SHORT RANGE TRENDS IN
DlSTl LLAT IO N TECH N0 LOGY J A M E S
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F A I R
N ing the last 18 months will play
As nonidealities and 4 n a m i c s are better under-
an important role in shaping the immediate rather than far future. Prominently featured are studies of liquid phase nonidealities. Regular solution theory is used to generalize vapor-liquid equilibrium and gas solubility data, and new correlations of diffusion cofficients for the liquid phase are developed. Electronic computers also figure prominently. They are used to make rigorous calculations of stage requirements, simulate equipment dynamics, and control commercial systems. L41so, in terms of commercial design, research in mass transfer fundamentals is active. More realistic contacting models are being developed, and cases where chemical reaction occurs are receiving more attention. Decline of the bubble-cap tray continues. Sieve- and valve-type perforated trays remain popular, and packed columns are returning to favor. Hydrodynamics of tray columns is better understood, and commercial performance data give new support to general design methods. Dynamic behavior of distillation systems continues to be probed, and a publication on transient response studies with rather large equipment is particularly valuable. Also, activity continues in improving process analyzers and control systems.
stood, full
umerous reports published dur-
General
Several books and reviews have been published. One of the most significant i s the “Proceedings of the International Symposium on Distillation” (64) which contains a wealth of information for industrial practitioners. Subjects range from heat transfer and interfacial tension effects to design and operation of a new
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vacuum fractionator. For both the student and graduate, a book on equilibrium stage processes (67) and another on absorption, distillation, and cooling towers (55) are useful. An unusual book has appeared; it contains a number of computer programs (in Fortran language) for designing distillation columns, flashers, and similar separation devices. Two reviews (37, 78) cover many detailed literature references, one of which is particularly interesting because it interprets in some depth a feu7 selected areas of current research (78). Finally, another volume on azeotropic data deserves mention ( d o ) , ex'en though its contents could be classified as supporting physicalproperty data. Academic research in distillation areas continues. Of the titles for chemical engineering theses (75)in 1962, some 32 have a direct bearing on distillation and, of course, a number of others have indirect relationships. Of the 32 titles, about a third deal with fundamentals of mass transfer, a third with vapor-liquid equilibrium. and the remaining third with a variety of subjects. This distribution approximates that for published literature also. The symposium on recent advances in distillation held during the 142nd Meeting of the American Chemical Society, covered stage calculation techniques, control system design. transient behavior of columns, and vapor-liquid equilibria. 'The AIChE symposium held in New Orleans, March 1963, featured equipment design and performance characteristics. Basic Physical Data
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I n this country, work on vaporliquid equilibria (VLE) often is reported in the Journal of Chemical and Engineering Data. In a review of 1960-1 961 literature appearing in another journal, VLE is noted for 116 different systems (37). At the present time, low-temperature VLE for cryogenic processing is of particular interest, and a number of papers were given at the Denver AIChE meeting in August 1962. The active work in VLE accumulation involves development of new or
INDUSTRIAL AND E N G I N E E R I N G CHEMISTRY
modified devices for amplifying phase compositions or for ensuring equilibrium contact between the phasese.g., as pecial six-stage unit (571,a vapor-recirculating apparatus for operation down to -340O F. (72),and a device in which composition changes with time are used without a need for attaining thermodynamic equilibrium (79). The great potential value of gas-liquid partition chromatography for rapid accumulation of \'LE is demonstrated further by work at pressures up to 2000 p s i . (77). Although further interpretation and generalization of VLE are needed, significant contributions of interest to the practicing engineer or chemist appear only infrequently. Regular solution theory seems promising as a means for treating liquidphase nonidealities; in this connection, the very welcome revision of the classic work by Hildebrand and Scott appeared 135). Application of the theory to hydrocarbon systems is discussed ( 2 3 ) ,and some comparisons between measured and calculated K values are given. The theory is used to develop a correlation of low pressure