Indian Chemical Engineer

ISSN: 0019-4506 (Print) 0975-007X (Online) Journal homepage: http://www.tandfonline.com/loi/tice20

Hydrodynamics of a Pulsed Sieve Plate Extraction

Column

Nitin Somkuwar, Nitin Kolhe & Virendra Rathod

To cite this article: Nitin Somkuwar, Nitin Kolhe & Virendra Rathod (2014) Hydrodynamics
of a Pulsed Sieve Plate Extraction Column, Indian Chemical Engineer, 56:3, 235-257, DOI:
10.1080/00194506.2014.910707

To link to this article: http://dx.doi.org/10.1080/00194506.2014.910707

Published online: 28 May 2014.

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INDIAN CHEMICAL ENGINEER 2014 Indian Institute of Chemical Engineers
Vol. 56 No. 3 September 2014, pp. 235257
Print ISSN: 0019-4506, Online ISSN: 0975-007X, http://dx.doi.org/10.1080/00194506.2014.910707

Hydrodynamics of a Pulsed Sieve Plate Extraction

Column

Nitin Somkuwar, Nitin Kolhe and Virendra Rathod*

Department of Chemical Engineering, Institute of Chemical Technology, N.P. Marg, Matunga,
Mumbai 400019, India

Abstract: Hydrodynamic characteristics, such as drop size, dispersed phase hold-up and
flooding have been studied experimentally in a pulsed sieve plate extraction column of
0.076 m diameter. Geometrical parameters like perforation diameter, plate spacing and
fractional free area (FFA) of sieve plate and operating parameters, such as pulse velocity
and superficial velocities of dispersed and continuous phase, were studied using kerosene-
water system. The drop size was reduced with decrease in perforation diameter, plate
spacing, FFA and pulse velocity. Dispersed phase hold-up was found to be a function of
drop size and superficial velocity of dispersed phase. At pulse velocity of 0.025m/s the
parabolic behaviour with maxima at the transition from mixer-settler to dispersion regime
of flooding curve has been noticed for all the different geometrical conditions. The
maximum mass transfer interface together with utmost throughput was obtained at
perforation diameter of 0.003 m, plate spacing of 0.05m and FFA of 0.2. The optimal
operating parameters were pulse velocity of 0.025 m/s and superficial velocity of 0.006 m/s
using organic to aqueous ratio (O/A) of 1:1. The drop size attained at these conditions was
0.0015 m with dispersed phase hold-up of 18%. The correlations developed can be used for
the prediction of hold-up and drop size.

Keywords: Pulsed sieve plate extraction column, Hydrodynamics, Drop size distribution,
Dispersed phase hold-up, Flooding characteristics.

1. Introduction
Liquidliquid extraction is used for separation processes in different process industries.
Diversified liquid-liquid extraction equipments like mixer-settlers, columns, centrifugal

*Author for Correspondence. Email: vk.rathod@ictmumbai.edu.in

236 S OMKUWAR ET AL .

extractors have been developed as per the process requirement. The search for improved
extraction efficiencies has led to the development of a class of liquid-liquid contactors in which
mechanical agitation is provided to increase the interfacial area between the two liquid phases.
One of these contactors is the pulsed sieve plate extraction column (PSPEC), which requires
external energy input in the form of pulsing motion usually sinusoidal superimposed on
counter-current flow of the liquid phases. This pulsation provides high turbulence which assists
in droplets breackdown. Consequently, the large interfacial area is obtained to get high mass
transfer coefficient. Wiegandt and Von Berg [1] have shown that under pulsing conditions, the
height of a packed column required to achieve the given degree of extraction is reduced by a
factor of three. Since the pneumatic pulsing unit can be placed remote from the actual
processing area, the pulsed columns have a clear advantage over other mechanical contactors,
while processing corrosive or radioactive solutions.
The design of any solvent extraction column necessitates the knowledge of cross-section and
height of the column to achieve the desired separation with given duty. The cross-section is
determined by the hydrodynamic characteristics like drop size, dispersed phase hold-up and the
maximum throughput from flooding curve. The latter requires the information of axial dispersion
and the rate of mass transfer between phases. All these characteristics are mainly dependent on the
drop size of dispersed phase. Extensive work has been done and various correlations are available
in the literature related to these hydrodynamic parameters. However, it is difficult to choose the
one correlation which is precisely fitted amongst the range of correlations. Thus, for design
accuracy, it is crucial to produce the comprehensive experimental data of hydrodynamic
characteristics for the desired system and correlate this with the available empirical correlations.
Hence, this work consists of evaluation of best conditions for the hydrodynamic parameters by
thorough experimental investigation on the basis of various geometrical and operating conditions
and examination of results with numerous available correlations.

2. Previous Work
In PSPEC, the hydrodynamic characteristics like dispersed phase hold-up, flooding, axial
dispersion and ultimately the mass transfer coefficient strongly depend on dispersed phase drop
size. Many investigators have studied the effect of various geometrical and operating conditions
on drop size in PSPEC. Kagan et al. [2], Boyadzhiev and Spassov [3], Lorenz et al. [4] and
Srinivasulu et al. [5] have studied the effect of pulse velocity on drop size and found that, with an
increase in the pulse velocity the drop size decreases along the height of the column. The individual
effect of pulse amplitude (A) and pulse frequency (f) was also observed by Khemongkorn et al. [6].
It was found that the drop size was reduced with increase in A and f. The influence of other
operating parameters like continuous and dispersed phase flow rates on drop size have been
examined by Boyadzhiev and Spassov [3], and Srinivasulu et al. [5]. Negligible effects of both the
continuous and dispersed phase flow rates have been observed in their study. Kagan et al. [2] have
observed that the phase ratio has no effect on drop size. Khemongkorn et al. [6] have also found
insignificant effect of dispersed phase superficial velocity on drop size.
The geometrical conditions have also a considerable effect on drop size in PSPEC. Misek
[7], Khemongkorn et al. [6], and Boyadzhiev and Spassov [3] have focused on perforation
diameter of sieve plate and revealed that perforation diameter influencing more on drop size
INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014
 Hydrodynamics of a Pulsed Sieve Plate Extraction Column 237

