Comput. chem. Engng, Vol. 11, No. 2, pp. 177-185, 1987 0098-1354)87 $3.00 +0.00 Printed in Great Britain, All rights reserved Copyright © 1987 Pergamon Journals Lid DYNAMIC SIMULATION OF LIQUID-LIQUID OPERATIONS USING SIMPLE NON-LINEAR MODELS ‘A. M, SeRENot and T. F, ANDERSON Department of Chemical Engineering, University of Connecticut, Storrs, CT 06268, U.S.A. A. G. MEDINA Centro de Engenharia Quimica, Universidade do Porto, Faculdade de Engenharia, 4099 Porto Codex, Portugal (Received 10 January 1986; revision received 10 April 1986; received for publication 12 May 1986) ‘Abstract—In this paper a new method forthe dynamic simulation of multistage, multifeedliqui-tiquid extraction operations is described. Ths is achieved by the use of simplifed non-linear local models for the equilibrium representation of patially-misible three-component systems. ‘The probable transient response of the system to perturbations inthe input parameters is illustrated Whilst this has yet to be confirmed experimentally several examples have'been succesfully solved and the steadycstate results agree with thote reported by previous authors. a ‘The method, using a simulation language (GEMS), is stable and shows computer requirements well within the range of the steady-state algorithms commonly used for simulation of extraction units. Scope—Dynamic simulation of multistage equilibrium operations is becoming increesngly important in the areas of process control, particularly when dealing with batch operations Liqui-iquid extraction is an example of such operations but, unlike distillation, the composition profiles are in this case strongly dependent on the individual composition of each component present. ‘This is due to the fact that liquid-liquid equilibrium is very sensitive to phase compositions, leading to the need for sophisticated thermodynamic models for all the calculations involved With these complex models, the simultaneous integration of the differential system of equations which represents the mathematical model of the operation is dificult to achieve, or even impossible. The most widespread method to overcome this dificulty is the use of linearized forms of the equilibrium relationships. While this may work well with some diluted systems, itis a serious limitation with highly ‘non-ideal patially-miscible systems, common in the petrochemical industry, where all the components are \ present in significant amounts D The simultaneous numerical integration of the full system of model equations may, however, be accomplished through the use of simplified but non-linear local representations ofthe phaie-dstribution ratios ofall the components present. The concept has been presented in detail by Chimowitz eal. [] and is modified slightly here for the case of liquid-liquid systems. These non-linear functions involve & ‘ few empirical parameters, which are easy calculated by a liner least-squares approximation from a limited number of experimental ti-lines obtained in the region of compositions of interest tothe problem. Jn this work, these local models are explained and their performance assessed by comparing calculated tie-ins in simple equilibrium stage problems with the experimental ones. The ability of the local models, to simulate multistaged columns is ilustrated by the solution of two problems described inthe literature and in the study of the dynamic behaviour of a five-stage extractor used to purify acetic aid ‘Conclusions and Significance—This method, making direct use of experimental data, made it possible to reproduce and interpolate equilibrium data for nine ternary Type I and Type II'systems, lesding to reasonably accurate results ‘The data produced, extending over most of the two-phase region, have average percentage residuals ‘values of 1.40 and 10.4 for the mole fractions and distribution ratios, respectively. a little higher than, but of the same order of magnitude as, the ones reported to have been obtained using the UNIQUAC equation (2. ‘There are, however, systems for which only a narrow zone may be represented by each set of empirical parameters. This is the case for solutropic systems or, in more general terms, for systems in which the distribution ratios show extreme points in the range of compositions being considered. ‘The mathematical mode! for the single equilibrium stage was