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Extraction Column*

By Guangsheng Luo** , Hangbo Li, Weiyang Fei, and Jiading Wang

In a pulsed sieve plate extraction column (PSEC) with a 150 understanding of the performance of the liquid-liquid extrac-

mm diameter, a dynamic process and a conventional tion columns, more than three models concerned with axial

concentration profile measurement process were used to mixing have been developed. All these models require an

evaluate the mass transfer and axial mixing coefficients for the accurate knowledge of both axial mixing and mass transfer

30% TBP (in kerosene)/nitric acid/water system. The mass parameters, together with additional information on drop size

transfer direction was from the continuous phase to the and distribution. In the past, much research has been

dispersed phase. Experimental results indicated that the much dedicated to the understanding of these parameters [36].

simpler dynamic process could be reliably used in place of the Concentration profile measurements coupled with diffu-

concentration profile measurement process. A simple equa- sion/backflow models are widely used to simultaneously

tion, (HTU)OC = KUC/f(1f)n, was derived to calculate the determine these parameters. Both Spencer et al. [7] and Rod

true height of transfer unit (HTU)oc (independent of et al. [8] have described numerical procedures based on matrix

column diameter) from the experimental mass transfer data formulations by means of which the various parameters can be

and hydrodynamic characteristics in PSEC with different determined from measured concentration profiles along a

diameters while the mass transfer rate of the extraction system column. But experiments for measurement of concentration

is controlled by the drop side resistance. The derivation of profiles of both phases under steady-state conditions are

calculated values from experimental data was up to 20%. material and time consuming, especially in large experimental

The equation was tested in several other differential type columns [9]. In order to avoid these difficulties, Rod et al. [10]

extraction columns. It was shown that this equation could also worked out an unsteady process using the solute to be

be used to predict the true height of transfer unit. extracted as the tracer and a stationary continuous phase in a

vibration plate column in diameter of 40 mm. Lei et al. [11]

worked out a similar dynamic process with a flowing

1 Introduction continuous phase in a pulsed sieve plate column 40 mm in

diameter equipped with dispersion-coalescence plate

Liquid-liquid extraction has been recognized as a powerful cartridge. Since Smoot and Babb [12] studied the true

separation technique for almost a century. Today liquid-liquid height transfer unit, many works have been related to this

extraction has been developed to be one of the most useful field. Some effective factors were explained and a few

separation processes. The knowledge concerning the design complicated correlations have been developed to calculate

and performance of extraction columns, however, is still far the mass transfer parameters [1315]. Until now, it was still

from satisfactory. The cause lies mainly in the complex necessary to find the relationship between the hydrodynamics

behaviors of the hydrodynamics and mass transfer perfor- and mass transfer.

mance [1,2]. The aim of this work is to reconfirm the dynamic process

A great deal of experimental effort has been expended suggested by Lei et al. [11] in a standard type pulsed sieve plate

principally for the purpose of evaluating column performance column of 150 mm in diameter with 30% TBP (in kerosene)/

for design and scale-up. In the design of liquid-liquid nitric acid/water as the working system. Starting from the

extraction columns, an important step is to determine the definition of the true height of transfer unit, a simple

column height in the case of differential contactors. In early equation derived from two phases flow and mass transfer will

design procedures, ideal plug-flow conditions were assumed in be tested.

both phases to estimate the height or number of stages

required for the desired separation. However, it is now widely

accepted that axial mixing dispersion in one or two phases can 2 Experimental

lead to considerable deviations from the ideal plug-flow

situation, resulting in an increase in the height or number of 2.1 Material and Experiments

stages required to achieve the design specification. With the

Experiments were carried out in an air pulsed glass column

of 150 mm diameter and effective height of 2 m equipped with

41 sieve plates of the standard type. A switch valve was located

[*] Some results in this paper were presented at ISEC'96.

[**] G. S. Luo , H. B. Li, W. Y. Fei, and J. D. Wang, Department of Chemical

port was located just below the bottom plate to collect the

Engineering, Tsinghua University, Beijing 1000084, China. raffinate samples while the experiments of dynamic process

Chem. Eng. Technol. 21 (1998) 10, WILEY-VCH Verlag GmbH, D-69469 Weinheim, 1998 0930-7516/98/1010-0823

0930-7516/98/0101-00823 $ 17.50+.50/0

$ 17.50+.50/0 823

Full Paper

equal distances along the 2 m effective height of the column.

