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A Simplified Correlation of Mass Transfer in a Pulsed Sieve Plate


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

on the feed line to introduce the tracer acid and a sampling


[*] 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

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were being performed. Eight sampling ports were situated at


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.

Table 2. Operating conditions.

In all, 63 sets of data were obtained by the dynamic process


and 21 sets by the steady-state concentration profile meas-
urement process.

Figure 1. Response curve of the raffinate.


2.2 Modeling and Algorithm

The dispersed phase hold up was estimated by the


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.

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Noting that in Eqs. (2) and (3) represents (11)

.
(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

3 Simplified Equation to Calculate (HTU)oc (14)

Eq. (4) is the definition of true height of transfer unit,


(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)

The mass transfer coefficient in the drop phase was derived


by Handlos and Baron [17].

(9)

For drop swarms in two phase flow in the extraction


columns, Ut is replaced by the slip velocity Us.

(10)

Zhu et al. [18] gave two semi-empirical equations for


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.

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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.

Table 3. Application of Eq. (13).

Figure 4. Comparison of calculated and measured profiles.

These results indicate that the dynamic process could be


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.

Figure 6. Comparison of evaluated (HTU)oc with the calculated data.

5 Conclusions

The dynamic process for evaluation of mass transfer and


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

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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 []
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