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Vertical extraction columns meet the needs of industrial applications, but when height limitation (especially
in indoor applications) is a concern it is required to use horizontal columns. Considering the signicant role
of mass transfer in the sizing and scale-up of horizontal extraction columns, no analytical and experimental
investigations have been conducted in this regard. In the present research, the eect of operating
parameters including pulsation intensity and phase ow rates on the mean drop size and the dispersed
phase holdup values was investigated in a horizontal pulsed sieve-plate column under both mass transfer
directions for the tolueneacetonewater, n-butyl acetateacetonewater and butanolacetonewater
systems. The results show that holdup decreases rst and then increases with an increase of pulsation
intensity. Increasing dispersed phase velocity also increases holdup. The mean drop size decreases with
an increment of pulsation intensity, whereas ow rates of both phases have little impact. Moreover, it is
Received 3rd December 2016
Accepted 23rd January 2017
observed that the presence of mass transfer signicantly aects the mean drop size and holdup. Finally,
new correlations were proposed for the prediction of mean drop size and holdup based on operating
DOI: 10.1039/c6ra27723c
variables and physical properties of the systems with and without mass transfer. Average Absolute
rsc.li/rsc-advances Relative Error (AARE) of the correlations was between about 6.8315.38% for their optimized constants.
8908 | RSC Adv., 2017, 7, 89088921 This journal is The Royal Society of Chemistry 2017
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of the column and together with the holdup, it determines the ooding characterization, drop size, holdup and mass transfer
interfacial area available for mass transfer.1215 as well as comparing proposed correlations for these variables.
Similar to drop size, dispersed phase holdup is an important However, in spite of extensive work and various correlations
design parameter aecting the column dimension, and also the which are available in the literature related to these hydrody-
overall mass transfer coecient. The dispersed-phase holdup namic parameters in the vertical pulsed sieve-plate columns,
(4) can be dened as the volume fraction of the extraction the investigations on the horizontal pulsed sieve-plate columns
column which is occupied by the dispersed phase: are scarce. In particular, Khajenoori et al.,10 have studied the
vd eect of operating parameters on the drop size as well as drop
4 (1)
vd vc size distribution in a horizontal pulsed sieve-plate column and
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phase volume. Values of holdup can be used for the determi- operating parameters in the absence of mass transfer. More-
nation of the ooding velocity16,17 and it is completely related to over, slip and characteristic velocities of both phases have been
the overall mass transfer coecients in the following manner: studied by the same author.45
64 Considering the signicant role of mass transfer in the
KE a KE (2)
d32 sizing of extraction columns, no analytical and experimental
investigations have been conducted into the impact of mass
64 transfer direction on the mean drop size and dispersed phase
KR a KR (3)
d32 holdup for the horizontal sieve-plate columns. Therefore, pre-
senting a reliable estimation of the mean drop size as well as
where KE and KR are the overall mass transfer coecients based
holdup for this type of column in dierent operating conditions
on the extract and ranate phases, respectively, a is the inter-
is needed. In this work, the Sauter-mean diameter and holdup
facial specic surface area (m2 m3), d32 is Sauter mean diam-
value with the mass transfer in both directions have been
eter (m) and 4 is the dispersed phase holdup. Therefore, it can
investigated in a horizontal pulsed plate column. The eects of
be concluded from the literature, drop size and holdup are two
operating parameters including pulsation intensity and ow
key parameters to understand the hydrodynamic of the extrac-
rates of the continuous and dispersed phases on drop size and
tion column.
the dispersed phase holdup have been studied. In addition,
Numerous investigations have been carried out on the
a theoreticalexperimental correlation for Sauter drop size as
impact of the column geometry in pulsed extraction
well as holdup in terms of the operating conditions and the
columns.1820 It was achieved that the column diameter is
physical properties of chemical systems is proposed.
