Rasio Oa Darekar2014
Rasio Oa Darekar2014
Rasio Oa Darekar2014
Hydrometallurgy
journal homepage: www.elsevier.com/locate/hydromet
a r t i c l e i n f o a b s t r a c t
Article history: Liquid–liquid extraction experiments have been carried out in two different types of microchannels using water
Received 9 July 2013 (Zn) D2EHPA + dodecane system, a standard reactive extraction system recommended for evaluation of liquid–
Received in revised form 18 October 2013 liquid extraction equipment. The microchannels used in the experiments are a t-junction serpentine
Accepted 9 January 2014
microchannel and a split and recombine microchannel. Effects of O/A ratio and residence time on overall volu-
Available online 24 January 2014
metric mass transfer coefficient have been studied and an attempt has been made to explain the experimental
Keywords:
trends with the help of liquid–liquid flow patterns observed by using a high speed image acquisition system. Cor-
Microchannel relations relating overall volumetric mass transfer coefficients to O/A ratio and velocity are reported for both the
Mass transfer coefficient microchannels.
Serpentine © 2014 Elsevier B.V. All rights reserved.
Split and recombine
D2EHPA
0304-386X/$ – see front matter © 2014 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.hydromet.2014.01.010
M. Darekar et al. / Hydrometallurgy 144–145 (2014) 54–62 55
Fig. 2. Schematic layout of the t-junction serpentine microchannel and its microfluidic junction.
is to ensure rapid mixing, the role of the reaction channels is to provide and is found to be 11.4. Flow patterns are observed using a high speed
sufficient time for reaction or mass transfer. image acquisition system. In both the microchannels the microfluidic
The split and recombine microchannel, its mixing unit and mixing junctions are not optically accessible and hence flow patterns have
principle are shown in Fig. 3. The chip has got two microchannels, been observed at locations away from the junctions. Experiments are
only one of which is used in the experiments. This microchannel carried out to study the effect of O/A ratio and residence time on overall
has very small volume i.e. 26 μL and is basically a micromixer work- volumetric mass transfer coefficient (KLa).
ing on the principle of multi-lamination, as shown in Fig. 3. The
equivalent diameters of the main channel and the side channels are 3. Evaluation of overall volumetric mass transfer coefficient
184 μm and 71 μm respectively. The volume of the tube connecting
the outlet of the microchannel with the membrane separator is Overall volumetric mass transfer coefficients are calculated based
3 μL. The liquid holdup in the membrane separator is 75 μL. on the concentration of zinc in the organic phase. The driving force
for mass transfer, in general, will vary from the entrance to the exit
2.3. Phase system and procedure of the microchannel and hence, in an analogy with log mean temper-
ature difference (LMTD) in a heat exchanger, a log mean concentra-
The phase system used in the experiments is a reactive extraction tion difference (LMCD) can be defined as
system. Several studies on mechanism of extraction in this reactive
extraction system are reported in literature (Mörters and Bart, ðC oi −C oi Þ−ðC oo −C oo Þ
2000; Wachter et al., 1993) and hence these details are omitted ΔLMC ¼ ð1Þ
ln C oi −C oi =ðC oo −C oo Þ
here for brevity. The feed is an aqueous solution of zinc sulfate in
water. The organic phase is a 5% (v/v) solution of di-(2-ethylhexyl)-
phosphoric-acid (D2EHPA) in dodecane. Initially the organic phase is Using LMCD, the mean value of mass transfer flux can be written as
equilibrated with demineralized (DM) water in a stirred tank. After
equilibration, the phases are separated and zinc sulfate is added to the N ¼ K L ΔLMC ð2Þ
equilibrated water to prepare 500 ppm zinc feed solution. The equili-
bration step ensures that in subsequent experiments the transfer of
the solute from the aqueous phase to the organic phase is solely due The mean value of mass transfer flux will also be equal to
to interphase mass transfer and not due to solubility. The distribution
coefficient of the system, defined as the ratio of the concentration of Q o ðC oo −C oi Þ
N¼ ð3Þ
the solute in the organic phase to that in the aqueous phase, is measured Va
Fig. 3. The split and recombine microchannel, its mixing unit and multi-lamination principle.