then used as the basis forthe development cof modes allowing the description of multiple staged units. The subsets of model equations for each stage were added together in a modular way, to form the complete system which represents the whole unit, These ‘models were used to simulate several columns with different configurations leading, in all cases to results in very good agreement with those reported from previous studies. This shows the soundness of the method as a steady-state simulation algorithm. To whom all correspondence should be addressed, presently at: Centro de Engenharia Quimica, Universidade do Porto, Faculdade de Engenharia, 4099 Porto Codex, Portugal. 7178 A.M, SeRENo et a [As the method is based on actual differential mass balances for each component, it also represents the probable dynamic behaviour when the integration is conducted under realistic assumptions and along a path where the approximate equilibrium representation used is able to produce accurate results. This is ‘extremely useful not only for the analysis of transient periods of time occurring during start-up and shutdown, but also for the evaluation of the effect of input disturbances on product specifications and for design and optimization of control schemes. INTRODUCTION Due to the increasing need for efficient use of thermal uid liquid extraction have recently become the object of intense research. The understanding and design of liquid extraction is considerably enhanced by computer simulation. Using a differential mathe- matical model which takes into ‘account the thermo- dynamic non-ideal behaviour of the systems involved, it is possible to simulate these operations on a digital computer. The first attempts on dynamic simulation of liquid-liquid extraction were reported in the late sixties and early seventies. Good reviews of these efforts were published by Pollock and Jobnson (3), Waggoner and Burkhart (4) and Wilkinson and Ingham [5 These early dynamic studies used linearized, forms of the model equations which were then integrated by Laplace transforms. This may be a serious limitation since the equilibrium relationships for highly non- ideal systems are seldom linear. In most cases, only the interphase transfer of one component, the solute, ‘was considered and a linear relationship between its equilibrium concentrations in both phases had to be assumed [6-8]. Dunn and Ingham (9] used MIMIC, a simulation program, for direct digital solution of the model developed by Jones and Wilkinson (8): A. linear equation was used to represent the distribution of solute between the two liquid phases. This way of representing the equilibrium relations constitutes an important limitation when dealing with complex ‘organic systems, very common in the petrochemical industry. In a recent article, Shacham et al. [10] have di cussed the advantages of the use of an equation- oriented (simultaneous) approach in the simulation of chemical engineering operations and plants. If a reliable integrating algorithm for systems of non- linear differential equations is available, a similar approach may be used with dynamic simulation; a non-linear differential model can then be solved simultaneously. Further, if the integration is sufficiently fast in terms of computer time, the intrin- sic stability of the method will make it a good steady-state simulator. ‘A general difficulty common to all simulation ‘methods is the need to include a numerical represent- ation of the physical and thermodynamic data for the systems involved. The experimental information on equilibrium data for liquid-liquid extraction is lim- ited. Therefore semi-theoretical models such as the NRTL [11], UNIQUAC [12] or UNIFAC [13] equa- tions are often used to extrapolate the available data. Recently, a table of UNIFAC group interaction contributions, specially developed for the prediction of liquid-liquid equilibrium, has been published (14). When these correlations, referred to in this paper as rigorous models, are used in the computer simulation of multistage operations, ‘they account for an im portant part of the total computer time [15]. This demand for computer time is particularly important in dynamic simulations of unit operations or in steady-state simulations based on quasi-dynamic or false-transient methods. To reduce the computational effort