almost ineective on the mean drop size and the variation of
drop sizes are more intense in initial internal plates. Due to the
importance of mean drop size, many researches were imple-
mented on the impact of operating variables including the 2. Experimental
pulsation intensity (Af) and ow rates of the dispersed and the 2.1. Description of equipment
continuous phases on drop size as well as introducing correla-
Experiments were carried out in a semi-industrial pulsed sieve-
tions for prediction of mean drop size in pulsed
plate column. A glass pulsed column in horizontal position with
columns.10,12,13,2131 Moreover, the evaluation of the dispersed
an internal diameter of 6.2 cm and length of the active area of
phase holdup in dierent conditions is also studied by many
146 cm was used in these experiments. The active part of
investigators.5,16,26,29,3238
column was a pipe housing an internal plate cartridge con-
In the absence of pulsation, interfacial tension and buoyancy
sisting of 25 pairs of sieve plates constructed from stainless
are the cause of the drop breakage,13,20 while in the presence of
steel 304. The plates are half-perforated and the holes laid on
pulsation, a smaller drop is formed as a consequence of an
triangular pitch of 4 mm. The pulsation applied to the liquid by
intensied collision between the drops and the internal plates
the pressure of air compressor and controlled by two solenoid
and the internal wall, which causes a higher breakage
valves. Due to counter-current ow of two liquid phases, each of
rate.10,30,39,40 Also it is achieved that increasing the ow rate of
them in the opposite direction of another side columns are
both phases lead to a slight increase in mean drop diameter
imported so that the light phase interred in direction of
which was in accordance with other studies.18,25,29,30,41
applying pulsation. To control the liquid level in the column
According to literature, an increase in the fractional free area
and regulate the discharge of heavy phase, an optical sensor in
or plate spacing reduces the shear forces on drops resulting in
the collecting tank, in the output of the light phase, is
an increase in drop size which leads to reduction in holdup.
embedded. Two settlers at both ends of the column were
Holdup is a strong function of the dispersed phase velocity (Vd)
employed to separate the two liquid phases. The inlet and outlet
and an increase in Vd increases holdup.4,42 However, the eect of
streams of the column were connected to four tanks, each of 25
continuous phase velocities (Vc) on holdup has been found be
liters capacity. The ow rates of the two phases were measured
negligible.43,44 Yadav and Patwardhan20 presented a well review
by two rotameters. For more information, the column charac-
on the design aspects of pulsed sieve-plate columns, consid-
teristics are listed in Table 1. Also, a schematic diagram of
ering investigations on ow regimes in pulsed plate columns,
experimental apparatus is shown in Fig. 1.
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Table 1 Geometrical characteristics of the column used present research, the values of physical properties have been
assumed to correspond to the mean values of acetone concen-
Characteristics Values
tration in the continuous and dispersed phases. The mean value
Column length (m) 1.46 of acetone concentration was obtained by averaging the values
Column diameter (cm) 6.2 obtained at the inlet and outlet of the column.
Material of construction the column Glass
Upper and lower settler diameter (cm) 9
Lower settler length (cm) 30 2.3. Analytic procedure
Upper settler length (cm) 60
Initially, both phases were mutually saturated each other before
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Plates thickness (mm) 1 step in the experiments since the volume fraction of acetone is 3%
Plate spacing (cm) 1a, 5b and the excessive dissolution of each phase to the other liquid
Average free area of the plates (%) 0.11
might signicantly aect the hydrodynamic and mass transfer
a
Spacing between two individual plates in a cell. b Spacing between two performance of the column. Aer complete separation, they were
adjacent cells.
transferred to the feed tanks. At the beginning of each run, the
column was lled completely with distillated water. Dispersed
phase was then entered to the column. Aer adjusting the ow
2.2. Chemical system
rate of each phase based on the operating conditions, the pulsa-
Three liquidliquid systems were chosen to cover a wide range of tion intensity with specied amplitude and frequency was applied
values of interfacial tension (1.530 mN m1). The chemical to the setup. All experiments were carried out under ooding
system used for testing were toluene, n-butyl acetate and butanol conditions and sucient time, 60120 min depending on the
as the light phase (dispersed phase) and distillated water as the phase ow rates and the particular liquidliquid system used was
heavy phase (continuous phase) with 3% volume fraction of provided for reaching the steady state conditions.
acetone dissolved in each of the phases regarding the considered Drop size was measured by taking digital images of the
direction of mass transfer. Technical grade solvents of at least 99.5 contents of the column using a Nikon D3100 camera. Drop sizes
wt% purity were used as the dispersed phase and all experiments were measured on the 5 stages of the column which were equi-
were carried out at the temperature 20 C. The physical properties distant from each other. To calculate the size of drops, images
of these systems are listed in Table 2. The viscosities of both were analyzed by AutoCAD soware. Indeed, the diameter of the
phases are measured by a laboratory LAUDA viscometer. The column and the distance between two plates were set on their
densities are determined by use of a scale in order of 0.0001 g. It known values to provide a coordinate grid for measuring the drop
should be noted that, under mass transfer conditions, a degree of sizes. 300 drops were analyzed in each experimental condition. A
uncertainty surrounds the estimation of physical properties picture of drops, for instance, is shown in Fig. 2.
