Chemical Engineering and Processing 111 (2017) 7–13

Contents lists available at ScienceDirect

Chemical Engineering and Processing:

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

Determination of slip and characteristic velocities in reactive

extraction with experiments in the Oldshue-Rushton column and
presence of samarium and gadolinium metals
Rezvan Torkaman* , Mehdi Asadollahzadeh, Meisam Torab-Mostaedi
Material and Nuclear Fuel Cycle Research School, Nuclear Science and Technology Research Institute, P.O. Box: 11365-8486 Tehran, Iran

A R T I C L E I N F O A B S T R A C T

Article history:
Received 22 September 2016 The slip and characteristic velocities of the reactive system (samarium, gadolinium and D2EHPA) were
Accepted 23 October 2016 investigated in the pilot plant Oldshue-Rushton extraction column. The experiments were carried out at
Available online 26 October 2016 the extraction and stripping stage. The influences of the agitation speed, dispersed as well as continuous
phase velocity were studied. An increase in dispersed phase velocity led to the increase of the slip velocity
Keyword: while it decreased with agitation speed and continuous phase velocity. More buoyancy and faster upward
Oldshue-Rushton extraction column movement of larger drops accelerate the slip velocity in the stripping condition as compared with the
Rare metals case of extraction condition. The experimental data were compared with the proposed correlations by
Slip velocity
Asadollahzadeh et al., and the related deviation was within 26% from these equations. Therefore, the
Characteristic velocity
modified correlations for prediction of slip and characteristic velocities were proposed with the
experimental data and the data from the physical systems in the literature.
ã 2016 Elsevier B.V. All rights reserved.

1. Introduction Among these technologies, solvent extraction is the most

Rare earth elements play a significant role in the manufacture of
catalysts, fluorescent lamps, permanent magnets, super alloys,
medicines and several other appliances [1–3]. Samarium is one of
the rare earth elements that is applied for the manufacture of Sm-
Co permanent magnets [2]. It is also used as a samarium iodide
catalyst for speeding up decomposition of plastics, dechlorination
of PCBs and ethanol dehydration [4]. The other rare earth element
is gadolinium whose organic compounds are used for magnetic
resonance imaging. It can reduce relaxation times and thereby
enhance signal intensity with its high magnetic moment [5]. It is
also added to optical glasses meant for use in the optical fibers. It
has a potential application as the functional material in magnetic
refrigeration [6]. In addition, samarium, gadolinium, and dyspro-
sium oxides are used in the nuclear industry in the radiation
shielding [7]. The large primary and secondary sources of rare
earth elements in the world have led to considerable research into
suitable extraction and separation processes including ion
exchange [8], solvent extraction [9,10] and chemical precipitation
[11] to produce individual rare earth elements.
* Corresponding author.
E-mail address: rtorkaman@aeoi.org.ir (R. Torkaman).
widely used technique in which commercially available extractant,
such as D2EHPA [12,13]; HEH/EHP [14]; Cyanex 272 [15]; Cyanex
301 [16]; Cyanex 302 [17]; Cyanex 923 [18]; Aliquat 336 [19] and
sec-octyl phenoxy acetic acid [20] for extraction and separation of
samarium from gadolinium, are utilized.
Mixer–settler contactors are used as the standard extraction
equipment in the rare earths processing plant. The actual
equipment arrangement depends on the nature of the feed and
product requirement [9,21]. However, large space requirement,
large solvent inventory, long residence time, and poor sealing of
the system can be listed as the disadvantages of mixer-settlers. To
achieve better flexibility and extraction efficiency, agitated
extraction columns such as rotating disc column (RDC) [22,23],
asymmetric rotating disc column (ARDC) [24], Kühni column [25],
Scheibel column [26] and Oldshue-Rushton column [27,28] were
scrutinized in the light of the solvent extraction processes.
Nonetheless, the applications of the Oldshue-Rushton extractor
were not observed in the literature for rare earth separation and
purification from the primary and secondary resources.
Information on hydrodynamic parameters in the Oldshue-
Rushton column such as droplet size, holdup, slip and characteris-
tic velocities is important for the scale up and the design of this
extraction column. The slip velocity controls the mass transfer
coefficient when a solute is transferred between the two phases,