local models, may be used to represent the equilibrium data. This concept is presented in detail by Chimowitz et al. [1]. The local models are non-linear functions derived from sémi-theoretical correlations. With only a few empirical parameters they can represent equilibrium distribution ratios over a moderate range of com- position, temperature and pressure. These ideas are used in this work to simulate the dynamic behaviour of multistage, multifed, liquid- liquid extraction columns working with three- component systems. First of al, a differential mathe- matical model representing the’ single equilibrium stage is derived and the ability of the local concept to simulate simple equilibrium operations is verified. This simple model is then used as a building block in the simulation of several multistage column configurations, Results indicate that reliable dynamic simulations are feasible for, liquid-liquid extraction. Further- more, this method allows the evaluation of the dy- namic response of the equipment to perturbations in the operating conditions. The requirements of com- puter time are low enough to allow the method to be used for steady-state simulations. In ll cases, the solution of the system of equations is achieved using a simulation package called GEMS (General Equation Modelling System), previously developed at the University of Connecticut (16). This package uses Brandon's [17, 18] implicit single-step algorithm to perform the integration; the method proved to be fast and reliable, MODEL DEVELOPMENT FOR THE SINGLE EQUILIBRIUM STAGE In Fig. | a single-stage liquid-liquid equilibrium separation is shown. In this process, a feed withDynamic imulation of liquid-liquid operations 179 Light product MH Heavy product uy Fig. 1. Scheme of a single equilibrium unit. molar flow rate F, separates into heavy and tight streams, with molar flow rates L and V, respectively. The separation is conducted at constant temperature and pressure, and heat effects between phases are neglected. It is further assumed that each phase is always well-mixed and in thermodynamic equi- librium with the other; this is a commonly accepted simplification and the existing departures from this idealized situation are accounted for by some efficiency factor. With these assumptions the algebraic and differential equations representing the single equi- librium stage are Fe,—Vy,~ Lx, Kixy K=f¥s J 1c, Q) rae! @) and Dane @ In equations (1)-(4), x;, ¥, 2, are the mole fractions of component / in phase L, phase V and in the feed, respectively; H, and Hy are the molar holdups corte: sponding to phase L and phase V, respectively, while K, represents the interphase distribution ratio of the same component i. It is reasonable to consider that phase holdups remain essentially constant. Thus equation (1) may be rewritten as Fe,— Vy) Lx, = (Ay + yk) St + yx © The differential mass balance for component i, represented by equation (5), cannot be made explicit in x, before some functional relation is obtained for K,, In distillation, X, is essentially a function of tem- perature, depending weakly on compositions and even then almost entirely on the liquid phase. In extraction separations, however, distribution ra are strongly dependent on the mole fractions of all the components in both phases. Therefore, it is very difficult to simplify equation (5) and it is almost impossible to make it explicit in just one of the time derivatives if a rigorous model is used to represent the ‘equilibrium. This is probably the main reason why, in the simulation of these operations, the distribution ratios are usually assumed constant or made invari- ant from one iteration to the next, with subsequent re-evaluation of the K,s at the new estimated com- positions [8, 19, 20]. LOCAL, APPROXIMATIONS FOR EQUILIBRIUM RATIOS Chimowitz et al. [I] suggested a simplified repre- sentation for the interphase distribution ratios of ternary systems using non-linear local models, valid ‘over a moderate range of compositions. In this work the following general model was adopted: INK, =Lixie+L2y% +13, £21,233, © where Li, L2, L3 are empirical adjustable par- ameters; Xj and y,,- are the mole fractions of some reference components in phase L and V, respectively. Tt was found that in order to produce simplified differential equations the dominant components