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Chemical Engineering and Processing 48 (2009) 224–228

Contents lists available at ScienceDirect

Chemical Engineering and Processing:


Process Intensification
journal homepage: www.elsevier.com/locate/cep

Stage efficiency of Hanson mixer-settler extraction column


Meisam Torab-Mostaedi a,b,∗ , Jaber Safdari b , Mohammad Ali Moosavian a ,
Mohammad Ghannadi Maragheh b
a
School of Chemical Engineering, College of Engineering, University of Tehran, P.O. Box 11365-4563, Tehran, Iran
b
Nuclear Science Research School, Nuclear Science and Technology Research Institute, P.O. Box 14155-1339, Tehran, Iran

a r t i c l e i n f o a b s t r a c t

Article history: Stage efficiency of a pilot plant Hanson mixer-settler extraction column with seven stages was measured by
Received 6 October 2007 using toluene-acetone-water system. The experiments were carried out for both mass transfer directions.
Received in revised form 11 March 2008 The effects of agitation speed, flow ratio, total throughput and solute concentration on stage efficiency
Accepted 23 March 2008
were investigated and found to be significant. The comparison of investigated column with some other
Available online 29 March 2008
type of extractors showed that the stage efficiency of this column is high, while its throughput is small.
Finally an empirical correlation was proposed for prediction of stage efficiency and very good agreement
Keywords:
between experimental data and calculated values was obtained.
Stage efficiency
Hanson extraction column © 2008 Elsevier B.V. All rights reserved.
Throughput
Axial mixing
Mass transfer direction

1. Introduction tors used different methods to decrease axial mixing by coalescing


small drops in the section between stages. Scheibel [5] set up the
A mixer-settler extraction column (vertical mixer-settler) has mixing part and the packing part alternately to promote drop coa-
the advantages of the horizontal mixer-settlers with high stage effi- lescence in the packing part. For the same purpose, Steiner et al.
ciency and low interstage mixing, while requiring a small ground [6] used a three dimensional lattice as a partition of the mixing
area and no additional pipes and pumps [1]. Mixer-settler extrac- stages. Horvath and Hartland [1] achieved high stage efficiency
tion columns are widely used in different industries especially with a mixer-settler extraction column in which the interstage mix-
in rare earth metal separating and hydrometallurgy processes. To ing was extremely small, while the throughput of the column was
separate species like rare earth elements which have chemical also small. Takahashi et al. proposed a mixer-settler extraction col-
properties similar to one another, the extraction plant needs a large umn (MS column) in which a mixer and a settler were in vertical
number of stages; hence it is desirable to develop an extraction with arrangement in each stage, and showed that both the throughput
high stage efficiency. From industrial point of view, an extraction [7] and stage efficiency [2] increased with agitation speed. Extrac-
column of high performance which achieves a large throughput tion behavior of rare metals within a MS column has been analyzed
and high stage efficiency is desirable [2,3]. Mechanical agitation with stage efficiency based on hydrodynamics and mass transfer
can promote stage efficiency due to the large interfacial area with within the column. Since the hydrodynamics in one stage of MS col-
small dispersed drops. As drop size decreases with agitation speed, umn is independent of that in other stage, they can be expressed
however, the relative velocity between the dispersed phase and quantitatively by several correlations [8]. The Wirz column has a
continuous phase decreases, which makes the throughput small [4]. mixer at the center of the column and a large settling space around
Moreover, axial mixing, which lowers the stage efficiency, becomes the mixer [9]. In the case of aqueous dispersion, Bailes and Stitt
appreciable at high agitation speed. Reduction or even elimination [10] used an electrostatic coalescence to obtain stable operation
of the axial mixing is the key to higher stage efficiency and is there- under vigorous agitation. Schweitzer [11] proposed a rectangular
fore of interest in column design. Coalescing small drops between mixer-settler tower with horizontal arrangement of the mixer and
stages may be effective to increase the relative velocity between settler in each stage, i.e., each stage in the mixer-settler extrac-
two phases and it can also reduce backmixing. Many investiga- tor was piled up in vertical direction. These partitioning between
stages can reduce the axial mixing and result in the enhancement
of separation efficiency.
∗ Corresponding author. Tel.: +9821 22832637; fax: +9821 44216659. In this paper, the stage efficiency of Hanson mixer-settler extrac-
E-mail address: mmostaedi@aeoi.org.ir (M. Torab-Mostaedi). tion column is measured for both mass transfer directions. The