http://dx.doi.org/10.1016/j.cep.2016.10.018
0255-2701/ã 2016 Elsevier B.V. All rights reserved.
8 R. Torkaman et al. / Chemical Engineering and Processing 111 (2017) 7–13

solvent (di-(2-ethylhexyl) phosphoric acid (D2EHPA)) from

Nomenclature
Aldrich, was employed as an extractant. Commercial salts (Sm
(NO3)3
6H2O, Gd(NO3)3
6H2O, Middle East Ferro Alloy Company,
d32 Sauter mean diameter (m)
99.9% purity) were used as rare earth metals in the experiments.
di Drop diameter (m)
The aqueous phase solutions were prepared by dissolving these
dr Rotor diameter (m)
salts in the deionized water.
g Acceleration due to gravity (m s2)
N Rotor speed (s1)
2.2. Apparatus
R Reaction parameter () in Eq. (7)
Vc Continuous phase velocity (m s1)
The samarium and gadolinium content in the aqueous stream
Vd Dispersed phase velocity (m s1)
was measured using ICP-AES spectroscopy and a Perkin-Elmer
Vk Characteristic velocity (m s1)
model 5500 inductively coupled plasma atomic emission spec-
Vs Slip velocity (m s1)
troscopy. The density measurements were performed using the
pycnometer method. The viscosity data were obtained by DVI-
Greek Letters
Prime viscometer and the interfacial tension data were measured
Dr Density difference between phases (kg m3) by a Krüss tensiometer. Table 1 shows the physical properties of
m Viscosity (Pa s) the two phases.
r Density (kg m3)
s Interfacial tension (N m1) 2.3. Pilot plant Oldshue-Rushton column
w Dispersed phase holdup ()
The schematic diagram of the pilot plant Oldshue-Rushton
Subscripts
column is shown in Fig. 1 and the general characteristics of the
c Continuous phase
column are also listed in Table 2.
d Dispersed phase
The extraction column consisted of a cylindrical shell and a
baffled stator. Moreover, it was equipped with 6-blade impellers
with accurate speed control. The main section was made of Pyrex
glass, 113 mm I.D, and the height of the column was 700 mm. The
value of the free area was 25% at the nine stages as compared with
the column cross-sectional area. The stirrer was located in the
while the holdup together with the drop size determines the center of each compartment with 6-blade impellers 50 mm in
interfacial area for mass transfer conditions [29,30]. Another diameter and these impellers were driven by an electric motor via a
important hydrodynamic parameter is the characteristic velocity variable gearbox. The two phases were introduced counter-
requiring a good knowledge so as to predict the flooding time and currently in the column through the circular perforated distrib-
maximum volumetric capacity of an extraction column [31]. utors with the light phase entering from the bottom, and the heavy
No information for the design and scale up of Oldshue-Rushton phase from the top of the column. The interface was maintained at
columns in reactive extraction conditions is available in the the required level by means of an optical sensor as previously
literature. In this research work, the effects of operating described [32].
parameters such as rotor speed, dispersed and continuous The aqueous phase of the reactive test system consists of water,
superficial velocities on the slip velocity and the characteristic samarium nitrate, gadolinium nitrate and nitric acid, whereas the
velocity in reactive extraction conditions with the presence of solvent kerosene and the cation exchanger D2EHPA form the
samarium, gadolinium and D2EHPA extractant were investigated. organic phase. D2EHPA is a surface-active component and extracts
The previous correlations in the literature for the physical samarium and gadolinium via an interfacial reaction as follows:
systems without reaction condition were studied and the þ
M3þ
ðaÞ þ 3H2 A2 $MH3 A6ðoÞ þ 3HðaÞ ð1Þ
comparison between them and the experimental results was
evaluated in this column. In addition, the modified correlations for 3+
where H2A2 and M represent the D2EHPA and samarium or
prediction of slip and characteristic velocities were proposed in gadolinium, respectively. The bars in Eq. (1) indicate the
this research work. components in the organic phase.
In extraction runs, the nitrate solution of samarium and
2. Experimental gadolinium with 500 ppm concentration, adjusted at 1.5 pH in
water and 0.12 M D2EHPA diluted with kerosene were used as the
2.1. Materials continuous phase and dispersed phase, respectively.
In stripping runs, nitrate solution with 0.1 M concentration and
Commercial grade of kerosene was used as a diluent in the the loaded organic phase of samarium and gadolinium with
extraction process without further purification and the organic

Table 1
Physical properties of the phases used in the system, at 25  C.