in each phase (diluent and solvent) should be chosen as reference components. Using equation (6), the time derivative of the distribution ratios may be calculated analytically to give dK, Xp Weer of 2 (Lise Het Lg ‘, =1,2,3. (2) With the time derivatives’ of liquid phase mole fractions denoted by: Equation (7) is substituted into equation (5) leading to the general equation representing the differential ‘mass balance of component i in the equilibrium unit: (H+ Hy Kix) = Fey— Vy, ~ Lx— Hy Ky (Ld Xe Xie + L2 Yee Piety 1,2,3. (9)180 A.M. SERENO et al, ‘Table 1. Dynamic model for singe equibrium uni Be, Bi ned ink Buber 0) ay 2) + Hy Kis = Fay = yy = Lay = 2Hy Ky (L224 + Ly) a3) wn Kin, 4, oe no Bs vs a) a ro) (Cette tm yo tne arnt « LaF yy Pay bay it HB) 2 Kalyx +L) a This equation, explicit in x}=dx;/d, is the basis for the mathematical model consisting of a set of ordinary differential equations, which is easily inte- grated by the implicit integration routine adopted in GEMS [16]. In the same manner, equation (1) may_ be made explicit in dy,/ds. This is used to represent the change in composition of the reference. component in phase V: Also, equation (4) may be substituted by a total ‘mass balance, as it proved more convenient in setting up the GEMS program. Table | outlines the complete dynamic model used to describe the single equilibrium stage separating a three-component feed. The parameters for the local models, Li,, L2,, L3,, i =1,2,3, are easily obtained by least-squares fitting of equilibrium ‘ratios predicted using one of the rigorous thermodynamic models or using direct ‘experimental data alone. This latter method is very convenient in practical applications and proved reasonably accurate. It was found that for most of the systems consid- ered, a single set of such parameters was able to represent the equilibrium distribution ratios through- out the entire two-phase region with the exception of a narrow strip close to the plait point of Type I systems (Fig, 2). For solutropie systems in which the distribution ratios show the existence of extreme points, the parameters have to be changed while moving along the two-phase region. GEMS program includes the empirical parameters for the local models together with the initial condi- tions. The simulation is started at a readily available initial condition corresponding to a true solution of the system of equations, for instance, one corre: sponding to the extremes of any known equilibrium tie-line. After a small period for starting and sta- bilizing the integration, the feed composition is changed by a step, which brings it to the specified one that corresponds to the mixture to be separated. The system is allowed to respond until no significant change with time is noticed. CALCULATION OF TIE-LINES IN SINGLE-STAGE EQUILIBRIUM PROBLEMS, The use of this method for single-stage equilibrium calculations is illustrated with examples involving both Type I and Type II liquid-liquid systems. These Acetic acid Water Fig. 2. Water/methyl isobutyl ketone/acetie acid system: experimental tie-lines (— miBK caleulated (©) equilibrium data, —— Interpolated tie-lines.Dynamic simulation of tiqui 18 Jiquid operations ‘n-Butanol 08. 02 Furfural Fig. 3. Furfural/water/n-butanol system: experimental tielines (~ Ref. 23]) and calculated (©) equilibrium data, ‘Table 2. Parameters for local models ‘Sytem Uy, 2, o, War 2s 1.462 Te MIBK 12.86 Holz 6.765 Acetic acid 339 L08ms 1.756 Furfural 4011 3393 as Water toe 1239 1713 Butanol 2s 91174 5.698 Benzene sass 3.059 0.2657 617 03885-02406 0.9382 0.1293 0.05061 two types of systems are believed to represent about 95% of all experimental data available [21] and certainly those of major industrial interest. As a first example, the systems. water/methyl ‘isobutyl ketone/acetic acid. and’ furfural/water/ n-butanol are studied, The results, reproducing the original tie-ines and some interpolated ones, are Table 3. Diforences between calculated results represented graphically in Figs 2 and 3. These also include the original experimental data of Sherwood et ai, (22) and Krupatkin and Glagoleva [23], re- spectively. In both cases the parameters are obtained by least-squares fitting of the experimental tie-lines, covering uniformly the two-phase region. Table 2 shows for both systems the values of the local parameters