M. Darekar et al. / Hydrometallurgy 144–145 (2014) 54–62 57
Combining Eqs. (2) and (3) the overall volumetric mass transfer co- becomes finer on reducing residence time from 98 s to 33 s. When
efficient can be written as the residence time is further reduced to 5 s, small slugs separated
by very fine droplets are observed. The droplets are now so fast mov-
C oo −C oi ing that higher shutter speeds are required to capture them causing
KLa ¼ ð4Þ
V illumination to be insufficient. Even at higher shutter speeds edges
Δ
Q o LMC of the drops are blurred. These images show that dispersion does be-
come finer and velocities are significantly enhanced when residence
With the inlet and the outlet concentrations, equilibrium data, time is reduced. Both these factors contribute to enhancement in
volume of the microchannels and flow rates known, Eqs. (1) and overall volumetric mass transfer coefficients with reduction in resi-
(4) can be used to calculate the overall volumetric mass transfer co- dence time as shown in Fig. 4.
efficient (KLa). To calculate the Reynolds number, average physical Fig. 6 shows the flow pattern in the split and recombine
properties of the phases, defined by Eqs. (5), (6) are used microchannel for O/A = 1/1. At 32 s residence time parallel flow
with intermittent droplets in both the layers is observed. As the res-
Qo Qa idence time is reduced to 6.6 s, annular flow is observed which per-
ρmix ¼ ρo þ ρa ð5Þ
Qo þ Qa Qo þ Qa sists when residence time is further reduced to 5 s. Annular flow
−1 will have more interfacial area than parallel flow causing overall volu-
1 Qo 1 Qa metric mass transfer coefficients to increase with reduction in residence
μ mix ¼ þ ð6Þ
μo Q o þ Q a μa Q o þ Q a time.
De ρmix U Fig. 4 shows that for the same residence time, KLa values for the
Re ¼ ð7Þ
μ mix serpentine microchannel, are, in most cases, more than KLa values
in the split and recombine microchannel. However, it will be useful
To calculate U and De the cross section of the reaction channels of to compare KLa values in the microchannels for the same Reynolds
serpentine microchannel and the cross section of the main channel number and average velocity also. Figs. 7 and 8 show this compari-
of split and recombine microchannel are used. Physical properties son. As seen from Fig. 7, for the same Reynolds number KLa values
of the equilibrated phases used in calculation of Reynolds number are higher in the split and recombine microchannel than in the ser-
are taken from the literature (Bart and Slater, 2001) and given in pentine microchannel. For the same residence time, the flow rate
Table 1. for the serpentine microchannel having 250 μL volume is more
than the flow rate for the split and recombine microchannel which
4. Results and discussion has much smaller volume. This causes the average velocity, hence
KLa which is directly related to the velocity, to be more in the serpen-
4.1. Effect of residence time on KLa tine microchannel, when comparison is done for the same residence
time. However, for the same Reynolds number, the velocities will be
Fig. 4 shows the variation of the overall volumetric mass transfer higher in the split and recombine microchannel due to its equivalent
coefficient with residence time for different O/A ratios. As can be diameter being smaller. This causes the K La values, for the same
seen, the overall volumetric mass transfer coefficient increases Reynolds number, to be the higher in the split and recombine
with reduction in residence time. In these experiments, residence microchannel than in the serpentine microchannel.
time is reduced by increasing flow rate. With reduction in residence Fig. 8 shows that for the same average velocity KLa values are higher
time, the flow rate increases causing kinetic energy, the only source in the split and recombine microchannel. Comparison for the same aver-
of energy available for generating dispersion, to increase. Increased age velocity seems to be a better way of comparing the performance of
kinetic energy makes the dispersion finer. Thus specific interfacial the microchannels as the average velocity is directly related to the kinet-
area increases with reduction in residence time. Also on reducing ic energy (the energy responsible for dispersion) and the film coeffi-
residence time, velocities prevailing inside the microchannel in- cients inside the microchannel. With kinetic energy and velocity the
crease causing film mass transfer coefficients to increase. With same, difference in the KLa values can solely be attributed to the geome-
both specific interfacial area and film mass transfer coefficients in- try of the microchannel. Therefore, among the two microchannels com-
creasing with reducing residence time, overall volumetric mass pared here, the split and recombine microchannel is found to be better.