Properties r(kg m-3) m(103 kg m1 s1) s(103 N/m)

Extraction Stage Continuous phase 1005 0.9216 22.1
Dispersed phase 789 1.2587
Stripping Stage Continuous phase 995 0.9204 23.5
Dispersed phase 795 1.2674
 R. Torkaman et al. / Chemical Engineering and Processing 111 (2017) 7–13 9

Fig. 1. Schematic diagram of the pilot plant Oldshue-Rushton column.

500 ppm concentration were used as the continuous phase and 2.3.2. Determination of drop size
dispersed phase, respectively. The droplets dispersed in the continuous phase are not the
The start-up of Oldshue-Rushton column was far from flooding same size and as a result, there is a distribution of drop size. In
conditions. Conditions became steady, as evidenced by a constant general, the Sauter mean diameter is used to indicate the droplet
interface level, after three or four column volumes of operation diameter and it is defined as Eq. (2), and n and i represent nth and ith
depending on the phase flow rates and rotor speed. To examine the values.
steady state condition in the Oldshue-Rushton column, the outlet
X
n
3
concentrations of samarium and gadolinium in the aqueous phase ni di
were measured every 15 min. To make sure that the validity and i¼0
d32 ¼ ð2Þ
reproducibility of the results were satisfactory, all of the experi- X
n
2
ni di
ments were carried out three times.
i¼0

2.3.1. Determination of holdup

There are several techniques that can be used for measuring the
dispersed phase holdup, including shutdown, hydrostatic, and
direct sampling. In this research work, the shutdown method was
used to measure holdup. When the conditions were steady, the
inlet and outlet valves and agitation were shut at the same time
and the volume of the dispersed phase was obtained by noting the
height difference at the interface level.
Table 2
Technical description of the Oldshue-Rushton column.
Parameter
Column height (H)
Column internal diameter (Dc)
Diameter of the rotor
No. number of stages
Height of the stages
Fractional free cross section area (%)
3. Result and discussion
3.1. Variation of holdup at extraction and stripping stages
The results from the variation of holdup with the continuous
and dispersed phase velocity are shown in Fig. 2a and b. An
increase in the dispersed phase velocity led to the increase in the
amount of the dispersed phase holdup at constant volume.
Therefore, the increase in the holdup was observed from Fig. 2a.
The increment of the drag force between the droplets and the
continuous phase with increasing the continuous phase velocities
led to the increase in the residence time and the dispersed phase
holdup (Fig. 2b).
The effect of the rotor speed on the holdup at the extraction and
stripping stages is shown in Fig. 3. The drop size was inversely
related to the rotor speed. An increase in rotor speed led to the
Size
decrease in drop diameter owing to the intensification of drops
700 mm breakage. Therefore, the increase in the dispersed phase holdup
113 mm
50 mm
was observed at the extraction and stripping stages. The effect of
9 mm solute and its direction of transfer at the extraction and stripping
67 mm stages were observed in Figs. 2 a, b and 3 . The presence of a solute
25 tends to lower the interfacial tension between the two immiscible
 10 R. Torkaman et al. / Chemical Engineering and Processing 111 (2017) 7–13
Fig. 2. Variation of the dispersed phase holdup with (a) dispersed phase velocity
(Qc = 36 L/h, N = 180 rpm); (b) with continuous phase velocity (Qd = 36 L/h, N = 180
rpm).
liquids. At the extraction stage, solute transfer occurs from the
aqueous phase to the dispersed phase. The solute concentration in
the draining film between the two adjacent drops will be higher
Fig. 3. Variation of the dispersed phase holdup with rotor speed (Qd = Qc = 36 L/h).
Fig. 4. Variation of the slip velocity with rotor speed (Qd = Qc = 36 L/h); and the
comparison of data by Asadollahzadeh et al. correlation.
than in the surrounding aqueous phase. In the stripping stage, the
concentration will be correspondingly lower. The gradients of
interfacial tension will inhibit coalescence at the extraction stage
and will accelerate to produce larger drops at the stripping stage.
Therefore, the reduction in the dispersed phase holdup was
observed at the stripping stage in comparison of the extraction
stage.
3.2. Variation of slip velocities at extraction and stripping stages
The slip velocity under conditions of countercurrent flow is
defined as the sum of the linear actual velocities of the dispersed
and continuous phases, as follows:
Vd Vc
Vs ¼ þ ð3Þ
f ð1  fÞ
The effect of operating parameters on the slip velocity by using
Eq. (3) is shown in Figs. 4–6 . As can be seen, the slip velocity
decreases with the increase in rotor speed. The drop size diameter
will be smaller because of more turbulence generated at the higher
Fig. 5. Variation of the slip velocity with dispersed phase velocity (Qc = 36 L/h,
N = 180 rpm); and the comparison of data by Asadollahzadeh et al. correlation.
 R. Torkaman et al. / Chemical Engineering and Processing 111 (2017) 7–13 11