(particularly interfacial tension), since these vary not only with the The most commonly-used representative diameter which
inlet solute concentrations, but also along the column. In the used to study the mean drop size in the solvent extraction
8910 | RSC Adv., 2017, 7, 89088921 This journal is The Royal Society of Chemistry 2017
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1 S
Li 2ri cos p (6)
2 ri
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the pulsation, the drops will be driven through the plate the solute concentration. Therefore, it is almost impossible to
perforations along with hitting of drops with the wall and plate determine the drop breakage via the constant interfacial
holes which leads to smaller drops. On the other hand, the tension in the presence of mass transfer, whereas the gradient
coalescence will induce rectication of liquid drops into larger of interfacial tension is of most importance.
ones. The main operating parameters found to inuence mean When there is mass transfer from the continuous phase to
drop are the phase ow rates and pulsation intensity. The eect the dispersed phase, smaller drops are produced in comparison
of pulsation intensity on Sauter-mean drop diameter at both to the same condition without mass transfer. In fact, because of
mass transfer directions is shown in Fig. 3. It is clear that drops the consequent interfacial tension gradient, the interface
produced from the high interfacial tension system (toluene movement of the drop and the inner circulation generated into
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acetonewater) is larger than those produced from the medium the drop gain the same direction. Therefore, this mass transfer
and lower interfacial tension systems. It can also be observed direction leads to an increase in the interface deformations,
Open Access Article. Published on 30 January 2017. Downloaded on 07/02/2017 06:27:15.
that the eect of pulsation intensity on the mean drop size of consequent deformation of drops and higher drop breakage.
high interfacial tension system is larger than that of other When mass transfer occurs from the dispersed phase into
systems. Drops become smaller with the increase of pulsation the continuous phase, larger drops are observed in comparison
intensity due to intense collision of the organic phase with trays to the same condition without mass transfer and with the
and column wall and breaking into the smaller drops. reverse direction of the mass transfer. It is expected due to the
Regarding to the mass transfer direction, it is clear that larger opposite interfacial tension gradient compared to the reverse
drops will be produced in the direction from the dispersed direction of the mass transfer. Therefore, in this case, the drops
phase to the continuous phase, which are achieved in all are consequently more stable than the former case. The eect of
systems. Also, the eects of pulsation intensity on the mean mass transfer direction on the mean drop size with increasing
drop size are similar in both directions which means that the the pulsation intensity for the tolueneacetonewater system is
impact of pulsation intensity is eectless of the direction of shown in Fig. 4.
mass transfer. The eect of dispersed phase ow rate on the mean drop size
Furthermore, in another investigation by Khajenoori et al.,10 in both directions of mass transfer is shown in Fig. 5. Increasing
the eect of operating parameters on the mean drop size was the ow rate of the dispersed phase leads to an increase in the
studied which their results are compared with the experimental drop size. With respect to Fig. 3, the impact of dispersed phase
data from this work due to the same column used in both ow rate is found to be weaker than the inuence of pulsation
studies. For instance, the variation of mean drop size versus intensity on the mean drop size. The increase of drop size may
pulsation intensity obtained from this work and Khajenoori be attributed to an increase in the coalescence rate due to the
et al.,10 for constant dispersed and continuous phase ow rates larger values of the dispersed phase holdup that are observed as
of 2.1 and 5 l h1 is illustrated in Fig. 4. The results show that the dispersed phase ow rate increases. From Fig. 5 also can be
the presence of mass transfer highly aects the mean drop size found that the drop size with mass transfer direction from the
in following manner: dispersed phase to the continuous phase is larger than that with
The presence of solute (3% volume fraction of acetone the one determined in the inverse mass transfer direction.