0255-2701/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.cep.2008.03.010
M. Torab-Mostaedi et al. / Chemical Engineering and Processing 48 (2009) 224–228 225

Table 2
Physical properties of liquid system at 20 ◦ C

Physical property Continuous phase Dispersed phase


3
Density (kg/m ) 994.4–995.7 864.4–865.2
Viscosity (mPa s) 1.059–1.075 0.574–0.584
−3
Interfacial tension (N/m) 27.5–30.1 × 10

respond to the arithmetic-mean concentrations of the continuous


and dispersed phases at inlet and outlet of the column.
The system was allowed to reach steady state, which necessi-
tated three changes of column volume. The interface of two phases
was kept fixed by using an optical sensor. The samples were col-
lected at the inlet and outlet of the first, forth and seventh stages
and they were analyzed by GC. The photographs of the droplets
were taken during steady state conditions and used to determine
Sauter mean droplet size. The holdup of dispersed phase was mea-
sured by rapid withdrawal of 100 ml sample from the mixers. In
Fig. 1. A schematic diagram of three stages showing the flows of light and heavy
all experiments, two phases were mutually saturated before the
phases.
experiments by repeated circulation through the column. Agita-
tion speed was varied between 200 and 440 rpm, because for this
effects of agitation speed, total throughput, flow ratio of the dis- column design and high interfacial tension system, agitator speeds
persed phase to continuous phase and solute concentration on the lower than 200 rpm were not found to be of practical significance
stage efficiency are investigated and an empirical correlation is and for speeds higher than 440 rpm the column operated unstable.
proposed for prediction of stage efficiency.
3. Results and discussion
2. Experimental
The performance of a separation device with well-defined stages
A pilot plant Hanson mixer-settler extraction column is used in can be expressed in terms of stage efficiency. The stage efficiency
these experiments. Two sides of column are made of stainless steel EOy based on the concentration of organic phase is defined as fol-
and the other sides are made of Plexiglas. The column consists of lows:
seven stages with 12 cm height; a schematic diagram of three stages
(yn − yn−1 )
is given in Fig. 1. Dispersion of the organic phase in each stage is EOy = (1)
(yn∗ − yn−1 )
achieved by means of a 6.5 cm diameter six-bladed turbine agitator.
In each stage, the light and heavy phases are mixed in the mixing where yn∗ = (mxn ) is the organic phase concentration in equilibrium
zone for providing initial contact, after that the unstable emulsion with the aqueous phase of nth stage. The mean value of stage effi-
is transferred to a settler zone through the port ‘A’. This port is ciency was obtained by averaging the values obtained in the first,
located in the middle of a dividing wall and in front of it a vertical forth and seventh stages.
plate ‘B’ is placed to decrease the effect of centrifugal rotation in the For the investigated mixer-settler column, the stage efficiency is
settler so that the drop coalescence is improved. In the settler zone, strongly dependent on the agitation speed. Fig. 2 shows the effect
the phases are separated, so the heavy phase is led to the previous of rotor speed on stage efficiency for both mass transfer directions.
stage mixer through a weir ‘C’ and the light phase is led to the next As it is shown in this figure, at low speeds, the stage efficiency is
stage mixer through a port ‘D’. The column geometry is listed in low due to inadequate mixing, resulting in low holdups and large
Table 1. drops (low interfacial area). The stage efficiency increases with
The liquid system that studied was toluene-acetone-water as increasing of agitation speed and reaches a maximum of 53.7% for
recommended by the E.F.C.E. [12]. Distillated water was used as c → d mass transfer direction at speed of 361.5 rpm and a maxi-
continuous phase and technical grade of toluene was used as dis- mum of 70.8% for the opposite direction at speed of 385 rpm. After
persed phase. Physical properties of the liquid–liquid system used
in the experiments are listed in Table 2. It should be noted that
in mass transfer condition, a degree of uncertainty surrounds the
estimation of physical properties, since these vary not only with the
inlet solute concentrations but also along the column. In the present
work, the values of physical properties have been assumed to cor-