solubilities for nonpolar gases in polar and nonpolar, nonassociated liquids (84), and also in correlating Van Laar constants for polar-nonpolar binary systems (27). Other work on generalization and prediction of VLE is reported (Z), where solvent selectivity is related to physical and chemical forces. Also, the principle of corresponding states is applied (46). However, need for a better understanding of liquid phase behavior is evident in all VLE generalization work. In distillation work, the liquid phase diffusion coefficient is of special interest. Unlike the gas phase coefficient, it is strongly concentration-dependent and, for nonideal solutions, predictive methods are not well established. A new correlation of liquid phase diffusion coefficients has been published (42), based on a statistical-mechanical approach and, for dilute solutions, appears to represent experimental data as well as the empirical correlation of
(Continued on page 58)
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Wilke and Chang (87). An engineering adaptation of this new work has also been published (43). Of special importance is the promise of the new correlation to represent concentration effects without the need for viscosity data. However, this has not been verified. Stage Calculations
The equilibrium stage concept is useful for tray-type fractionator design, even if it tends to mask some of the actual physical mechanisms which occur. Digital computers are now used widely for carrying out stage calculations, and published programs in the distillation area have been reviewed ( 3 1 ) . A book of programs (33) is available and another has been announced (38). The AIChE c,ontinuesto make available programs for distillation calculations, the most recent being multicomponent batch separations (52). The-time-honored McCabe-Thiele graphical method for establishing stage requirements is still popular, because it is a simple and easily visualized representation of actual tower flows. Two recent refinements in its use have been reported: a special plotting technique (48) for pinch zones where many trays are required together with a special graph paper ( 4 1 ) ; and a combined analytical-graphical technique for low relative volatility zones where many trays are needed (39). Mass Transfer and Tray Efficiency
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INDUSTRIAL A N D
ENGINEERING
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The two-film theory of mass transfer between phases involves concepts which are easy to understand and to apply : additivity of resistances, interfacial equilibrium, and molecular diffusion through films with "effective" thicknesses. The theory has been surprisingly successful in many applications where its physical representation was known to be faulty. It is not surprising that more effort is now devoted to developing a more realistic and practical model. This requires more fundamental approaches and precise experimentation. An excellent review of mass transfer to interfaces has appeared (34). Other articles deal with subjects such as droplet oscillation ( 7 6 ) , circulation patterns inside bubbles and
droplets (65), resistance at the interface ( 7 9 ) ,heat transfer influences in distillation (78), and unsteady state transfer at fresh surfaces (74). Simultaneous absorption and chemical reaction which have been especially popular (4, 5, 9, 24, 62, 7 7 ) , are of interest not only for equipment design but also for establishing more reliable mass transfer models. Many fundamental mass transfer publications show that the penetration model, together with its several modifications, is both reliable and realistic. Continued brisk activity is expected in these several fundamental mass transfer areas. Transfer occurs across a gas-liquid interface and, therefore, extent of this interface is important in equipment design. Several articles deal with interfacial areas in froths developed above perforated trays (72, 73, 60). Such work usually results also in the determination of over-all dimensions of the froth, residence time of gas in the froth, and the entraining tendencies of the gas as it leaves the froth. Related work on packed column interfacial areas continues: The most recent contribution notes that type of transfer influences effective area separately from the usual influences of hydrodynamic conditions (85). Reliable methods for predicting tray efficiencies of commercial distillation columns are needed. Where laboratory or pilot plant measurements are lacking, the AIChE twofilm predictive method is the best available. If measurements are necessary or desirable, the Oldershaw laboratory sieve-tray column is o€ten preferred. Data on Oldershaw columns have been summarized ( Z ) , along with attempts to interpret such data according to system foaming tendencies. Oldershaw column scale-up methods are often of a proprietary nature, but a tentative scaleup method has been devised (74).