dissolved in each of the phases is considered in this study) is The eect of continuous phase ow rate on Sauter-mean
along with the evolution of the interfacial tension. According to drop size with both mass transfer directions is illustrated in
Msek et al.,46 the interfacial tension declines with increasing Fig. 6. It is observed that the mean drop diameter slightly
Fig. 4 Variation of mean drop size versus pulsation intensity under Fig. 5 Eect of the dispersed phase ow rate on the mean drop size at
dierent mass transfer conditions obtained from this work and Kha- constant pulsation intensity of 0.8 cm s1 and the continuous phase
jenoori et al.,10 at constant dispersed and continuous phase ow rates ow rate of 5 l h1 for dierent liquidliquid systems in the presence of
of 2.1 and 5 l h1. mass transfer in both directions.
8912 | RSC Adv., 2017, 7, 89088921 This journal is The Royal Society of Chemistry 2017
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the continuous phase to the dispersed phase than those observed that increasing the ow rate of the dispersed phase
measured with no mass transfer, and even higher than those leads to an increase in the dispersed phase holdup. With
measured when acetone transferred in reverse direction. As respect to Fig. 7 and 8, the impact of pulsation intensity on
discussed in Section 3.1, this is due to the evolution of inter- holdup is found to be stronger than the eect of the dispersed
facial tension with the direction of mass transfer. This phase ow rate as similar trends are observed for the mean drop
phenomenon is called Marangoni eect.47 Generally, higher diameter. Regarding to the presence of mass transfer, the ow
holdup values can be found with mass transfer direction from rate of the dispersed phase shows similar impact on the holdup
the continuous phase to the dispersed phase, leading to higher values in both directions of mass transfer.
performances but earlier ooding points. The variation of the dispersed phase holdup versus the
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The eect of the dispersed phase ow rate on holdup with continuous phase ow rate is illustrated in Fig. 9. It is revealed
both two directions of mass transfer is shown in Fig. 8. It is that the holdup slightly increases with an increase in the
Open Access Article. Published on 30 January 2017. Downloaded on 07/02/2017 06:27:15.
Pulsed column
Reference type Correlation
!
22 VPSPC Af0:3 s0:5 mc 0:1
d32 0:92
rc 0:6 g0:4
1:2
48 VPSPC Af
d32 2:03 105
h1:3
0:6
49 VPSPC s
d32 C Af1:2
rc
0:6 0:8 0:4
25 VPSPC s a d
d32 0:57
rc 2Af1:2
50 VPSPC !0:18 0 1
10:14
0:06
d32 h @ md g A s Af 2
4
p 1:35a0:4 p 0:23 exp 29:66
s=Drg s* =r* g 1 3 s* ga
r* 4 s* 4
1!
0 1
51 VPSPC 0:10 1
d32 0:74 h AfDr4 AfDr 4
p Ca exp 3:00 1 1 exp@28:56 1 1 A
s=Drg h*
g 4 s4 g 4 s4
0:4
52 VPSPC s
d32 C Af0:8 a0:48 d 0:26 h0:34
rc
4 0:2304 4 0:0514
30 VPPC Af rc mc g Qc 0:0321
d32 8:26 105 1
sg Drs3 Qd
!0:239 0:0473 0:1645
5 Af4 rc mc 4 g h
d32 7:1 10
sg Drs3 H0
0 10:444
10 HPSPC 0:203 0:025
Q m B s C
2:8 104 1
c
@ qA
d
d32
Qd mc
rd Af Qd
3
8914 | RSC Adv., 2017, 7, 89088921 This journal is The Royal Society of Chemistry 2017
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Pulsed column
Reference type Correlation
bhs1=4 g5=4 gs Vd rc rc s3
!1:90 0:36 !
