bottom of the bubble column
[which has recently been confirmed by Devanathan et
al. (1990)]. Obviously, due to turbulence the up and
($). =E(gq +&(dcd,dy.
downflowing liquid interacts and will, therefore, ex- (9)
1788 F$TER M. WILKINSON et al.

Then subtracting eq. (7) from eq. (8) and rearranging from eq. (ll)]. In other words, a hi& liquid circula-
leads to tion rate will not contribute to a high overall liquid
mixing rate if this high liquid circulation rate is ac-
companied by significant interaction (high K) be-
tween the up- and down-flowing recirculating liquid.
Figure 5 also shows some calculated tracer response
(10) curves for intermediate values of the exchange factor.
These tracer response curves show [as predicted by
This equation is differentiated with respect to x and eq. (ll)] that the mixing rate increases for higher
(because C,, z C,) it is assumed that all terms on the values of F (or lower K values). Although these results
right-hand side of eq. (IO) containing C,, - C. can be cannot be used quantitatively to explain the differ-
neglected. Combining the result with eq. (9) leads to ences between liquid mixing at high and low pres-
sures, some aspects of the calculations are of interest.
First of all, it seems likely (as argued in the previous
sections) to assume that both the liquid circulation
rate U&l - .s,Jand the dispersion coefficient E due to
(11) turbulence are larger at atmospheric pressure than at
high pressures. The calculations, therefore, indicate
with that the (experimentally determined) higher ouerall
dispersion coefficient (El) at high pressures can only
F=
W%Jz be explained if the exchange factor (K) is higher at low
16(1 - E#)’ KE’
than at high pressures. Such a trend is not unexpected:
Equation (11) is equal to eq. (l), if E(1 + F) is sub- at low pressures many more large (3-5 cm) fast rising
stituted by Et. In other words, eq. (11) indicates that bubbles were seen than at high pressures, while, pre-
the experimental value of Et can be the result of sumably, especially these large bubbles increase the
a combination of dispersion (E) and circulation (term radial interaction of the liquid (thus, increase K), due
F). On the basis of eq. (11) it can be shown that to their size and due to the high liquid turbulence in
a higher liquid circulation rate U,/(i - a#) increases the wakes of such bubbles. It is interesting to note that
the value of F, whereas interaction (K) between the the assumption that large bubbles decrease the ouernll
up-flowing and down-flowing liquid decreases the axial-dispersion coefficient is also confirmed by ex-
contribution of liquid circulation on the mixing rate. periments of Gondo et al. (1973). Gondo et al. deter-
In order to illustrate these influences (Fig. 5), mined a relatively high axial-dispersion coefficient
the tracer response was calculated numerically from when mainly small bubbles occurred (due to the use of
eqs (7) and (8) for different values of F with a porous plate), whereas the axial-dispersion coeffi-
U,/(l - E,) = 0.4 m/s and E = 0.02 m’/s. Figure cient decreased when large bubbles were introduced
5 shows that when there is no exchange between up- in the dispersion through a side-stream. These experi-
and down-flowing liquid (K = 0 or F = co), an oscil- ments [and experiments of Ohki and Inoue (1970),
latory tracer response would result which is obviously and Kato and Nishiwaki (1972)], together with the pres-
not in accordance with the experimental tracer re- ent results, confirm that a more homogeneous disper-
sponse that fitted well with eq. (2). The other extreme sion with fewer large bubbles (either due to a higher
is obtained when the exchange factor is infinite pressure or due to a more effective sparger) leads to an
(K = 00 or F = 0). For this “ideal exchange” case, the
increase of the liquid dispersion coefficient E,.
liquid circulation has no influence on the tracer re- Finally, it is also noted that more (specific) experi-
sponse and mixing rate [this result can also be seen ments are certainly desirable in order to establish the
validity of the proposed model: for instance, by
measuring the response of a tracer (the conductivity
*.o signal) at a number of different radial positions, valu-
lina F able information can be obtained on radial mixing (or

Ha
C&i =x,0 Luwn F “.,“a. ---_ 0 radial liquid interaction). If the present theory is cor-
- 1.‘
0.1
Cx.m -=x.0 rect, such experiments must show slower radial mix-
--1

1.0 #ip . -4 ing at high than at low pressures.