concentration of extractant at the interface will decrease so that

the drops will rise faster. However, the mass transfer in the physical
extraction systems inhibits Marangoni effects which reduce the
internal circulation of the drop and, therefore, decrease the drop
velocities, likewise.
Accurate prediction of the slip velocity for reactive extraction
conditions is very difficult for the lack of experimental data in the
published literature and the empirical correlations for predicting.
Asadollahzadeh et al. recommended forward the following
correlation (Eq. (4)) for calculation of slip velocities in the
Oldshue-Rushton extraction column for the three physical systems
(Toluene-Water, n-Butyl acetate-Water, n-Butanol-Water) [33].
" #0:36        0:23
V slip mc N2 dr rd 9:75 md 1:44 V c 0:24 mc g0:25
¼C 1þ
s g rc mc Vd r0:25
c s 0:75
" #0:11
V 4d rc
ð4Þ
gs
Fig. 6. Variation of the slip velocity with continuous phase velocity (Qd = 36 L/h,
N = 180 rpm); and the comparison of data by Asadollahzadeh et al. correlation. The comparison of the experimental results with the predicted
values by Eq. (4) is shown in Figs. 4–6. The percentage of the
average absolute value of the relative error between the present
agitation speed, consequently, the slip velocity decreases (Fig. 4). It experimental data and model by Asadollahzadeh et al. was 26.53%.
is observed from Fig. 5 that the slip velocity slightly increases with This model is based on physical systems without reaction
the increase in the dispersed superficial velocity. However, it condition, but the experimental data were obtained from the
decreases slightly with the increase in the continuous superficial reaction between samarium, gadolinium with D2EHPA extractant.
velocity (Fig. 6). As seen in these figures, the value of the slip Because of errors in these equations to accurately predict
velocity for the extraction stage is smaller than that of the stripping results, the modified correlations with consideration of reaction
stage. Continuous to dispersed transfer showed the smaller drop conditions are proposed as follows:
size and larger holdup than the reverse direction, so the smaller " #0:357      1:037
V slip mc N2 dr rd 5:277 V c 0:698 mc g0:25
values of slip velocities for this direction were expected. To better ¼ K1 1þ
illustrate the variation in the slip velocities, the publication data
s g rc Vd r0:25
c s 0:75
reported by Asadollahzadeh et al. [33] for the physical systems ð5Þ
were compared with the experimental data in Table 3. It is
The effect of the reactive extraction condition through the
observed from Table 3 that the slip velocities in the reactive
column is shown by constant parameter (K1) in the above equation.
extraction system were larger than those in the physical systems.
The values of this parameter for the reactive extraction systems
The variation is related to the interfacial active properties of
and physical systems are presented in Table 4.
D2EHPA. The surface active component (samarium, gadolinium
and D2EHPA) if takes part in the surface reaction, the

Table 3
Variation in the slip velocities in the physical systems (publication data by Asadollahzadeh et al.) and reactive system (experimental data) (Qc = Qd = 36 L/h).