as compared to plate spacing and fractional free area (FFA). The effect of plate spacing and
FFA was observed by Miyauchi and Oya [8] and Srinivasulu et al. [5] and found that the drop
size increases notably with FFA than that of other geometrical parameters. Khemongkorn
et al. [6] and Kleczek et al. [9] have focused on the effect of mass transfer direction and
proposed correlations for drop size prediction. It was observed that the drop size obtained
was smaller for mass transfer direction from dispersed to continuous phase than that from
continuous to dispersed phase. Usman et al. [10] also reported that pulse velocity have more
influence on drop size distribution. However, the uniform drop size distribution was found in
the top portion of the column.
Dispersed phase hold-up is also one of the important parameters of column from design
point of view. Hold-up is a measured quantity of dispersed phase that contacted with the
continuous phase during the counter-current flow. Larger hold-up helps to achieve the greater
efficiency of the column, and together with the drop size it gives maximum interfacial area for
the mass transfer. Sehmel and Babb [11], Pietzsch and Blass [12], and Venkatnarsaiah and
Verma [13] have studied the effect of pulse velocity extensively and revealed that at low pulse
velocity the larger drops accumulate beneath the sieve plate in the mixer-settler regime and
hold-up obtained is higher. With increase in pulse velocity in this regime the hold-up
decreases and obtained minimum value at transition pulse velocity. Further increase in pulse
velocity results in increase in hold-up. Cohen and Beyer [14], and Lorenz et al. [4] have also
observed that, the dispersed phase hold-up increases with increase in pulse velocity. Cohen
and Beyer [14], Sehmel and Babb [11], and Khemongkorn et al. [6] also found an increment in
hold-up values with increase in A and f separately.
Miyauchi and Oya [8], Mishra and Dutta [15], Lorenz et al. [4], and Venkatnarsaiah and
Verma [13] studied scrupulously the effect of geometrical conditions of PSPEC on dispersed
phase hold-up. In this study, it was observed that increase in plate spacing, perforation diameter
and FFA results in reduction of shear forces acting on droplets. Hence, the drop size obtained
was greater, and ultimately, due to high slip velocity of large size drops, the hold-up was
reduced. Kumar and Hartland [16] also studied the physical properties of 14 different liquid
liquid systems, along with the operating and geometrical properties of the systems. This study
showed that column diameter has insignificant effect on the hold-up and perforation diameter
shows its effect only in the mixer-settler regime of operation. Hold-up is independent of column
diameter over the range of 0.0250.213 m. Most of the investigators also concluded that, the
effect of plate spacing and FFA has greater effect on the slip velocity rather than perforation
diameter, while calculating the hold-up and proposed the correlation for slip velocity. The
influence of continuous and dispersed phase superficial velocity on hold-up was investigated by
Cohen and Beyer [14], Sehmel and Babb [11], Miyauchi and Oya [8], Mishra and Dutta [15],
Bell and Babb [17], Lorenz et al. [4], and Venkatnarsaiah and Verma [13]. Prominent effect of
dispersed phase superficial velocity on hold-up as compared to all other geometrical and
operating conditions has been observed in each work. On the other hand, the consequence of
continuous phase superficial velocity on hold-up was negligible. Khemongkorn et al. [6] have
also studied the effect of mass transfer direction on hold-up. At low pulse velocity the mass
transfer influence was nil and the hold-up obtained was of same order as in case of no mass
transfer. Miyauchi and Oya [8] have proposed the separate empirical correlation for hold-up
considering mass transfer.
INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014
238 S OMKUWAR ET AL .

Thornton [18] considered the behaviour of pulsed column under high pulsations like spray
column. The slip velocity (Vslip) relation was differentiated to obtain the flooding capacity with
respect to continuous and dispersed phase velocities. A correlation for predicting the
characteristic velocity (Vo) was developed using experimental data obtained on five liquid
liquid systems. Kagan et al. [2], Berger and Walker [19] and Lorenz et al. [4] have studied the
effect of operating parameters, that is, pulse velocity and phase ratio on throughput in PSPEC.
It was observed that, in mixer-settler regime, as pulse velocity increases capacity of the column
increases and flooding occurs at higher flow rates. Once the column reaches its maximum
capacity, further increase in pulse velocity resulted in decrease in its capacity. Thus, the well-
known parabolic behaviour with maxima at the transition from mixer-settler to dispersion
regime has been noticed. In the same study, the individual effect of A and f have also been
examined. As there was no significant effect of A and f separately, the product Af has been
suggested to study the flooding behaviour. Kagan et al. [2], and Berger and Walker [19]
studied the effect of phase flow ratio (Vd/Vc) on throughput. It was found that increase in
dispersed phase flow rate increases the resistance to the flow of continuous phase through the
column cross-section which causes flooding of column at greater phase ratio of Vd/Vc. Hence,
with increase in phase flow ratio, the column capacity reduces. The effect of plate spacing was
focused by Tribess and Brunello [20]. Increase in plate spacing resulted in reduction of the
frequency of shear force application on droplets. Hence, an increase in mean drop diameter was
observed, with greater rising velocity. Thus, the throughput was increased with plate spacing.
They have also studied the effect of mass transfer from dispersed to continuous phase on the
flooding behaviour of PSPEC for the system tolueneacetonewater. In the presence of mass
transfer, the maximum flow rate was achieved without flooding. Thus, flooding in the column
was delayed. Yadav and Patwardhan [21] have scrutinized the information available in
literature, gathered the experimental data from previous work and checked the fitting of
various correlations reported in literature for drop size, hold-up and flooding.
Taking into consideration the comprehensive previous work it was noticed that extensive
experimental study with all geometrical and operating conditions have to be accomplished for
all hydrodynamic characteristics like drop size, dispersed phase hold-up and flooding. Sauter
mean diameter decides the value of other hydrodynamic properties like hold-up, throughput,
axial dispersion and eventually mass transfer coefficient. So, it was crucial to study drop size and
drop size distribution scrupulously. Altogether, to achieve greater efficiency with high capacity,
it was necessary to study the drop size, hold-up and flooding characteristics thoroughly.
Consequently, the objectives of the present work were the systematic study of all hydrodynamic
characteristics at different geometrical and operating parameters and development of the
correlations based on the results for design of PSPEC.