Table 1
Geometrical characteristics of the column used

Column components Dimensions (cm)

Mixer dimensions (length × width) 13 × 13


Settler dimensions 26 × 13
Stage height 12
Column height 172
Number of stages 7
Column active volume 55.36 (l)
Agitator diameter 6.5
Blade height 1.3
Inner port dimension 13 × 4 Fig. 2. Effect of agitation speed on stage efficiency.
226 M. Torab-Mostaedi et al. / Chemical Engineering and Processing 48 (2009) 224–228

Fig. 4. Effect of flow ratio on stage efficiency.

Fig. 3. Effect of throughput on stage efficiency.

of dispersed drop increases with decrease in residence time. As


having reached to its maximum, it falls with further increase in effects of flow rate on stage efficiency, the contribution of holdup
agitation speed. The fall in stage efficiency is probably a result of a is positive and that of residence time is negative, for the interfacial
substantial decrease of mass transfer coefficients for small drops, area is proportional to the holdup and inversely proportional to the
behaving as rigid spheres, present in the mixer. This phenomena drop size. The former may be compensated by the latter and the
cause molecular diffusion to govern the system and consequently stage efficiency is not affected by throughput in the case of c → d
mass transfer rate decreases. It can be also observed that the transfer. But for mass transfer direction d → c, as it is shown in Fig. 3,
stage efficiency of this column is affected by axial mixing between for lower throughputs (higher residence times), higher stage effi-
stages. When the rotor speed becomes more than 400 rpm, cir- ciency are obtained. For this mass transfer direction, the residence
culation of continuous phase and the entrainment of dispersed time of dispersed drops is small, so the effect of decreasing resi-
drops in continuous phase cause a decrease in stage efficiency, dence time is higher than that of increasing dispersed phase holdup
because the flow channels of the continuous and dispersed phases and consequently the stage efficiency decreases with increase in
are not separated in the present mixer-settler column. More- throughput.
over, in this range of rotor speed, the centrifugal rotation in the The effect of flow ratio on stage efficiency is given in Fig. 4.
settler become significant and a large number of the dispersed According to this figure, the stage efficiency increases with an
drops passes through the settler without coalescing and conse- increase in flow ratio of dispersed phase to continuous phase for
quently a decrease in stage efficiency and maximum throughput both mass transfer directions. The holdup of dispersed phase and
follows. the drop diameter also increases due to the decrease in residence
Also, it was found that mass transfer direction has a significant time with increase in flow ratio, but it was observed that interfa-
effect on stage efficiency. As it can be seen in Fig. 2, the stage effi- cial area increases by increasing the flow ratio of dispersed phase
ciency in the case of d → c transfer is obviously higher than that to continuous phase because the holdup effect becomes more
in the opposite direction. During solute transfer from the contin- predominant than the drop size one and consequently the stage
uous phase to the dispersed phase, solute equilibrium is quickly efficiency will increase.
established between the drops and the continuous phase between The effect of solute concentration on stage efficiency is given in
them, whereas solute transfer continues over the rest of the drop Fig. 5 for continuous to dispersed phase mass transfer direction. It
surface. This creates an interfacial tension gradient which opposes can be observed that the stage efficiency in runs with higher solute
the forces causing drainage in the film, thus reducing coalescence.
During solute transfer in the opposite direction, the increased con-
centration of the solute in the film between the two drops creates
an interfacial tension gradient which complements the drainage
forces, enhancing coalescence of the drops. So the higher values of
stage efficiency in the case of d → c transfer are a result of increased
mass transfer rates in drops of bigger sizes due to the presence of
oscillations created by coalescence between the droplets which is
enhanced by the Marangoni effect [13,14].
The effect of throughput on stage efficiency is given in Fig. 3.
According to this figure, the stage efficiency varies little with
throughput for mass transfer direction c → d, while throughput
has significant effect on stage efficiency of opposite direction. For
mass transfer direction c → d, it is found that the dispersed phase
holdup increases with increase in flow rate of dispersed phase and
decreases with increase in flow rate of continuous phase, but the
effect of Qd is larger than that of Qc , i.e., the holdup may increase by
increasing total throughput at constant phase ratio. The residence
time of dispersed phase decreases with increase in Qd and the size Fig. 5. Effect of solute concentration on stage efficiency.
M. Torab-Mostaedi et al. / Chemical Engineering and Processing 48 (2009) 224–228 227