,,,,,.,.,,.,...““‘-_ _ _ - ___---- --- 10
I ,,,,,/.., _--- --m
,/
0.0 ,,...
,,,“,,-
,.” ,*
ESTIMATING E, FOR DESIGN PURPOSE
,./;x Numerous empirical equations for the liquid axial-
.’ ,
J
0.0
0 10 10 00 ‘0 00
dispersion coefficient have been published. In Fig.
time (8) 6 a comparison is shown between the present experi-
mental results and a number of empirical equations
Fig. 5. Dynamic tracerresponsecalculatedfrom eqs (7) and from the literature (Table 1). From this comparison, it
(8) at H = 1.25m after tracer injection (at t = OS and
H = 0 m) in a bubble column (H = 1.5 m and D, = 0.15 m) is seen that especially El at atmospheric pressure is
for different values of F. predicted fairly well by these equations, whereas the
 Liquid mixing in a bubble column under pressure 1789

kru PtMPmI
+ 0.1
. 0.0
0 1.0
. 1.0
. 0.3
. e.* I

OdO ’ 0.00 ’ I
0.00 0.0s 0.10 0.1‘ a*0
0.00 0.0s 0.10 0.16 0.10 0.m

ua (mls) % (m/s)

Fig. 6. The liquid axial-dispersion co&Gent data of Fig. 7. ~~(1 _ Eg) vs the superficial gas velocity as a function
Fig. 1 vs the superficial gas velocity compared to the pre- of pressure for two different column sizes [D&= 0.078 m:
dicted value from different empirical equations (Table 1). data of Holcombe et al. (1983); D, = 0.15 m: calculated from
data of Figs 1 and 21.

Table 1. Empirical equations for predicting E,

EI W/s) Reference

E, = 1.23D’~5U0~” Towell and Ackerman (1972)

E, = 0.68$ f.+ Deckwer er al. (1974)
E, = (0.065’+ 0.%J,0.77)D:.25~;0.12 Hikita and Kikukawa (1974)’
E, = 0.3502’3 U,“Sg”3 Baird and Rice (1975)

‘Recalculated to SI units.

experimental results obtained at high pressures (and
high gas velocities) are underestimated. Consequently,
these equations still require some improvement before
they can be applied at high pressures. It is, however,
also obvious that a large amount of experimental data
is necessary in order to determine such an improved
empirical correlation for the liquid axial-dispersion
coefficient that holds for low as well as high pressures
(and in different liquids). Unfortunately, however, at
present sufficient experimental data on liquid mixing
are available only for atmospheric conditions (and
mostly in air-water systems). The previously pub-
lished literature experimental studies on the liquid
axial-dispersion coefficient at high pressure were usu-
ally confined to extremely low superficial gas
velocities [Ishii and Takeya (1967): U, c 1 mm/s;
Houzelot et al. (1985): U, < 6 mm/s] or to extremely
small column diameters [Sancnimnuan et al. (1984):
D, = 1.9 cm] and are, therefore, of little significance
for reactor design. Furthermore, although Holcombe
et al. (1983) determined the liquid axial-dispersion
coefficient between 0.3 and 0.71 MPa in a 0.078 m
diameter bubble column for gas velocities as high as
0.6 m/s, their results cannot be used for a direct com-
parison with the present results; Holcombe et al.
(1983) used an experimental technique for determin-
ing the axial-dispersion coefficient that leads to the
value of E,(l - zg) instead of El. However, provided
the gas hold-up is known, this experimental value
E,(l - .sg) can be recalculated to the value of E,.
Unfortunately, the gas hold-up could not be deter-
mined for their experimental set-up and, therefore,
they estimated the gas hold-up on the basis of an
empirical gas hold-up equation of Hills (1976). This
equation of Hills does not, however, account for the
influence of pressure on gas hold-up and, conse-
quently, the value of El calculated by Holcombe et al.
is presumably incorrect. However, multiplying this
(incorrect) value of E, by 1 - .sg(from Hills’ equation)
leads to the original experimental value of E,(l - se).
Interestingly, this experimental value of E,(l - EJ
shows virtually no influence of pressure and, there-
fore, the present experimental results were also recal-
culated to E,(l - Ed), as shown in Fig. 7. Figure
7 shows that, although the scatter in our data is larger
than for the Holcombe data, these results also indicate
that the liquid axial-dispersion coefficient is practic-
ally uninfluenced by pressure provided it is based on
the liquid volume (1 - E@). In other words, the above-
mentioned literature empirical equations for pre-
dicting the liquid axial-dispersion coefficient at atmo-
spheric pressure can give a reasonable estimate of El
for low as well as high pressures provided the follow-
ing correction is made:
E, (high pressure) 2: E, (atmospheric pressure)
x E, (atmospheric pressure)
. (13)
E, (high pressure)
Obviously, this equation is still based on a limited
number of experimental results; therefore, more re-
search is certainly desirable in order to determine
whether eq. (13) holds also for liquids other than
water and in larger columns.
1790 PETER M. WILKINSON et al.

CONCLUSIONS Subscripts
-The one-dimensional liquid axial-dispersion co- d downflow
efficient increases slightly with increasing pres- r radial coordinate in bubble column
sure, whereas the gas hold-up increases consider- T total
ably with increasing pressure. u upflow
- 7’heoretical literature equations available for X axial coordinate in bubble column
predicting the axial-dispersion coefficient based
on the energy balance method predict the oppo-
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