Samples of the two phases were taken simultaneously from

each port for concentration profile measurements under each

given operation condition. For experiments of dynamic

process under each operating condition, a limited but

adequate amount of the aqueous phase, nitric acid of 0.5

mol/L, and the organic phase, 30% TBP (in kerosene), were

circulated in the column to achieve mutual saturation and

equilibrium between the two phases. The aqueous feed was

then switched to 2 mol/L nitric acid for about 5 min as a tracer

signal and the flow was switched back again to the dilute acid

stream. The raffinate samples were taken every minute at the

same time and analyzed by titration for concentration of nitric

acid to construct the response curve. A typical response curve

of the raffinate is shown in Fig. 1. For experiments of

concentration profile measurement, 2 mol/L nitric acid and

30% TBP (in kerosene) flowed countercurrent until steady Figure 2. Sketch of experimental setup.

state was attained and then samples for the two phases were

Table 1. The physical properties of the system at 25 C.

taken simultaneously by the 8 samplers which were specially

designed [9] to guarantee the purity of each phase. A sketch of

the experimental setup is shown in Fig. 2.

and 21 sets by the steady-state concentration profile meas-

urement process.

2.2 Modeling and Algorithm

Based upon the diffusion model and material balance, the

volumetric replacement method.

equations for the dynamic process were established over

All the materials were purchased from a Beijing chemical

differential elements of the column with a cross-section area S

plant. TBP and nitric acid were chemical grade. Water was

and total effective height H, while operated under constant

deionized. They were used directly without any purification.

superficial velocities Uc and Ud at any given pulse amplitude

The physical properties of mutual saturated aqueous and

and frequency. They are shown as Eqs. (2) and (3).

organic phase are listed in Tab. 1. Operating conditions are

shown in Tab. 2.

(2)

The equilibrium relationship in mol/L of the present system

was represented as1)

(3)

x* = 4.14y + 0.114, (y 0.06 mol/L). (1)

where

.

1) List of symbols at the end of the paper.

824 WILEY-VCH Verlag GmbH, D-69469 Weinheim, 1998 0930-7516/98/0101-00824 $ 17.50+.50/0 Chem. Eng. Technol. 21 (1998) 10

Full Paper

.

(12)

For solution of these equations, a differential equation in

mean implicit form was applied with suitable time step and Combining Eqs. (812), Eq. (13) is obtained.

distance step. A set of differential equations were obtained

and parameters Pex, Pey, and Noc were evaluated by Marquadt (13)

optimization with the measured raffinate response data [16].

Eqs. (2) and (3) were applied to the steady state while dx/dt0 From the derivation of this equation, one can see that the

and dy/dt0 and the measured concentration profiles were constant K varies with the physical properties of the working

used to evaluate the three parameters. system and the configuration of the column. It can be written

as K = K1 /C

(HTU)oc, and where C is the constant in Eq. (11) for calculation of U0,

which varies only with the configuration and the type of

(4) column. Validity of this simple equation was tested with data

of various systems and a few columns types as described in the

Where the interfacial area per unit volume, a, can be next section.

expressed as

4 Results

(5)

For the dynamic process, 63 sets of evaluated parameters

If the equilibrium line is linear, the overall mass transfer were obtained from experimental results under the operating

coefficient of the drops based on a continuous phase will be conditions mentioned. For the concentration profile meas-

obtained by using the two-film model, i.e., the addition of two urement process (steady-state process), 21 sets of data were

individual resistances of the dispersed and continuous phases. obtained. Fig. 3 shows an example of the simulated response

curve (from the estimated parameters) compared with the

(6) measured values. Here only the rising part of the response

curve was plotted to simplify the calculation process and to

For the systems, the mass transfer is controlled by the mass save time. Concentration profiles simulated by the evaluated

transfer coefficient of the drop phase; Eq. (6) is written as parameters from the dynamic experimental data are com-

pared with that measured profiles under steady-state condi-

(7) tions; Fig. 4. shows that the simulated curves fit the measured

data very well.

Eqs. (5) and (7) are substituted in Eq. (4), then

(8)

by Handlos and Baron [17].

(9)

columns, Ut is replaced by the slip velocity Us.

(10)

calculating U0 and n based on their works on four extraction

systems in a pulsed sieve plate column. Figure 3. Comparison of experimental and simulated dynamic curves.