Fig. 7. Comparison of experimental values of stage efficiency with calculated ones.


Fig. 6. Comparison of extractor performance. System toluene- acetone-water,
Ud /Uc = 1.5.
defined as follows:

1  |Predicted value − Experimental value|


concentrations is higher than others with lower solute concen- NDP

trations. The interfacial tension decreases with increasing solute AARE =


NDP Experimental value
concentration [13], so for the same rotor speed, throughput and i=1
mass transfer direction, a larger interfacial area per unit volume is
in which NDP is the number values of data points. The value of AARE
created, resulting higher stage efficiency. For this reason, it is essen-
in the predicted values of stage efficiency by using correlations (2)
tial for scale-up purposes that the range of solute concentration be
and (3) from experimental data is 9.39%. Fig. 7 shows the agreement
kept similar.
between experimental and calculated data, using correlations (2)
A comparison of the separation performance of the present
and (3).
mixer-settler column with some other type of extractors is shown
in Fig. 6. The criterion is, as suggested by Pratt and Stevens [15],
4. Conclusions
the number of theoretical stages per unit of length against total
volumetric throughput of both phases.
The stage efficiency of the investigated mixer-settler extraction
This plot is of value in providing a rapid comparison of the rel-
column increased with agitation speed and reached a maximum,
ative areas of application of the various extractor types, despite
but after having reached to its maximum, it decreased with fur-
being based on data for single system, viz. toluene-acetone-water
ther increase in agitation speed, because axial mixing became
at a phase ratio of 1.5. As it is shown in this plot, the present mixer-
significant for high agitation speed. It was observed that the stage
settler column reached values of between 3.65 and 6.4 NTS/m at
efficiency varied little with total throughput for mass transfer direc-
low total throughputs. So it can be concluded that the present
tion c → d while it decreased with increase in total throughput
mixer-settler extraction column has high stage efficiency while its
for the opposite mass transfer direction. The results showed that
throughput is small.
the stage efficiency increased by increasing flow ratio of dispersed
The experimental data of stage efficiency are correlated in terms
phase to continuous phase. Also, the stage efficiency increased with
of dimensionless numbers Re and Fr for both mass transfer direc-
increase in solute concentration, so it is important for scale-up pur-
tions by using least square method, as follows:
poses that the range of solute concentration be kept similar. The
EOy = 1.417 Re0.101 Fr −0.822 Re > 10 (2) comparison of present mixer-settler column with some other type
of extractors showed that the stage efficiency of this column is high,
EOy = 0.068 Re0.874 Fr 0.222 Re < 10 (3) while its throughput is small. Finally an empirical correlation was
proposed for stage efficiency and very good agreement between
where:
calculated and experimental results was obtained.
d32 Vslip c
Re = (4)
c Appendix A. Nomenclature
g
Fr = (5)
dR N 2
A cross section area of the mixer (m2 )
in which d32 is Sauter mean diameter, N is rotor speed, dR is agitator d32 Sauter mean drop diameter (m)
diameter and Vslip is slip velocity between two phases. Since the dR impeller diameter (m)
dispersed and continuous phases flow concurrently through the EOy stage efficiency based on organic phase concentration (–)
mixer, the slip (or relative) velocity, Vslip , between the phases is Fr Froude number (g/dR N) (–)
obtained as follows [16]: g acceleration due to gravity (m/s2 )
Qd Qc m distribution ratio (–)
Vslip = − (6) N rotor speed (rps)
A A(1 − )
Q flow rate (m3 /s)
The average absolute value of the relative error, AARE, is used Re Reynolds number (d32 Vslip c /c ) (–)
to compare the predicted results with experimental data. This is Vslip slip velocity (m/s)
228 M. Torab-Mostaedi et al. / Chemical Engineering and Processing 48 (2009) 224–228