transfer coefficient also increases with reducing residence time, as Although for the same residence time overall volumetric mass transfer
seen in Fig. 4. coefficients are higher in the serpentine microchannel than in the split
To confirm that dispersion indeed becomes finer on reducing resi- and recombine microchannel, if the later is made longer to have volume
dence time, few imaging experiments, in which flow patterns inside equal to the serpentine microchannel it is likely to show higher overall
the microchannels were observed using a high speed image acquisition volumetric mass transfer coefficients than the serpentine microchannel
system, were performed. The flow patterns observed in the serpentine even when the comparison is done on the basis of the same residence
microchannel and split and recombine microchannel for O/A = 1/1 time. The reason for better performance of split and recombine
are shown in Figs. 5, 6 respectively. Fig. 5 shows that when residence microchannel can be attributed to chaotic advection and improved
time is 98 s, long slugs with a few large droplets in between are ob- mixing in both phases due to multi-lamination. Our finding is similar
served. When residence time is reduced to 33 s, length of the slugs to that of an earlier study in which a split and recombine micromixer
reduces and droplets become smaller indicating that dispersion is found to perform better than a T-junction microchannel for a mass
transfer controlled liquid–liquid two-phase reaction (Guan et al., 2008).
Table 1
Physical properties of the phases. 4.3. Effect of O/A ratio on KLa
3
Phase Density (kg/m ) Viscosity (mPa·s)
Variation of KLa with Reynolds number for different O/A ratios for
Organic phase 758.6 1.37 the serpentine microchannel is shown in Fig. 9. In these experiments
Aqueous phase 998.5 0.958
the organic phase is the dispersed phase. As O/A ratio is increased the
58 M. Darekar et al. / Hydrometallurgy 144–145 (2014) 54–62
0.1 0.1
O/A = 4/1 O/A = 2/1
0.01 0.01
KLa (1/s)
KLa (1/s)
0.001 0.001
Serpentine Serpentine
Split & recombine Split & recombine
0.0001 0.0001
1 10 100 1000 1 10 100 1000
Residence Time (sec) Residence Time (sec)
0.1 0.1
O/A = 1/1 O/A = 1/2
0.01 0.01
KLa (1/s)
KLa (1/s)
0.001 0.001
Serpentine Serpentine
Split & recombine Split & recombine
0.0001 0.0001
1 10 100 1000 1 10 100 1000
Residence Time (sec) Residence Time (sec)
0.1
O/A = 1/4
0.01
KLa (1/s)
0.001
Serpentine
Split & recombine
0.0001
1 10 100 1000
Residence Time (sec)
Fig. 4. Variation of overall volumetric mass transfer coefficient with residence time for different O/A ratios.
holdup of the dispersed phase increases causing specific interfacial causing dispersion to become coarser and specific interfacial area
area to increase with O/A. Also with increase in O/A ratio, the flow to reduce. With these two factors affecting the specific interfacial
rate and hence dispersing power of the continuous phase reduces area in opposite ways, on increasing O/A ratio the specific interfacial
area may not change monotonically. Similarly, when O/A ratio is re-
duced, the dispersed phase holdup reduces causing specific interfa-
cial area to reduce. However, with reduced O/A ratio, flow rate and
hence dispersing power of the continuous phase increases causing
dispersion to become finer and specific interfacial area to increase.
Again with the two factors affecting the specific interfacial area in
opposite ways, specific interfacial area and hence K La may not
change monotonically as O/A is reduced.
On changing the O/A ratio, flow pattern may also change as
shown in Fig. 10. While for O/A = 1/4 loosely packed large droplets
are observed, for O/A = 1/1 closely packed slug and small droplets
are observed. For O/A = 4/1 annular flow with occasional tiny slug
in the outer layer is observed. If the flow pattern changes on chang-
ing the O/A ratio, the relationship between specific interfacial area
and the O/A ratio may become even more complex. The complex re-
lation between the O/A ratio and the specific interfacial area reflects
in the complex relation between the O/A ratio and KLa as shown in
Fig. 9. As can be seen in Fig. 9, the overall volumetric mass transfer
coefficients are the highest for O/A = 4/1 and then for O/A = 2/1.