Chem. Eng. Technol. 21 (1998) 10, WILEY-VCH Verlag GmbH, D-69469 Weinheim, 1998 0930-7516/98/0101-00825 $ 17.50+.50/0 825

Full Paper

Eq. (13) was tested in the same kind of pulsed sieve plate

extraction columns equipped with standard sieve plate

cartridge. For this work, values of K = 25.86, K1 = 13.45, and

C = 0.52 were obtained from the properties of the system. Data

from some other sources were processed with Eq. (13), while

Eq. (12) was used to calculate the exponent n. Results are

listed in Tab. 3.

reliably used in place of the steady-state method and it has the Data listed in Tab. 3 were performed in the steady state and

advantages of saving time and material. Furthermore, for the work of Qin et al. [20] was done in a pulsed sieve plate

experiments using the dynamic process, the organic phase can column of annular type 100 mm in diameter. Because the

be recycled without reprocessing. columns have a standard structure, the same constant C was

The evaluated data of Noc were converted to (HTU)oc and used in all these works. From results in Tab. 3, it can be

correlated using the simpler form of Eq. (13), which has the concluded that the constant K calculated directly by the above

form equations is almost the same as the correlated value from the

experimental data. As shown in Fig. 6, comparison of the

(15) evaluated (HTU)oc with the calculated data from Eq. (13) is

plotted with a standard deviation of 9.16% and a maximum

The exponent value n = 1.48 was obtained from Eq. (12). To deviation of 23.56%. This result also indicated that Eq. (13)

simplify Eq. (15), we chose n = 1.5. The calculated values of has a generality in the calculation of (HTU)oc although the

(HTU)oc from Eq. (15) are compared with the experimental working systems and the diameter of the columns were

data of both the dynamic and steady-state methods as shown different.

in Fig. 5 with a standard deviation of 11.0% and a maximum

deviation of -20.06%. One can see the dynamic process

method can be reliably used to evaluate the mass transfer

characteristics. This result also shows that the simpler Eq. (13)

can be used to calculate the data of (HTU)oc easily. A

relationship between the flow of the two phases and mass

transfer performance has been found with this equation.

5 Conclusions

axial mixing parameters worked successfully in a pulsed sieve

plate column of 150 mm diameter. Experimental and

Figure 5. Comparison of evaluated values and calculated data of (HTU)oc. computational results in this work show that it is a reliable

826 WILEY-VCH Verlag GmbH, D-69469 Weinheim, 1998 0930-7516/98/0101-00826 $ 17.50+.50/0 Chem. Eng. Technol. 21 (1998) 10

Full Paper

but less material and time consuming method compared with s [mN/m] Interfacial tension

the concentration profiles measurement process. Its applica- tx, ty [] Constants in equations

tion would facilitate the fundamental research work in large

experimental extraction columns.

The simple equation derived to calculate the true height Subscripts

of the transfer unit has a more fundamental basis than those

from pure empirical equations. It can be used in different c Continuous phase

kinds of extraction columns for many extraction systems d Dispersed phase

having a mass transfer rate controlled by drop side resistance.

The relationship system having mass transfer performance is

apparent in the equation. Acknowledgment

Received: January 9, 1997 [CET 880]

We acknowledge the support of the National Natural

Science Foundation of China for this work.

Symbols used

A [m]

Pulsed amplitude References

C []

Constant

[1] Lo, T. C.;. Baird, M. H. I; Hanson, C., (Eds.) Handbook of Solvent

d3,2 [m]

Sauter mean diameter of droplets

Extraction, Wiley-Interscience, New York 1983.

Ec [m2/s]

Diffusion coefficient of solute in [2] Thornton, J. D. (Ed.) The Science and Practice of Liquid-Liquid

continuous phase Extraction, Oxford University Press, Oxford 1992.

[3] Sleicher, C.A., Axial Mixing and Extraction Efficiency, AIChE J. 5 (1959)

Ed [m2/s] Diffusion coefficient of solute in p. 145.

dispersed phase [4] Sleicher, C.A., Entrainment and Extraction Efficiency of Mixer-Settlers,

f [1/s] Pulsed frequency AIChE J, 6 (1960) p. 529.

[5] Korchinsky, K. J., A Dispersion Entrainment Model for Liquid-Liquid

g [m/s2] Acceleration of gravity Extraction Column Performance Prediction, Chem. Eng. Sci. 43 (1988)

H [m] Effective height of column p. 349.