used in the calculations. Other ternary systems were tested using the same procedure. The agreement of the results with the experimental. data, expressed as average percentage residuals on, compositions and. distribution ratios were evaluated as suggested by Sorensen ef al. [21] and are shown in Table 3. APPLICATION TO THE DESIGN OF MULTIPLE-STAGE EXTRACTORS ‘A countercurrent multistage extraction column is schematically represented in Fig. 4, In general, a and experimental data (percentage deviations) This method Using UNIQUAC™ BR. SR System x x, bx x ‘enzenejwater/acee acid [24] 21 = = (rom UNIQUAG) 2 = = ‘Water MIBK acetic acid (22) 18 = = Benzene/fufural/-octane [25] 1s = = Waterl,12-richloroetane/acetone (26) 0.93 048 2 ‘Benzene/furfuraljeyciohexane (25) 1s 010 23 ‘Waterchloroform acetone (27) 28 076 54 Furfuralwatr/n-butanol (23) os7 = 2 FFurfuralwater/-butanol [23] 047 034 38 CCyclobexane/furfral/-octane [25] 01 0.09 ies Average 140 035, an "Ref.182 ALM, SERENO et al. ie Yory Table 4 Modified equations forthe mulplestage model (H+ Hy Kyi = Fit + Kye dort ly ka Vt Py = LyX = Ay Ki Xu Stoge 1 5 XC xuxh + yaya) 03) (fitter Fin + Vernet bse Lyons Bets Vis Fas, - = bx 1H 2 Pie ey, Bra baat HE Mb x Xj) + Layarjad a7) UB AV t br YB as) Ot Piya Ftp Yartaist bro yoy Yortiors Abt By Kaka Csxu Xj + L2syavia) 19) Stage may be specified and that correction factors for backmixing may be included. bus Sens ‘Only molar quantities have been considered so far. Fig. 4. Schematic representation of a multistage counter. ‘current extractor. solvent with a flow rate S is used to extract one of the ‘components from liquid feeds Ly and F,, producing product flows V; and P, and a raffinate product flow Ly. The mole fractions in the raffinate (phase L) and in the extract (solvent or phase V) leaving stage j are represented by x,, and ),; the feed F) has a com- position z,, and the product P, is withdrawn from the extract with a composition yj,. In addition to previous assumptions, it is consid- cred that the holdup is the same for each stage and that there is no backmixing between stages. These last two assumptions do not represent limitations of the method, but greatly simplify the formulation of the equations. With slight modifications to account for its posi- tion in the column and provision for the existence of intermediate feeds or product withdrawals, the set of equations of Table 1 may be used to represent each stage of the multiple unit. Table 4 shows the equa- tions which have to undergo stronger modifications. this modified set of equations the complete mathematical model for any column is easily formu- lated in a modular or “custom-built” manner. It is also apparent that individual holdups for each stage However, most of the experimental data are reported jn mass fractions. The conversion to mole fractions often introduces some skewness in the equilibrium iagram, which served to decrease the accuracy of the local models used, particularly close to the plait point. The method works equally well with mass units, if the parameters for the local models are regressed using compositions in mass fractions. Thi will usually enhance the ability of the local models to represent the equilibrium. ‘Two numerical examples illustrating this technique are described. Example 1 In the first example the extraction of cyclohexane from a mixture with n-heptane is simulated; furfural is the solvent in a 12-stage countercurrent column. This problem was proposed by Roche [28] and was also considered by Kehat and Ghitis [29]. The results obtained here are in exact agreement: with those of previous workers and are shown in Table 5. The local model parameters are calculated by fitting equilibrium tie-lines generated by the three-suffix Margules equation’ with the parameters given by Kehat and Ghitis (29) Example 2 The extraction of acetone is used here to illustrate “Table 5. Cycloherane extraction with furfural ‘Compositions Raffinate This Roche Kebat and This Component __Feed_Solvent__work [28] Gils (291 __work (28) Furun 00 10 00870087 087s 0876 07s Cycloherane 08 00 a.010 0010 0100s 0.108.106 sw Hepiane 02 00-0932 0933 ©0933 «alsa 018 Flow rates 100 665.77 142 666 604 103 660" sm 7542 Resa: obtained by: “This work, "Roche (28 “Kehat and Ghitie (29)Dynamic simulation of liquid-liquid operations os} 3 oz Mass fraction