3. Experimental
3.1. Experimental Setup
Fig. 1 shows the schematic of PSPEC. The glass column consists of 0.076 m internal diameter
and 1.05 m length. Material of construction used for plate cartridge was SS-316. Thickness of
the sieve plates was 0.0016 m. To study the consequence of perforation size, two different
perforation diameters of 0.0015 m and 0.003 m with triangular pitch were used. To determine
INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014
 Hydrodynamics of a Pulsed Sieve Plate Extraction Column 239

Fig. 1. Schematic of experimental set up of pulsed sieve plate extraction column. 1. Column shell
(Diameter = 0.076 m, Length = 1 m), 2. Plate cartridge, 3. Liquid disengaging section, 4.
Liquid distributor for aqueous phase inlet, 5. Liquid distributor for organic phase inlet, 6.
Glass Square box lled with continuous phase, 7. Organic phase outlet, 8. Aqueous phase
outlet, 9. Pulse leg, 10. Rota meter, 11. Ball valves, 12. Centrifugal pump, 13. Storage tank, 14.
Solenoid valve, 15. Electronic timer, 16. Pressure regulator, 17. Compressor, 18. Jack leg.

the effect of plate spacing, the sieve plates were stacked at a distance of 0.05 m and 0.1 m. Two
different types of sieve plates of FFA of 0.2 and 0.3 were employed separately. To achieve the
complete phase separation the glass disengaging sections of 0.15 m diameter and 0.2 m length
were fitted at the top and bottom ends of PSPEC. The perforated liquid distributors were

INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014

240 S OMKUWAR ET AL .

provided to feed continuous and dispersed phases in the column. The superficial velocities of
continuous and dispersed phase were varied with the help of rotameters. Jackleg was used to
control the constant level of phase interface at the top of the column. The pneumatic pulsation
was provided to the liquid pool in the column. A pulse leg of 0.05 m diameter and 1.8 m
length was fitted to the bottom disengaging section. The desired magnitude of pulsation was
obtained by controlling compressed air flow rate with pressure regulating valve. Solenoid
valve (3/2 way) was used for constant interruption of air flow rate. The pulse frequency was
varied by on/off control electronic timer. The square boxes were provided outside the column
at three different heights (top, middle and bottom) and filled with water to eliminate the
curvature effect of glass column to get an accurate drop size of dispersed phase in the column
by photographic method. The inlet and outlet flow rates of both the phases were controlled
by using ball valves.

3.2. Experimental Procedure

The PSPEC was initially filled with water. The pneumatic pulsation was started and the pulse
amplitude was varied by compressed air flow control. The amplitude was adjusted by
measuring the water level displacement in the pulse leg with the help of scale. The desired
pulse frequency was achieved by solenoid valve. The water and kerosene flow was started
through the respective liquid distributors. The superficial velocities of continuous aqueous
phase (water) and dispersed organic phase (kerosene) in the column were adjusted for
different set of operating conditions. The liquid interface was maintained steady for each
experimental run.

3.2.1. Drop Size Measurement Method

Photographic technique was used to measure the drop size in the active length of the column.
The drop size was measured by taking photographs at three different sections starting from
bottom, middle and top as explained in the experimental setup. The bottom section consisted
of the first three plates, middle section from 10th to 12th plates and top section from 17th to
19th plates from the bottom. To eliminate the distortions caused by the curvature of the
column, the cross-section of the column under consideration was surrounded by a rectangular
box of acrylic sheets and filled with the continuous phase liquid. A number of videos were
taken from these three sections of the vertical column. Camera used in the measurement of
drop size was Canon SX20 IS. Most of the photographs were taken on apparature value (AV)
programme with SM (super micro) mode by adjusting the micro-scale approximately 0.05 m
with respect to distance between the lens and focus the object. The shutter speed was adjusted
at 2500 to 3000 and frames at f/7.5 to f/8. The videos were converted into approximately 500
images in to the convertor (magic video and K-Multimedia Player) and finally by making the
PDF of these images analysis of drop size was done.

3.2.2. Dispersed Phase Hold-up Measurement Method

Integral dispersed phase hold-up over the entire length of the column was measured by the
displacement method. This involves measurement of interface level at the top of the column
during the operation. Subsequently, the operation of the column was interrupted by closing
INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014
 Hydrodynamics of a Pulsed Sieve Plate Extraction Column 241

all inlets and outlets. After complete collection of the dispersed phase from the top of the
column, the level of the separation layer was measured again. The volume of the dispersed
phase, which was present over the entire active length of the column during operation, was
determined from the difference between the levels at the interface.

3.2.3. Flooding Measurement Method

The superficial velocities of both the phases were adjusted with the help of rotameters. The
pulse velocity was increased from the minimum value. Flooding was observed at different
pulse velocities.