Tray efficiency, especially in multicomponent systems, cannot always be predicted accurately. Judgment is still needed to determine when the AIChE method can be applied, and experimental back-up is often necessary. Present research and that needed in the future are thoroughly reviewed and discussed (28).
NEW DATA
Equipment
The cross-flow tray-i.e., bubble tray with downcomers-is still the most important contacting device for commercial fractionators. Within the cross-flow category, bubble-cap trays are now specified only occasionally, and sieve and valve trays are the most popular. That there is no one “best” device for all services is often obscured by advertising claims. A worthwhile and objective comparison on devices is available (86),based on distillation studies in an 18-inch column. The authors conclude that for normal problems, sieve trays are most attractive, but that for greater flexibility the valve tray can be justified. Another publication compares various tray types, but no specific ratings are given ( 7 ) . Cross-flow trays can be designed now with fair confidence, even though the contacting mechanisms are not well understood. To bolster confidence further, several welcome papers report performance of commercial distillation trays. Large (11to 12-foot diameter) sieve trays are found to excel bubble-cap trays in terms of efficiency, pressure drop, and low cost (58). Indirectly, it is also shown that single cross-flow designs-i .e,, without intermediate downcomers-can be specified for such large sieve trays without concern for hydraulic gradient problems. Efficiency and capacity data for large columns with hybrid sieve-valve trays are reported (69). I n one case, operation was fairly close to the critical point and vapor capacity was limited, possibly because of AUTHOR James R. Fair is Manager of foaming. Entrainment-flooding caPlanning and Deuelopment in the Research pacity data reported (68) for bubbleand Engineering Division, Monsanto cap, sieve, and valve trays show little Chemical Co., St. Louis, Mo. He difference in capacity between the authored the previous review which features longer range trends in distillation [IND. three types. This conclusion is veri(Continued on page 60) ENG.CHEM.54, 53 (June 1962)].
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fied (25),but with the additional conclusion that immediate preflood entraining characteristics can be quite different. Interest is active in characterizing liquid mixing which can afTect efficiency of cross-flow trays. Using the eddy diffusion model, coefficients in a sieve tray simulator were measured (8) by both steady and unsteady state techniques. Sieve tray data were correlated by the mixing stage model (53). Also bubble-cap trays were used (73) and instead of a mixing model, the concept of partial bypassing of liquid on the tray was substituted. Further, mixing data were correlated by a graphical approach (54). All reported information was obtained in simulators and extended to distillation columns by the indirect method of comparing calculated point efficiencies with measured over-all (Murphree) tray efficiencies. Confirmation under actual distillation conditions is needed. Other work with cross-flow devices includes bubble-cap tray efficiency measurements in high and low concentration ranges (&), studies of valve tray hydrodynamics (56) and valve stability (83), sieve tray entrainment phenomena (75), sieve and bubble-cap tray entrainment data ( I O ) , and the efficiency of cartridge-type valve t r a y for small columns (17). Counterflow tray devices, having lost their earlier popularity, are still used for critical pressure drop or fouling service. Interestingly, by using combinations of perforation size, the flexibility of Turbogrid trays can be improved (61). Pressure drop data for irrigated Turbogrid trays of various types are available (0’6).,4 new counterflow tray device containing a number of downcomer-like passages for both liquid and vapor is described j47),having high efficiency but limited capacity. Interest seems to be renewed in the use of large towers containing dumped or arranged packing materials. For years, packed columns generally have been limited to corrosive or other special services. Certain cost advantages of packings are now being recognized for vacuum fractionations,