of acetone 183 Rottinare ‘Stage number Fig. 5. Concentration profiles for a two-feed nine-stage extractor. —, Ref. 30}; -—-, calculated. the simulation of a two-feed column [30], A 50% acetone-water solution is fed to the top of a nine- stage extractor at a rate of 100 Ib/h. An equal amount of a 25% acetone/75% water solution goes into its fourth stage. The acetone in these mixtures is to be extracted with I,1,2-trichloroethane at 50 Ib/h. Com- position and flow-rate profiles along the column at steady state are obtained. The results, represented in Fig. 5, are in agreement with Treybal’s [30] work. (COMPUTER CALCULATION OF THE. (DYNAMIC BEHAVIOUR ‘The previous examples have shown how a differential model coupled with a simplified repre- sentation of the equilibrium relationships could pro- duce surprisingly accurate ‘results when used for steady-state calculations involving liquid-liquid ex- traction. However, the most important result of this investigation is certainly the ability to simulate the transient paths of the output variables of such a process when itis being operated under time-variant conditions. The robustness of the model and the flexibility of the simulation package used puts no restriction on the conditions that can be modified, For example, a five-stage column with two. feeds. and two product withdrawals is considered. In this operation, sketched in Fig. 6, acetic acid is to be extracted from 2 mixture with benzene using water as solvent. The simulation is initialized assuming that the top and bottom feed streams start at equilibrium with the flow rates shown in Fig. 6, while the side feed and the product are set to zero: xy = (0.9970, 0.0030, 0.0000), _¥6= (0.0004, 0.9996, 0.0000). ‘Ten minutes after the start, these compositions are stepped to the existing ones: = (0.75, 0.00, 0.25), ¥%4= (0.00, 1,00, 0.00). fier 80 and 120 min, the other feed F, with Z; = (0.85, 0.00, 0.25), and the lateral withdrawal P,, respectively, are started. The response of the column along this changing path is illustrated in Fig. 7 by the concentration profiles of acetic acid in the extract phase. COMPUTER REQUIREMENTS The CPU time required by a CDC Cyber 175 computer to simulate each of the illustrative examples studied is detailed in Table 6. 10 tomol/ min 75% Benzene Bom cate ele Lf 3 timot7min 25% Berzece 85% heal aod ro1emer/min | Stage 5 wevorel Lage 05 omat/ min Fig. 6. Specification for dynamic acetic acid extraction.184 A.M. SERENO ef al o3e o2e| 2a 20 Mole fraction one 012] 008 004 720 165 200 Time Fig. 7. Transient profiles of acetic acid concentration in extract. ‘When using a simulation language like GEMS, the user-written program is first translated into a FOR- TRAN program together with a set of subroutines which are then compiled, loaded and executed. The uuse of such a problem-oriented language is very convenient but naturally increases the computer time necessary for the simulation. The execution time depends on several factors such as the extension of the change, phase holdups and the detail of the output requested. Table 6 is, however, indicative of the range of computer requirements. Acknowledgements —The financial support of the Instituto ‘Nacional _de Investigagio. Cientifia, Portugal, ‘and the Control Data Corp., Minn., U.S.A., is greatly appreciated. NOMENCLATURE, (C= Number of components F = Feed flow rate H =Holdup K = Distribution ratio, y/ L = Molar raffinate flow rate L1, L2, L3 = Empirical parameters for local models WN = Number of stages P= Intermediary product flow rate ‘S = Solvent flow rate t= Time V = Extract flow rate %y=Mole fraction of component i in stage j (afinate) x’ = Time derivative of x Yum Mole fraction of component / in stage j (ex- tract) y= Time derivative of y = Mole fraction of component ! in the feed to stage / Subscripts i= Compoent i = Stage j L = Raffinate, phase I, heavy phase ref = Reference component Ve Extract, phase I, light phase [REFERENCES 1. E. Chimowitz, T, F. Anderson, 8. Macchietto and L. F. ‘Stutzman, Ind, Engng Chem: Process, Des, Dev. 22,217 (1983) 2. T. Magnussen, J. M. Sorensen, P. Rasmussen and A. Fredenslund, Fluid Phase Equll: 4, 151 (1980). 3. GC, Pollock and A. I. Johnson, Can. J. Chem. Engng 47, 469 (1969. 4. RC. Waggoner and L. E. Burkhart, Comput. chem. 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