4. Results and Discussion

4.1. Drop Size
In PSPEC, the Sauter mean diameter and drop size distribution influence the terminal rise
velocity of drop, dispersed phase hold-up, the residence time of the dispersed phase, axial
dispersion and throughputs. Moreover, the interfacial area available for mass transfer
depends on drop size and the corresponding dispersed hold-up and plays a very important
role in continuous and dispersed phase mass transfer coefficient. Hence, the knowledge of
drop size and drop size distribution has prime importance in a design of column. In a PSPEC,
drop size and drop size distribution depend basically upon the drop breakage and drop
coalescence. The breakage of drop was obtained enormously by agitation produced by the
pulsing motion (up stroke and down stroke) of liquid pool in the column, which causes the
jetting of the dispersed phase drops through the perforation of horizontal plates and hitting
on the wall of sieve plates and the column shell. The drop size depends on the geometrical
conditions like perforation diameter, FFA and plate spacing as well as operating parameters,
such as pulse velocity and superficial velocities of continuous and dispersed phase. The effect
of these parameters have been studied comprehensively and discussed herein.

4.1.1. Effect of Phase Reversal on Drop Size

Phase reversal gives rise to bigger drop size as compared to the aqueous phase as the
continuous phase. From Fig. 2, it could be seen that at the same geometrical conditions and
same set of operating parameters, when the aqueous phase was dispersed phase the drop size
obtained was relatively very high because of plate wetability characteristic. From visual
observations also it was noticed that, the aqueous phase drop coalescence takes place to form
a bigger drop. So, the phase reversal gives less interfacial area for mass transfer compared to
organic phase as dispersed phase. Therefore, for whole study, organic phase was used as the
dispersed one.

4.1.2. Effect of Pulse Velocity on Drop Size

Fig. 3, shows the Sauter mean diameter as the function of pulse velocity. The effect of pulse
velocity (Af) on Sauter mean drop diameter was studied with different geometrical conditions
at constant continuous and dispersed phase superficial velocities. In this study, three flow
regimes have been observed depending on the intensity of pulse velocity at constant phase flow
INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014
242 S OMKUWAR ET AL .

Fig. 2. Effect of phase reversal on the drop size.

rates. At low pulse velocity range of 0.0080.015 m/s, mixer-settler regime was observed. At the
end of the each pulse cycle, the separation of light and heavy phases into two distinct layers on
each plate of the column have been observed and performed as a series of mixers and settlers.
At every pulse cycle, the drop formation of the light kerosene phase during upstroke and the
drop coalescence during down stroke took place. In this regime the distribution of drop swarm

Fig. 3. Effect of pulse velocity on Sauter mean drop diameter.

INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014

 Hydrodynamics of a Pulsed Sieve Plate Extraction Column 243

was also sluggish, which was also reported by Lorenz et al. [4]. At low pulse velocity, the shear
force applied on the drops was also low. All these aspects resulted in formation of relatively
large drop size in this low range of pulse velocity.
In the pulse velocity range of 0.0150.03 m/s, the dispersion regime was observed. The
agitation intensity was found to be increased with the pulse velocity in the column. Similarly,
the shear force applied on the dispersed phase drops, while pushing through the perforations
of the plates, was enhanced. Also, there was much less possibility of coalescence of dispersed
phase drops in this regime due to high turbulence. Because of above pulse velocity of 0.03 m/s
due to very high energy input, the related shear forces on drops were excessive. Also, the drop
breakage occurred intensely due to collision of drops on the wall of sieve plates and the
column. At high pulse velocity, the greater oscillatory Reynolds number prevents hindrance
of drops beneath the sieve plate of the column. The entire dispersed phase drops were seen to
spread throughout the active length of the column. The smallest drop size of 0.001 m was
obtained with smooth working of column in this emulsion regime. This observation was in
agreement with Srininivasulu et al. [5], Khemongkorn et al. [6], Luo et al. [22] and Prabhakar
et al. [23].

4.1.3. Effect of Geometrical Parameters on Drop Size

From Fig. 3, it has been also observed that, along with pulse velocity the plate geometry like
perforation diameter and plate spacing also have considerable effect on Sauter mean drop
diameter. The substantial decrease in the drop size was found with 0.0015 m perforation size
as compared to 0.003 m. However, with increase in pulse velocity in both cases the drop size
difference was reduced and with the pulse velocity of 0.025 m/s and onwards there was little
change in the drop size at both perforation diameters. It has been revealed that, the resistance
offered by smaller orifice was relatively greater in case of 0.0015 m perforation diameter
plate. Hence, the drop size was smaller that is, 0.0019 m as compared to 0.0027 m at
perforation diameter 0.003 m at low pulse velocity. However, an influence of pulse velocity
on drop size was high relative to perforation diameter. Consequently, the drop sizes beyond
the pulse velocity of 0.025 m/s for all perforation diameter plates were in close proximity.
Lorenz et al. [4] have found that the constant drop size was achieved sooner at a smaller
perforation diameter. Khemongkorn et al. [6] have observed smaller drops with decrease in
the perforation diameter because of increase in shear forces on drops. Misek [7] has also
proposed that the Sauter mean drop diameter was proportional to perforation diameter, d0.4.
Whereas in industrial operations the pulsed columns can be operated smoothly up to 0.025 m/s
pulse velocity. Hence, from maintenance point of view, as well as to avoid chances of blockage
of 0.0015 m perforation diameter sieve plate, the 0.003 m perforation diameter has been
recommended.
At constant pulse velocity, the plate spacing also plays an important role in deciding the
drop size in PSPEC. From Fig. 3, it was observed that at the plate spacing of 0.05 m the Sauter
mean drop diameter was slightly smaller than that of 0.1 m. There was no significant effect on
the drop size for the pulse velocity in the range of 0.0080.035 m/s. So, plate spacing has also a
slight effect on Sauter mean diameter as compared to perforation diameter. Miyauchi and Oya
[8] have reported the same results that the drop size increases with the plate spacing. Also,
INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014
244 S OMKUWAR ET AL .