x mass fraction of acetone in continuous phase (–) [4] V.J. Kirou, L.L. Tavlarides, J.C. Bonnet, C. Tsouris, Flooding, holdup and drop size
y mass fraction of acetone in dispersed phase (–) measurements in a multistage column extractor, AIChE J. 34 (1988) 283–292.
[5] E.G. Scheibel, Fractional liquid extraction, Chem. Eng. Prog. 44 (1948) 681–690.
y* equilibrium mass fraction of acetone in dispersed phase [6] L. Steiner, E. Von Fisher, S. Hartland, Performance of a liquid–liquid extrac-
corresponding to continuous phase (–) tion with enhanced coalescence lattice, AIChE Symp. Ser. 80 (No. 238) (1984)
130–138.
[7] K. Takahashi, H. Nakashima, S. Nii, H. Takeuchi, Maximum throughput in mul-
Greek letters tistage mixer-settler extraction column, Kagaku Kogaku Ronbunshu 19 (1993)
 viscosity (Pa s) 440–445.
 density (kg/m3 ) [8] K. Takahashi, A.A. Abdeltawab, S. Nii, T. Yajima, F. Kawaizumi, Extraction of rare
earth metals with a multistage mixer-settler extraction column, Chem. Eng. Sci.
 holdup of dispersed phase (–) 57 (2002) 469–478.
[9] W. Wirz, German Patent 1918225, 1968.
[10] P.J. Bailes, E.H. Stitt, Column liquid contacting with vigorous agitation balanced
Subscripts by electrostatic coalescence, Part I. Intensified coalescence-redispersion, Chem.
c continuous phase Eng. Res. Des. 65 (1987) 514–523.
d dispersed phase [11] P.A. Schweitzer, Hanson Mixer-Settler Handbook of Separation Techniques
for Chemical Engineering, 3rd ed., McGraw-Hill, New York, 1997, pp. 461–
469.
Superscripts [12] T. Mı́šek, R. Berger, J. Schroter, Recommended systems for liquid extraction
* equilibrium value studies, European Federation of Chemical Engineering, Institution of Chemical
Engineers, Rugby (1978).
[13] C. Gourdon, G. Casamatta, Influence of mass transfer direction on the oper-
References ation of a pulsed sieve-plate pilot column, Chem. Eng. Sci. 46 (1991) 2799–
2808.
[1] M. Horvoth, S. Hartland, Mixer-settler extraction column: mass transfer effi- [14] A. Kumar, S. Hartland, Mass transfer in a Kühni column, Ind. Eng. Chem. Res. 27
ciency and entraiment, Ind. Eng. Chem. Process Des. Dev. 24 (1985) 1220– (1988) 1198–1203.
1225. [15] H.R.C. Pratt, G.W. Stevens, Selection, design, pilot-testing and scale-up of extrac-
[2] K. Takahashi, S. Nii, K. Nakanishi, H. Takeuchi, Stage efficiency of mixer-settler tion equipment, in: J.D. Thornton (Ed.), Science and Practice in Liquid–Liquid
extraction column, J. Chem. Eng. Jpn. 26 (1993) 715–719. Extraction, Oxford University Press, 1992, pp. 491–502.
[3] L.M. Rincon-Rubio, A. Kumar, S. Hartland, Characterization of flooding in Wirz [16] J.D. Thornton, Spray liquid-–liquid extraction columns: prediction of limiting
extraction column, Can. J. Chem. Eng. 71 (1993) 844–851. holdup and flooding rates, Chem. Eng. Sci. 5 (1956) 201–208.

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