System Aqueous phase Organic phase Solute transfer N Slip Velocity (mm/s)
(rpm)
no c to d d to c
mass
Physical Water Toluene Acetone 140 11.25 10.74 12.57
system 160 10.23 9.76 11.43
180 9.40 8.98 10.51
200 8.72 8.33 9.75
Water n-Butyl acetate Acetone 140 8.32 7.94 9.29
160 7.56 7.22 8.45
180 6.95 6.64 7.77
200 6.45 6.16 7.21
Water n-Butanol Acetone 140 6.17 5.89 6.89
160 5.61 5.36 6.27
180 5.16 4.92 5.76
200 4.79 4.57 5.35
Reactive Solution of samarium and D2EHPA and Kerosene Complex of D2EHPA, samarium and 140 – 24.62 –
system gadolinium gadolinium 160 – 20.47 –
180 – 16.78 –
200 – 14.28 –
Nitric acid D2EHPA, Kerosene and complex of D2EHPA, samarium Samarium and gadolinium 140 – – 26.43
and gadolinium 160 – – 23.05
180 – – 18.43
200 – – 16.07
12 R. Torkaman et al. / Chemical Engineering and Processing 111 (2017) 7–13
Table 4
Values of K1 in Eq. (5) for physical systems and reactive extraction system.
System direction of mass transfer K1
Physical system no mass 0.01842
c to d transfer 0.01753
d to c transfer 0.01978
Reactive system c to d transfer 0.02671
d to c transfer 0.03154
Fig. 7 shows the calculated values of the slip velocity from
Eq. (5) versus the experimental values of slip velocity. It is observed
that the experimental and calculated data are close enough to the
bisector line, which corroborates the correlation preciseness.
3.3. Variation of characteristic velocities at extraction and stripping
stages
There are many correlations for relating slip velocity to the
continuous phase holdup (1  w). Four main types of correlations
were proposed by Gayler and Pratt [34], Richardson and Zaki [35],
Misek [36] and Letan and Kehat [37].
The simplest equation for calculation of characteristic velocity
suggested by Gayler and Pratt for w < 0.2 and is given as follows
[34]:
V slip ¼ V k ð1  fÞ
The dependence of the characteristic velocity on the rotor speed
is shown in Fig. 8. As can be seen, the characteristic velocity is
inversely proportional to the rotor speed.
To compare the experimental data for the characteristic velocity
with the literature data, the correlation proposed by Asadollahza-
deh et al. [33] was used. The percentage of the average absolute
value of the relative error between the present experimental data
and the correlation presented by Asadollahzadeh et al. correlation
was 40.67%. Therefore, the modified correlation for better
Fig. 7. Comparison of experimental results with calculated values of the proposed
correlation for slip velocity by using Eq. (5).
AARE
7.36%
10.06%
8.07%
6.56%
5.71%
Fig. 8. Variation of characteristic velocity with rotor speed by using Eq. (6).
prediction was proposed as follows:
V k mc
¼ 0:00162
s " #0:567      0:037
N2 dr rc 1:170 md 1:833 mc g0:25
ð6Þ R ð7Þ
g Dr mc rc s
0:25 0:75
The effect of reactive extraction condition is defined by constant
parameter (R) in the above equation. The value of R equal to 12.405
was obtained from the experimental data at the extraction and
stripping stages for samarium and gadolinium separation.
This equation with a relative error of about 13.22% value has the
sufficient agreement with the experimental data in reactive
extraction conditions and the experimental data from Asadollah-
zaded et al. for physical systems.
4. Conclusion
We have been made a special study of liquid-liquid extraction
with chemical reaction in the pilot plant Oldshue-Rushton
extraction column. The extraction of samarium and gadolinium
from aqueous nitrate solution in the presence of D2EHPA as an
extractant and kerosene as a diluent was chosen for the study.
Hydrodynamic parameters such as slip velocity, characteristic
velocity and holdup were investigated under reactive extraction
conditions. The slip velocity at the stripping stage was higher than
that at the extraction stage because of the mass transfer direction,
Marangoni effect and the change in the interfacial tension. In
addition, the slip velocities in the reactive extraction system were
higher than those in the physical systems. The variation is related
to the interfacial active properties of D2EHPA. The modified
correlations for slip and characteristic velocities and reactive
system are presented for the first time and can be useful for high
accurate design of Oldshue-Rushton extraction column.
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