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I N D U S T R I A L A N D E N G I N E E R I N G CHEMISTRY
and availability of new design methods has made scale-up factors more reliable. Relative packing efficiencies are discussed (27) and isolated performance data for a number of commercial systems are given. A new stacked metal packing material is described (82),but little performance information in included. In vacuum service, Stedman packing has hig,her efficiency than Raschig rings but less capacity and flexibility (20). Axial mixing in irrigated packings (3.2) is discussed, including use of cocurrent flow (30). This type of work is important in establishing true driving forces within the packed bed. Also published are analog computer solutions ( 7 I) for packed columns, under conditions of plug flow of both gas and liquid. Mass transfer and other data for packed columns with cocurrent flour of gas and liquid is reported (80). This mode of operation permits higher throughputs, because the usual countercurrent flooding problems are not encountered. If driving force disadvantage is not serious, designs for cocurrent flow can be useful. Column Dynamics a n d Control
The dx namic behavior of distillation systems is important to designers and operating supervisors. Bestknown of the dynamics problems are start-up time to reach steady state, transition timr between steady states, batch distillations, and control system design and operation. Distillation systems are popular with control and dynamics workers, and much theoretical material has been written. Only a few selected articles are mentioned here, but certain reviews are available (3, 631, where more comprehensive information is given. Regarding the need for experimental data on dynamic behavior of columns and their auxiliaries, it is encouraging to note that a carefully planned study at the University of Delaware is now under way. The equipment is that used earlier by the AIChE Research Committee program, and the column diameter of 2 feet is larqe enouqh to have commercial significance. O n this work, a series of four articles has appeared:
The first (6) dealt with step changes in reflux composition, and the column response was found to be predictable by the perturbation equations of Lamb and others (45). The second (7) showed that changes from total reflux to stripping could also be predicted by the equations. The third (70) covered the dynamics ol the condenser and thennosiphon re. boiler. And the fourth (50) treated feed perturbations. Successful pre. dictive methods have been developed, and valuable information will continue to come from this program. Computer-generated data have been used (29) to develop a general method for predicting the dynamic behavior of a binary system in a tray column. Also, despite a great many assumptions, a commercial tower which had been experiencing control difficulties was simulated, accurately enough to indicate proper corrective action (57). Useful dynamic data as well as interesting descriptions of ex. perimental techniques, obtained primarily by- a frequency response technique is available for a 91-tray Turbogrid column (59). Other artides cover process analyzers (76) as control elements (not process monitors), the important control variable of column heat input (49), and general methods of column control (36). The articles on heat input and column control note increased use of computen in control of internal reflux and feed enthalpy. As the dynamics of columns become better understood, full control by computer can be expected. REFERENCES (1) Aleksandmv, I. A,, Skablo, A, I., “Basic Characteristics and Application Ranges for Various Rectification and Absorption Column Plates,” Inram. Chm. Eng. 2,353 (1962). (2) Anderson, R., Cambia, R., Rausniu, J. M., “Physical and Chemical Forces in Solvent Selectivity for Hydrocarbons,” A.LCh.E. J., 8,66 (1962). (3) Archer, D. H., Rothfus, R. R., "Dynamics and Control of Distillation Units and Other Maas Transfer Equipment,” Ckm. Eng. Ram. 57, Symp. Ser. 36,2 (1961). (4) Astarita, G., Beek, W. J.,
“Effects of Liquid Phase Mixing in a Packed Tower on the First-Order Chemical Absorption,” C h m . Eng. Sci. 17, 665 (1962).