Srinivasulu et al. [5] has proposed in their correlation for drop size that the Sauter mean drop
diameter is proportional to plate spacing, h0.34.

4.1.4. Drop Size as a Function of Column Height

Drop size was measured at three different cross-sections along the axis of PSPEC as shown in
the schematic representation of PSPEC in Fig. 1. Maximum break-up of drops occurred at
the first two to three plates from the bottom of the column, as the organic light phase layer
spread beneath these plates and then jetted through the orifices of the sieve plates. Maximum
shear force was applied on the droplets by orifices of sieve plates, as the drop size at bottom
section of column was greater than the perforation diameter of plates. It has been observed
that an average reduction in the drop size was approximately 70% from the bottom section
plate (3rd from bottom) to middle plate (10th from bottom). Since, the dispersed phase
droplets of smaller size moved up through the middle section of the column, the shear force
recognized on these drops was low as compared to that of the bottom section. Hence,
the reduction in the drop size was marginal as compared to the bottom half section of the
column. Nearly 30% average reduction in the drop size has been observed from the middle
section to the top section plate (18th from bottom). From Fig. 4, it could be clearly seen that
the drop size profile is the function of active length of the column. Lorenz et al. [4], Jones
et al. [24], and Srinivasulu et al. [5] have also shown that the majority of drop breakage
was observed to occur during passage through the first two or three plates just above the
distributor.

Fig. 4. Drop size as function of column height.

INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014

 Hydrodynamics of a Pulsed Sieve Plate Extraction Column 245

4.1.5. Drop Size and Drop Size Distribution

The drop size distribution depends upon the breakage and coalescence of the drops at each sieve
plate of the column. It strongly depends on the range of pulse velocity. Generally, coalescence
of drops takes place at low pulse velocity and the mass transfer coefficients decreases as the
interfacial area decreases. Breakage of drops facilitates increase of the interfacial area and thus,
increases the mass transfer coefficients. Typical drop size distribution throughout the length of
column at three different sections, starting from bottom to the top, specifically at 3rd, 10th and
18th number of plates with four different pulse velocities have been shown in Fig. 5. In
particular, the effect of different pulse velocity on drop size distribution was studied and it was
found that, the drop size distribution narrowed down with increase in pulse velocity from 0.01
to 0.035 m/s. At low pulse velocity, the oscillatory Reynolds number (i.e. Reo = DAf/) was less,
so the turbulence was low. Flow developed due to oscillation of pulse velocity was characterized
by dimensionless number Reo. As a result, large size of droplets was formed. Due to low pulse
velocity, the coalescence of some of the drops also occurred. This causes the formation of
greater size drops in the column. Hence, high drop size distribution was observed at low pulse
velocity. Same results were also observed by Srinivasulu et al. [5] using kerosenewater system
for 0.76 m diameter column. As the pulse velocity increases, the energy input to the pool of the
continuous phase in the column increases. While forced through the perforations due to high
turbulence, the shear forces on droplets also increased proportionately with the pulse velocity.
As a result, the greater size droplets become unstable and the drop size reduced subsequently.
Eventually, the uniform size droplets were formed at high pulse velocity. It can be easily
observed from Fig. 5, that the effect of pulse velocity on the drop size distribution was minimum
at the 18th plate from bottom because of high pulse velocity (Af = 0.035 m/s), which means that,
deviation in the drop size decreases with increase in pulse velocity as production of more
homogenous drops takes place. Lorenz et al. [4] have also established that with increase in pulse
intensity, the drop size moved to the smaller diameter and also the drop size distribution turns
out to the thinner. Kagan et al. [2] attributed that at high pulse frequency the occurrence of
shear force on dispersed drops was repeated in less interval of time and resulted in the smaller
size drops. Also the break-up of greater size drops had taken place due to turbulence.
As the dispersed phase drops passes above the first 23 plates from bottom, the repeated
break-up at plate perforations, as well as horizontal plates and column walls, occurred. Drop
size distribution decreased as the dispersed phase flows upward in the column. At all pulse
velocities studied, with an increase in height of column from bottom to top, the drop size
distribution was shifted towards the narrow range of the drops.
It has been observed that the drop size distribution was also dependant on the
geometrical conditions. The drop size distribution was unimodal from second bottom plate
and uniform at low pulse velocities for 0.0015 m perforation diameter plates. As the
perforation diameter was small, the orifice velocity was very high, as well as resistance offered
by small flow area to the drops were also high. It has caused the high shear force on dispersed
phase drops. As the orifice velocity was high, the turbulence maintained throughout the
length of the column was greater even at low pulse velocity. Hence, the coalescence rate was
also very low at the bottom section of the column. With plate spacing of 0.05 m the repeated
break-up of drops was observed. Therefore, the rate of coalescence was also low and frequent
INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014
246 S OMKUWAR ET AL .

Fig. 5. Drop size distribution along the column height (from bottom to top).

application of shear force was realized by drops. Thus, the drop size distribution was thinner
at low plate spacing. Lorenz et al. [4] also revealed that the uniform drop size distribution was
dependent on plate geometry and it could be attained quickly at smaller perforation diameter
of the sieve plates. They have also reported that the drop size distribution was the function of
number of sieve plates and it was independent of plate spacing in the upper section of
the column. Moreover, it was observed that Sauter mean drop diameter and drop size
distribution were independent of the operating parameters like continuous and dispersed

INDIAN CHEMICAL ENGINEER Vol. 56 No. 3 September 2014

 Hydrodynamics of a Pulsed Sieve Plate Extraction Column 247

phase superficial velocity. The same results have been reported by Lorenz et al. [4] and
Srinivasulu et al. [5].