[6] Chartres, R. H.; Korchinsky, W. J., Modeling of Liquid-Liquid Extraction

(HTU)oc [m] Height of transfer unit

Columns: Predicting the Influence of Drop Size Distributions, Trans. I.

k [m/s] Mass transfer coefficient Chem. E. 53 (1975) p. 247.

koc [m/s] Overall mass transfer coefficient [7] Spencer, J. L.; Steiner, L.; Hartland, S., Model-Based Analysis of Data

from Countercurrent Liquid-Liquid Extraction Processes, AIChE J. 27

based on continuous phase (1981) p. 1008.

K, K1 [] Constants in equations [8] Rod, V.; Fei, W.; Hanson, C., Evaluation of Mass Transfer and Backmixing

m [] Equilibrium constant Parameters in Extraction Columns from Measured Solute Concentra-

tions, Chem. Eng. Res. Des. 61 (1983) p. 290.

n [] Constant in equation [9] Luo, G. S., A Study on Mass Transfer and Axial Mixing in Pulsed Sieve

Noc, (NTU)oc [] Number of transfer unit Plate Extraction Column, Ph.D. Thesis, Tsinghua Univ., Beijing, P.R.

China 1993.

Pe [] Peclet number

[10] Rod, V.; Hancil, J., Prediction of Extractor Performance from Tracer

S [m2] Cross-section area of column Experiments with Stationary Continuous Phase, Proc. ISEC'86. DE-

t [s] time CHEMA, Munchen, II-57 (1986).

[11] Lei, X.; Qian, Y.; Fei, W. Y.; Wang, J. D., Evaluation of Mass Transfer and

U [m/s] Superficial velocity Axial Mixing Parameters in Pulsed Sieve Plate Extraction, Proc. ISEC'86.

Uo [m/s] Characteristic velocity DECHEMA, Munchen. III-215 (1986).

Us [m/s] Slip velocity [12] Smoot, L.; Babb, A. L., Mass Transfer Studies in a Pulsed Extraction

Column, I & E Fundamentals 1 (1962) p. 2.

Ut [m/s] Terminal velocity [13] Prvcic, L. M., Axial Dispersion and Backmixing Studies in Pulsed

x [mol/L] Solute concentration in continuous Perforated Plate Columns, Ph.D. Thesis, University of Melbourne 1987.

[14] Gao, G. D., Mass Transfer Characteristic in Pulsed Sieve Plate Extraction

phase

Column, MS Thesis, Tsinghua University, Beijing, China 1965.

x* [mol/L] Equilibrium concentration of [15] Tung, L. S.; Luecke, R. H., Mass Transfer and Drop Sizes in Pulsed Plate

solute in the continuous phase Extraction Columns, Ind. Eng. Chem. Process Des. Dev. 25 (1986) p. 664.

[16] Marquardt, D. W., An Algorithm for Least Squares Estimation of Non-

y [mol/L] Solute concentration in the linear Parameters, J. Soc. Ind. App. Math. 11 (1963) p. 431.

dispersed phase [17] Handlos, A. E.; Baron, T., Mass and Heat Transfer from Drops in Liquid-

Liquid Extraction, AIChE J. 3 (1957) p. 127.

[18] Zhu, S. L.; Zhang, B. Q.; Shen Z. Y.; Wang, J. D., A Study on Two-phase

Flow Characteristics in Pulsed Sieve Plate Column for Liquid-Liquid

Greek symbols Extraction, J. Chem. Ind. and Eng. (China) 1 (1982) p. 1.

[19] Qian, Y., Evaluation of Mass Transfer in Pulsed Sieve Plate Column, Ph.D.

Thesis, Tsinghua Univ., Beijing, 1987.

a [m2/m3] Interfacial area [20] Qin, W., Mass Transfer and Axial Mixing in Annual Pulsed Sieve Plate

f [%] Dispersed phase hold-up Column, Ph.D. Thesis, Tsinghua Univ., Beijing, 1992.

[21] Wang, Z. W., Mass Transfer Characteristics in RDC, MS Thesis, Tsinghua

m [mPaS] Viscosity Univ., Beijing, 1991.

r [kg/m3] Density [22] Fei, W. Y.; Wen, X. M.; Fang, S. H.; Mao, H., A High Efficiency Packing for

Dr [kg/m3] Density difference Liquid-Liquid Extraction, Proc. ISEC'93. SCI, London (1993) p. 49.

Chem. Eng. Technol. 21 (1998) 10, WILEY-VCH Verlag GmbH, D-69469 Weinheim, 1998 0930-7516/98/0101-00827 $ 17.50+.50/0 827

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