(5) Astarita, G., Marrucd, G, “Gas Absorption with Zcm-Order Chemical
(Continued on page 6.2)
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Reaction,” IND. ENG. CHEM. Fundamentals2, 4 (1962). (6) Baber, M. F., Edwards, L. L., Harper, \Y. T., Witte, M. D., Gerster, J. A , , “Experimental Transient Response of a Pilot Plant Distillation Column,” Chem. Eng. Progr. 57, Symp. Ser. 36, 148 (1961). (7) Baber, M. F., Gerster, J. A,, “Experimental Transient Response of a PilotPlant Distillation Column. 11. Response to Liquid and Vapor Rate Perturbations,” A.Z.Ch.E. J . 8, 407 (1962). (8) Barker, P. R., Self, M. F., (‘Evaluation of Liquid Mixing Effects on a Sieve Plate Using Unsteady State and Steady State Tracer Techniques,” Chem. Eng. Sci.17, 541 (1962). (9) Brian, P. L. T., Vivian, J. E., Habib, A. G., “Effect of the Hydrolysis Reaction Upon the Rate of Absorption of Chlorine intoWater,” A.Z.Ch.E. J . 8 , 145 (1962). (10) Brown, A. J. H., “Separation of Liquid Mixtures by Distillation,” Brit. Chem. Eng. 7,102,178 (1962). (11) Brown, E. C., von Rosenberg, D., “Solution of Packed Column Distillation Problems by Analog Computation,” A.1.Ch.E. Meeting, New Orleans, March 1963. (12) Calderbank, P. H., Evans, F., Rennie, J., “Mass-Transfer Efficiency of Distillation and Gas-Absorption Plate Columns. I. Techniques for Measuring Gas-Liquid Interfacial Areas and Foam Densities in Plate Columns,” Proc. Intern. Symp. Distn., p. 51, Brighton, Engl., 1960. (13) Calderbank, P. H., Rennie, J., “Physical Properties of Foams and Froths,” Trans. Znsl. Chem. Engrs. (London) 40, 3, 191, (1962). (14) Calvert, S.,Kapo, G., “How to Use Penetration Theory to Evaluate Transport Coefficients,” Chem. Eng. 7 0 , No. 3, 104; No. 5, 105 (1963). (15) Chem. Eng. Progr, “Research Roundup for 1962,” 59, No. 1, 81 (1962). (16) Constan, G. L., Calvert, S., “Mass Transfer in Drops Under Conditions that Promote Oscillation and Internal Circulation,” A.Z.Ch.E. J . 9, 109 (1963). (17) Dale, G. H., Dove, W. T., Huntington, R. L., “Can Trays Be Used in Small Towers?” Petrol. Rejner, 41,No. 8 , 117 (August 1962). (18) Danckwerts, P. V., Sawistowski, H., Smith, W., “Effects of Heat Transfer and Interfacial Tension in Distillation,” Proc. Intern. Symp. Distn., p. 7 Brighton, Engl., 1960. (19) Delaney, L. J., Eagleton, L. C., “Test of the Assumption of Interfacial Equilibrium in Measurements of the Gas Film Mass Transfer Coefficient,” A.2.Ch.E. J.8, 418 (1962). (20) Delzenne, A., “Comparing the Efficiency of Different Types of Packings in Low-Pressure Rectifying Columns,” Gknie Chim.88, No. 2, 33 (1962). (21) Eckert, J. S., “Comparative Distillation Performance of Tower Packings,” A.1.Ch.E. Meeting, New Orleans, March 1963. (22) Ellis, S. R. M., Legg, R. J., “Surface Tension Effects on the Efficiency of an Oldershaw Column,” Can. J . Chem. Eng. 40, 6 (1962). (23) Ellis, S. R. M., Spurr, M. J., “New Circle NO. 32
62
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INDUSTRIAL A N D ENGINEERING CHEMISTRY