4.1.6. Model Predictions for Sauter Mean Diameter

All of the experimental drop size data reported in this study was correlated on the basis of all
operating parameters of PSPEC like continuous and dispersed phase superficial velocities and
pulse velocity and geometrical parameters, such as perforation diameter and plate spacing.
Linear regressions were performed to obtain the intercepts and correlation coefficients and
model has been formulated. The correlation developed for the Sauter mean diameter is,

d32 0:137d 0:16 h0:18 Vd0:07 Vc0:02 Af 0:55 1

From Fig. 6 it was found that, the correlation developed was fitted with 15% deviation from
the experimental values of Sauter mean diameter. It could be concluded from the operating
parameters that, with an increase in pulse velocity, the shear force on the drops increases
resulting in the smaller size of drops. It has also been established that the perforation diameter
and plate spacing have little role in reducing the Sauter mean diameter. Continuous and
dispersed phase superficial velocities have an insignificant part in drop size.

4.2. Dispersed Phase Hold-up

The design of PSPEC requires the information of cross-section to accommodate the specified
flows in the column. The knowledge of dispersed phase hold-up was required to determine the

Fig. 6. Plot of Sauter mean diameter computed from correlating equation versus experimental values.

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248 S OMKUWAR ET AL .

cross-section of column that corresponds to the flooding of the column. Hold-up means the
total amount of dispersed phase that contacted with the continuous phase in the active length
of the column. It was a function of drop size formed during pulsing motion in the column and
the dispersed phase flow rate. The interfacial area available for mass transfer depends on
hold-up besides drop diameter. Also, any counter-current column has limit of maximum
hold-up beyond which flooding occurs. Hence, one of the important control objectives to
achieve during column operation was to maintain a high value of dispersed phase hold-up,
while keeping away from flooding point for its efficient performance. Consequently, the hold-
up study was carried out extensively.

4.2.1. Effect of Pulse Velocity on Dispersed Phase Hold-up

From Fig. 7, three different regimes like mixer-settler, dispersion and emulsion regime have
been observed with increase in pulse velocity in PSPEC. In case of mixer-settler regime below
each of the horizontal sieve plate, dispersed phase layer was formed which gave slightly
higher value of hold-up, but the dispersed phase was not distributed in the continuous phase.
So, in mixer-settler regime, hold-up decreases to some extent with increase in the pulse
velocity, which corresponds to the transition from mixer-settler to the dispersion regime.
Further increase in pulse velocity gave the higher concentration of dispersed phase drops in
the neighborhood of the plates relative to the average concentration of the drops at every
section created by sieve plates. It was observed that, the hold-up increased in this regime with
additional pulse velocity. This is due to uniform distribution of dispersed phase drops in the
continuous phase throughout the active length of the column. The drop size in this regime
was smallest and the hold-up obtained was highest as a result of low rising velocity of small
size droplets. In the present work, the dispersed phase hold-up was measured for the pulse

Fig. 7. Effect of dispersed phase supercial velocity on hold-up at different pulse velocity.

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 Hydrodynamics of a Pulsed Sieve Plate Extraction Column 249

velocity ranging from 0.0150.031 m/s and around 10% increase in dispersed phase hold-up
has been observed at constant throughput. The maximum value of hold-up obtained was 21%
for a pulse velocity of 0.031 m/s and dispersed phase superficial velocity of 0.006 m/s.
Below the pulse velocity of 0.02 m/s the hold-up obtained was less and beyond 0.025 m/s
pulse velocity, the steady state operation would be difficult. Hence, for industrial scale, the
preferable pulse velocity range of 0.020.025 m/s has been selected. Lorenz et al. [4] have also
obtained the results in the same line.

4.2.2. Effect of Dispersed and Continuous Phase Superficial Velocity on Hold-up

The vital operating parameters next to the pulse velocity in PSPEC are dispersed and
continuous phase superficial velocities. From the experimental results shown in Fig. 7, it has
been observed that the dispersed phase superficial velocity was strongly influencing the
dispersed phase hold-up. Rapid increase in the hold-up was obtained with the dispersed phase
flow rate. However, the continuous phase superficial velocity has negligible effect on the hold-
up as shown in Fig. 8 at constant pulse velocity and dispersed phase throughput with same
geometry. In the range of continuous phase superficial velocity of 0.0020.005 m/s, the
dispersed phase hold-up was 13%. From this it can be concluded that the hold-up increases
with phase ratio Vd/Vc. Lorenz et al. [4] have also obtained the same results for three different
systems. They have revealed that drop size is independent of throughput. Hence, the higher
values of hold-up was only the effect of throughput enhancement up to flooding point with
direct inducement of dispersed phase by increase in Vd. Other investigators, Sehmel and Babb
[11], Bell and Babb [17], Mishra and Dutta [15], Khemongkorn et al. [6] and Venkatanarasaiah
and Verma [13] have also obtained the same results.

Fig. 8. Effect of continuous phase supercial velocity on hold-up.

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250 S OMKUWAR ET AL .

4.2.3. Effect of Plate Spacing on Hold-up

As shown in Fig. 9, dispersed phase hold-up was measured at different plate spacing of 0.05
m and 0.1 m. It was observed that hold-up reduces with increase in plate spacing in the
PSPEC. The visual observation concluded that close plate spacing helped in breaking the
drops as they pass through more number of plates and higher restriction was created in
the direction of the flow. Hence, the shear force realized on the dispersed phase drops was
more and small size of drops was formed with maximum number of plates (obstacles). As a
result of this rise, velocity of dispersed phase drops decreases and residence time of the drops
increases. Eventually dispersed phase hold-up increases. This finding was also in line with the
observation of various authors like Miyauchi and Oya [8], Mishra and Dutta [15], Kumar
and Hartland [16], Venkatanarasaiah and Verma [13].