54 VPSPC
Af md 2 r Af3
4C Vd 1:1 ; for c 2 $ 0:06 kg s2
bh1=3 sDr 2a
44 VPSPC 4 K1 expK2 Af Afm Vd 0:86 Vc Vd 0:28 Dr0:30 rd 0:93 md 0:77
!0:33
3 sDr a
1=4
Afm 9:69 10
md 3=4
mass transfer, which covers the eect of operating parameters et al.,10 and the results are illustrated in Fig. 11. It is found
and physical properties of the liquid systems. They proposed that eqn (10) is not able to satisfactorily predict the mean drop
following correlation: size with the presence of mass transfer. Since there is no
0 10:444 correlation for prediction of mean drop size in the horizontal
0:203 0:025 pulsed plate column, there is a need to propose a correlation
Q m B s C
d32 2:8 104 1
c
@ qA
d
Qd mc 3 as a function of operating parameters and physical properties.
rd Af Qd
Consequently, for prediction of mean drop size, a new
(10) theoreticalexperimental correlation is developed in terms
of physical properties of the systems and operating parame-
ters by dimensional analysis methods (Buckingham's pi-
The experimental data with the presence of mass transfer
theorem):
are compared with the correlation proposed by Khajenoori
8916 | RSC Adv., 2017, 7, 89088921 This journal is The Royal Society of Chemistry 2017
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Table 6 Regressed constant C for eqn (15) based on experimental 0:124 !0:286
0:783
HPC data Qc Af4 rc rc
4 C 1
Qd gs Dr
Data source Mass transfer C AARE (%) 4 0:071 !0:282
md g Af3 Qd rd 2
Khajenoori45
(16)
None 0.97 15.47 s rc
3 s2
This study c/d 0.101 8.02
This study d/c 0.089 6.36 where C 0.089 for mass transfer from the continuous phase to
the dispersed phase and C 0.101 for mass transfer with the
opposite direction. Moreover, the experimental data from the
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Table 7 Experimental studies on vertical pulsed sieve plate columns: details of operating conditions and column dimensions
Investigators
8918 | RSC Adv., 2017, 7, 89088921 This journal is The Royal Society of Chemistry 2017
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Table 8 Experimental studies on vertical pulsed sieve plate columns: details of chemical systems investigated and physical properties
Investigators
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PDDC Pulsed disc and doughnut column 14 N. A. Moraes, J. B. A. Paulo and G. S. Medeiros, Brazilian
Q Volumetric ow rate, m3 s1 Journal of Petroleum and Gas, 2011, 5, 7585.
V Velocity, m s1 15 G. Zhou and S. M. Kresta, Chem. Eng. Sci., 1998, 53, 2063
Vc Supercial velocity of continuous phase, m s1 2079.
Vd Supercial velocity of dispersed phase, m s1 16 W. Pietzsch and E. Blass, Chem. Eng. Technol., 1987, 10, 73
Vslip Slip velocity, m s1 86.
VPPC Vertical pulsed packed column 17 S. Akhgar, J. Safdari, J. Towghi, P. Amani and M. H. Mallah,
VPSPC Vertical pulsed sieve-plate column RSC Adv., 2017, 7, 22882300.
v Kinematic viscosity, m2 s1 18 N. M. Spaay, A. J. F. Simons and G. P. Ten Brink, in Proc.
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42 M. Asadollahzadeh, J. Safdari, A. Haghighi-Asl and M. Torab- 51 A. Kumar and S. Hartland, Liq.-Liq. Extr. Equip., 1994, 625
Mostaedi, Chem. Ind. Chem. Eng. Q., 2012, 18, 255262. 735.
43 Y. Wang, K. A. Mumford, K. H. Smith, Z. Li and 52 K. Sreenivasulu, D. Venkatanarasaiah and Y. B. G. Varma,
G. W. Stevens, Ind. Eng. Chem. Res., 2016, 55, 714721. Bioprocess Eng., 1997, 17, 189195.
44 A. Kumar and S. Hartland, Chem. Eng. Process., 1988, 23, 41 53 A. Kumar and S. Hartland, Chem. Eng. Res. Des., 1983, 61,
59. 248252.
45 M. Khajenoori, J. Safdari, A. H. Asl and M. H. Mallah, Chem. 54 L. Tung and R. Luecke, Ind. Eng. Chem., 1986, 664673.
Eng. Technol., 2015, 38, 17831792. 55 S. Dimitrova Al Khani, C. Gourdon and G. Casamatta, Ind.
46 T. Msek, R. Berger and J. Schroter, EFCE Publ. Ser., 1985, 46, Eng. Chem. Res., 1988, 27, 329333.
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