Use of Solubility Parameter on Binary Systems,” PetrojChem Engr. 34, No. 4, 33 (1962). (24) Emmert, R. E., Pigford, R. L., “Gas Absorption .4ccompanied by Chemical Reaction: A Study of the Absorption of Carbon Dioxide in Aqueous Solution of Monoethanolamine,” A.Z.Ch.E. J . 8, 171, 702, (1962). (25) Fair, J. R., “How to Predict Sieve Tray Entrainment and Flooding,” Petrol Chen Engr. 33, No. 10: 45 (1961). (26) Fair, J. R . , “Trends in Distillation Technology,” IND. ENG. CHISM.54, No. 6, 53 (1962). (27) Finch, R. N., Van Winkle, M., “Prediction of Vapor-Liquid Equilibrium for Polar-Nonpolar Binary Systems,“ A.I.Ch.E. J . 8, 455 (1962). (28) Gerster, J. A., “Tray EfirienciesIs More Research Needed?,” A.1.Ch.E. Meeting, Chicago, December 1962. (29) Gilliland, E. R., Mohr, C. M., “Transient Behavior in Plate-Tower Distillation of a Binary Mixturc,” Chem. Eng. Progr. 58, No. 9, 59 (1962). (30) Glaser, M . B., Lichtenstein, I., “Interrelation of Packing and Mixed Phase Flow Parameters with Liquid Residence Time,” A.Z.Ch.E. J. 9, 30 (1963). (31) Goulcher, R. \V., “Use of Digital Computers in the Solution of Multicomponent Distillation Problems,” Brit. Chem. Eng. 7 , 590, 663 (1962). (32) Gray, R. I., “Dynamics of a Packed Gas Absorber by Frequency Response Analysis,” Ph.D. thesis, Univ. Tenn., 1961. (33) Hanson, D. N., Duffin, J. H., Somerville, G. F., “Computation of Multistage Separation Processes,” Reinhold, New York, 1962. (34) Harriott, P., “ A Review of Mass Transfer to Interfaces,” Can. J . Chem. Eng. 40,60 (1962). (35) Hildebrand, J. H., Scott, R. L., “Regular Solutions,” Prentice-Hall, Englewood Cliffs, S. J., 1962. (36) Hoffman, H. L., “Automatic Control for Distillation,” Hydrocarbon Process. Petrol. Refiner 42,No. 2, 107 (1963). (37) Holdsworth, S. D., “Distillation,” Chem. ProcessEng. 43, 172 (1962). (38) Holland, C. D., “Multicomponent Distillation,” Prentice-Hall, Cnglewood Cliffs, N. J., in press. (39) Holland, F. A., Brinkerhoff, R., Carlson, R. C., “Designing ManyPlate Distillation Columns,” Chem. Eng. 70,No. 4, 153 (1963). (40) Horsley, L. H., and Tamplin, TV. S., “Azeotropic Data. 11,” Adv. Chern. 35 (1963). (41) IND. EKG. CHEM. 5 5 , h-0. 2, 10 (1962). (42) Kamal, Pvl. R., Canjar, L. N., “Binary Liquid Diffusion Coefficients,” A.Z.Ch.E. J . 8, 329 (1962). (43) Kamal, M. R., Canjar, L. N., “Finding Liquid Diffusion Coefficients,” Chem. Eng. 69, No. 25, 159 (1962). (44) Kirschbaum, E., Fischer, H . , Tl’olf, D., “Performance and Capacity of a Rectifying Column Containing a Large Number of Plates,” Chem. Zng.-Tech. 34, 423 (1962). (45) Lamb, D. E., Pigford, R. L., Rippin, D. W. T., “Dynamic Characteristics and Analogue Simulation of Distillation
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Need surface active groups? Try propane
-
(3-hydroxy-1-propanesulfonicacid sultone) HELL
propane sultone reacts with a
S variety of salts and amines via cleavage of the carbon-oxygen bond. This leads to 3-substituted propanesulfonic acid derivatives. Propane sultone should be of particular interest in preparing intermediates for cosmetic and surfactant applications where watersolubilizing groups or an increase in polarity is needed. Typical reactions: Propane Sultone
+ RONa
RO-CH,-CH,-CH,-S0,Na Propane Sultone
+ RNH,
+ RNH,-CH,-CH,-CH,-SO,
-
Properties: Appearance
Nearly colorless crystalline solid.
Melting Point Solubility
31°C. Soluble in the lower alcohols and aromatic hydrocarbons; partially miscible in water (reacts).
For product literature and a sample, write to : Product Development Department, Industrial Chemicals Division, Shell Chemical Company, 110 West 51st Street, hTew York 20, New York.
on Readers’ Service Card NO. 5 M A Y 1 9 6 3
Circle No. 13
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