4.2.4. Effect of Perforation Diameter on Hold-up

The sieve plate of two different perforation diameters of 0.0015 and 0.003 m was studied
separately for dispersed phase hold-up measurement. It was observed from Fig. 9, that the
hold-up decreases with increase in the perforation size. The shear force exerted on drops at
0.0015 m perforation diameter was greater than that of 0.003 m perforation size plates. The
reduction in drop size took place throughout the active length of the column started at the
first plate from the bottom. Dispersed phase hold-up was increased as a result of high
residence time of smaller size droplets. The hold-up does not change according to perforation
diameter, once the drop size becomes smaller than perforation size. Hence, the effect of
perforation size was less as compared to other geometrical parameters like plate spacing and
FFA. The same results were observed by Mishra and Dutta [15]. They have also studied the
effect of perforation size, plate spacing and FFA of the multiorifice sieve plates on 0.0765 m

Fig. 9. Effect of plate spacing and perforation diameter on hold-up.

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 Hydrodynamics of a Pulsed Sieve Plate Extraction Column 251

column diameter. It was concluded that hold-up decreases with increase in any of these
geometrical properties. Venkatanarasaiah and Verma [13] have also studied the effect of
geometrical parameters using the kerosene-water system with n-butyric acid and benzoic acid
as solute. They have carried out experiments on the geometrical conditions of sieve plate and
obtained similar results.

4.2.5. Effect of Fractional Free Area on Hold-up

Two different sieve plates of 0.2 and 0.3 FFA with 0.003 m perforation diameter and 0.05 m
plate spacing were used to study the effect of free area on hold-up. The reduction in dispersed
phase hold-up was observed with increase in the FFA of the plate, as shown in Fig. 10.
Increase in the FFA resulted in decrease in restriction of drops to travel in the direction of
flow. Hence, less shear force was realized by drops at greater FFA of 0.3 as compared to the
FFA of 0.2. At dispersed phase superficial velocities above 0.005 m/s, the significant increase
in hold-up was observed with high FFA. Mishra and Dutta [15], Lorenz et al. [4], Kumar and
Hartland [16], and Venkatanarasaiah and Verma [13] have also obtained the similar trend for
free area of the plate.

4.2.6. Model Predictions for Dispersed Phase Hold-up

The dispersed phase hold-up data was also correlated with the model formulated form linear
regression method as follows,

/ 8:98d 0:12 h0:16 a0:2 Vd0:92 Vc0:05 Af 0:7 2

From Fig. 11 it was observed that, the correlation developed was fitted with 20% deviation
from the experimental values of dispersed phase hold-up. The dispersed phase superficial

Fig. 10. Effect of fractional free area on hold-up.

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252 S OMKUWAR ET AL .

Fig. 11. Plot of dispersed phase hold-up computed from correlating equation versus experimental
values.

velocity was highly influencing the dispersed phase hold-up. Pulse velocity also plays an
important role to obtain greater dispersed phase hold-up. Negligible effect of the continuous
phase superficial velocity was found on dispersed phase hold-up. Perforation diameter, plate
spacing and FFA are inversely proportional to the dispersed phase hold-up.

4.3. Flooding Characteristics

PSPEC was operated in a counter-current mode in which aqueous phase was fed at the top of
the column and organic phase was dispersed by charging from bottom of the column. The
liquid phases in the column were displaced in converse direction with the help of energy input
in the form of pulse velocity. The pulse velocity helps to generate agitation inside the column
that leads to the breakage of lighter or organic phase as it was forced to pass through the
perforated plates. Thus, formation of small drops throughout the length of the column had
taken place. Pulse velocity was the only parameter that has decided the flow regime and the
flooding inside the column. Flooding was the limitation of the operation and the column
cross-section area can be measured by the flooding throughput. Flooding was mainly
depending on the operating pulse velocity and phase flow rates. Flooding curve was a
parabolic curve which starts at the origin of the co-ordinates and it forms by different flow
rates of the phases, insufficient pulsation and higher pulsation depending on regime of
operation.

4.3.1. Effect of Pulse Velocity on Flooding Curve

When the column was operated below the minimum pulse velocity that is, insufficient pulse
velocity zone, the flooding occurred in the mixer-settler regime of operation as shown in Fig. 12.
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 Hydrodynamics of a Pulsed Sieve Plate Extraction Column 253

Fig. 12. Effect of pulse velocity on throughput at different geometry.

Flooding commenced at the bottom plate because of insufficient pulses available to push the
organic phase, through perforations. In mixer-settler regime of operation, the dispersed phase
drops were larger in size and form a settled layer beneath the next plate before the arrival of the
next pulse. Hence, the dispersed phase accumulated into the column and finally went out from
the outlet of the continuous phase. In this regime, with increase in pulse velocity the capacity of
the column decreased and operation was shifted to the dispersion regime. In this regime, the
dispersed phase was evenly distributed throughout the continuous phase with the increase in
pulse velocity in the column. It was also observed that the rise velocity of the drops was less
compared to the upcoming flow of the continous phase. Hence, drops have started
accumulating in the disenging section of the column and finally passed out through the outlet
of the continuous phase. This was the flooding due to excessive pulsing in the emulsion regime
of operation. Thornton [18], McAllister et al. [25], Smoot and Babb, [26], Kagan et al. [2],
Berger and Walter [19], Lorenz et al. [4] and Tribess and Brunello [20] have also observed the
same results. Kagan et al. [2] have also used the kerosene-water system and found that, in
mixer-settler regime as the pulse velocity increases, the capacity of the column increases.
However, flooding occurs with further increase in the pulse velocity in dispersion regime at
higher flow rates, which decreases the capacity of the column.
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254 S OMKUWAR ET AL .