For other O/A ratios there is no clear trend. Thus at higher O/A ratios
(2/1 and 4/1) the increase in holdup due to increase in O/A ratio seems to
5 sec 33 sec 98 sec
be dictating KLa values. While for low O/A ratios (1/1, ½ and ¼) some-
Fig. 5. Flow patterns in the serpentine microchannel for O/A = 1/1. times holdup appears to dominate and sometimes fineness of dispersion
M. Darekar et al. / Hydrometallurgy 144–145 (2014) 54–62 59
appears to dominate. Similar trends of variation of KLa with O/A ratio volumetric mass transfer coefficient as the dependent variable to ob-
were observed for the split and recombine microchannel. tain correlations for both the microchannels. Selection of average ve-
locity is based on the fact that it is directly related to the overall
4.4. Correlations for KLa volumetric mass transfer coefficient through its effect on the specific
interfacial area and film mass transfer coefficients. Velocity has been
There are several studies on liquid–liquid extraction in microchannels used as an independent variable in the correlations reported in a re-
in which experimental data have been used to obtain correlations for cent study which compares different types of microchannels (Kashid
overall volumetric mass transfer coefficients. The correlations reported et al., 2011a). In the present study, LABFit (Silva and Silva Cleide,
in these studies are usually not dimensionless. Here we use average 1999-2010) was used to obtain the correlations for overall volumetric
velocity and O/A ratio as the independent variable and overall mass transfer coefficient. The best fit correlations for the serpentine
0.1 0.1
O/A = 4/1 O/A = 2/1
0.01 0.01
KLa (1/s)
KLa (1/s)
0.001 0.001
Serpentine Serpentine
Split & recombine Split & recombine
0.0001 0.0001
1 10 100 1000 1 10 100 1000
Re (-) Re (-)
0.1 0.1
O/A = 1/1 O/A = 1/2
0.01 0.01
KLa (1/s)
KLa (1/s)
0.001 0.001
Serpentine Serpentine
Split & recombine Split & recombine
0.0001 0.0001
1 10 100 1000 1 10 100 1000
Re (-) Re (-)
0.1
O/A = 1/4
0.01
KLa (1/s)
0.001
Serpentine
Split & recombine
0.0001
1 10 100 1000
Re (-)
Fig. 7. Variation of overall volumetric mass transfer coefficient with Reynolds number for different O/A ratios.
60 M. Darekar et al. / Hydrometallurgy 144–145 (2014) 54–62
0.1 0.1
Serpentine O/A = 4/1 Serpentine O/A = 2/1
Split & recombine Split & recombine
0.01 0.01
KLa (1/s)
KLa (1/s)
0.001 0.001
0.0001 0.0001
0.01 0.1 1 0.01 0.1 1
U (m/s) U (m/s)
0.1 0.1
Serpentine O/A = 1/1 Serpentine O/A = 1/2
Split & recombine Split & recombine
0.01 0.01
KLa (1/s)
KLa (1/s)
0.001 0.001
0.0001 0.0001
0.01 0.1 1 0.01 0.1 1
U (m/s) U (m/s)
0.1
Serpentine O/A = 1/4
Split & recombine
0.01
KLa (1/s)
0.001
0.0001
0.01 0.1 1
U (m/s)
Fig. 8. Variation of overall volumetric mass transfer coefficients with average velocity for different O/A ratios.
microchannel and the split and recombine microchannels are given −4 O 4
K L a ¼ −1:2092 10 þ 0:051939U−0:075017U ð9Þ
by Eqs. (8) and (9) respectively. A
0.030
0.025
KLa (1/s)
0.020
0.015
1/4 4/1
0.005
2/1
0.000
0 50 100 150 200 250
Re (-)
O/A = 4/1 O/A = 1/1 O/A = ¼
Fig. 9. Effect of O/A ratio on the overall volumetric mass transfer coefficient for the serpen-
tine microchannel. Fig. 10. Flow patterns in 250 μL serpentine microchannel at residence time of about 33 s.
M. Darekar et al. / Hydrometallurgy 144–145 (2014) 54–62 61
0.035
Experimental
microchannel and split and recombine microchannel are within the
0.030 range of KLa values calculated for the hollow fiber contactor. With
KLa (1/s) - correlation
Table 2
Comparison of KLa values in microchannels and hollow fiber contactor for Zn–D2EHPA system.
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Liu, H., Huang, J., Sun, D., Lin, L., Lin, W., Li, J., Jiang, X., Wu, W., Li, Q., 2012. Microfluidic
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Acknowledgment microreactors. Chem. Eng. J. 215–216, 876–885.
Ren, J., He, S., Ye, C., Chen, G., Sun, C., 2012. The ozone mass transfer characteristics and
ozonation of pentachlorophenol in a novel microchannel reactor. Chem. Eng. J. 210,
The authors acknowledge the analytical support received from LSS, 374–384.
ChED, BARC. Silva, W.P., Silva Cleide, M.D.P.S., 1999–2010. LAB fit curve fitting software (nonline-
ar regression and treatment of data program) V 7.2.47 (1999–2010). online,
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