4.3.2. Effect of Plate Spacing on Throughput

From Fig. 12, it was observed that with increase in plate spacing the throughput increased.
Increase in plate spacing from 0.05 m to 0.1 m resulted in reduction of the number of plates
from 20 to 10 in 1 m length column. Hence, the occurrence of the application of the shear
force on droplets was reduced. Thus, the drop size was greater at plate spacing of 0.1 m
compared to 0.05 m. Consequently, with further increase in rise velocity more number of
drops easily reached the top of the column resulting in higher throughput. It was concluded
that the throughput increases with an increase in the plate spacing. This was also consistent
with the result observed by McAllister et al. [25], Smoot and Babb [26], Kagan et al. [2].
Tribess and Brunello [20] reported that with increase in plate spacing, the number of plates
reduces and the shear force on the drops also reduces, which results in an increase in the mean
drop diameter with greater throughput.

4.3.3. Effect of Perforation Diameter on Throughput

Decrease in perforation size reduced the throughput slightly as shown in Fig. 12. However,
the effect of perforation size was less compared to plate spacing. The perforation diameter
used for this study was 0.0015 and 0.003 m. Since, the dominance of pulse velocity was higher
than that of different perforation diameters; the comparable sizes of drops were formed.
Thus, no substantial difference in throughput occurred. Lorenz et al. [4] have also explained
the effect of perforation size on flooding curve by considering the 0.004 m and 0.006 m
perforation sizes. They have observed that, maximum throughput was obtained at 0.006 m
perforation diameter. This effect was also explained on the basis of drop size formation and
its rise velocity with two different perforation sizes.

4.3.4. Effect of Fractional Free Area on Throughput

It was observed that, the throughput increases with FFA in PSPEC. At high FFA the cross-
sectional area, available for both phases was greater. So, at upstroke and down stroke the
shear force realized by drops was low. From Fig. 12, it was found that for FFA of 0.2 and 0.3
the maximum throughput obtained was 0.016 and 0.02 m at pulse velocity of 0.025 m/s. It
was also observed that, beyond pulse velocity of 0.025 m/s the reduction in throughput was
significant with FFA of 0.2 as compared to 0.3 due to greater turbulence generated in case of
FFA of 0.2. Berger and Walter [19] and Lorenz et al. [4] have also studied the effect of free
area and concluded that with increase in FFA, maximum throughput increased. They have
also found the effect of physical properties on flooding curve with increasing free area using
three different systems and concluded that flooding increased with the interfacial tension due
to increase in the drop size.

4.3.5. Effect of Phase Ratio on Throughput

From Fig. 13, it was observed that with increase in phase ratio (O/A) from 1:6 to 1:1,
throughput decreases. Since the dispersed phase flow rate increases, the dispersed phase hold-
up increases and consequently the drop population throughout the length of column
increases. In the presence of greater number of drops, the flow area available for continuous
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 Hydrodynamics of a Pulsed Sieve Plate Extraction Column 255

Fig. 13. Effect of phase ratio on throughput at different geometry.

phase flow was reduced. So, the resistance to the continuous phase flow increased and
ultimately the overall throughput increased at low O/A ratio. Berger and Walter [19] and
Lorenz et al. [4] have also observed that the flooding curve decreases with increase in O/A
ratio. They have also studied flooding for the different systems and finally concluded that the
flooding curve was function of interfacial tension, density and visocity of the system. Kagan
et al. [2] also found that the throughput decreased with increase in the phase ratio Vd/Vc for
kerosene-water system.

5. Conclusions
Hydrodynamic characteristics in a PSPEC have been studied scrupulously at different
geometrical and operating parameters. From this comprehensive work it has been observed
that, all hydrodynamic properties that is, drop size, dispersed phase hold-up and flooding
characteristics are influenced by column sieve plate geometry like perforation diameter, plate
spacing and FFA. Pulse velocity was the vital operating parameter in hydrodynamics of
PSPEC and notably influences the Sauter mean diameter and consequently the dispersed
phase hold-up and throughput in the column. Dispersed phase superficial velocity affect hold-
up and throughput substantially. However, insignificant effect of continuous phase superficial
velocity has been found on drop size.
For design of PSPEC the preferable geometrical conditions for kerosene-water system
were perforation diameter of 0.003 m, plate spacing of 0.05 m and FFA of 0.2 with the
operating parameters like pulse velocity of 0.025 m/s and superficial velocity of 0.006 m/s
using organic to aqueous ratio (O/A) of 1:1. The drop size obtained at these conditions was
0.0015 m with dispersed phase hold-up of 18%. The correlations developed in the work will
help in predicating the values, which will further helpful in a design of the column.
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256 S OMKUWAR ET AL .

Nomenclature
A amplitude of pulsation (m)
Af pulse velocity (m/s)
D column diameter (m)
d perforation diameter (m)
d32 Sauter mean diameter (m)
f frequency of pulsation (Hz)
h plate spacing (m)
Reo oscillatory Reynolds number
Vc superficial velocity of the continuous phase (m/s)
Vd superficial velocity of the dispersed phase (m/s)
Vo characteristics velocity of drops (m/s)
Vslip slip velocity (m/s)
Greek Symbols
fractional free area
dispersed phase hold-up
kinematic viscosity (m2/s)

Acknowledgement
The authors would like to acknowledge Department of Atomic Energy (DAE) for the financial support.

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