m$
HIGH TEMPERATURE DISTILLATION T. J. WALSH, CASEINSTITUTE
OF TECI-INOLOGY, C L E V E L A N D 6, OHIO
. e
I n the’past year, there were two outstanding developments in the held of high temperature distillation. First was the challenging of the position long held b y bubble-cap trays as the sole practical contact unit in large scale distillation equipment, by several simpler trays. Second was the application of computing mdchines to the solution of distillation problems. Much progress has also been made in the theory of unsteady-state distillation.
Specially designed bubble-cap trays are being used successfully in the vacuum distillation of thermally unstable hydrocarbons. Distillation of H E Celanese Chemical Co. is using perforated plates in fatty acids in continuous vacuum stills gives greater yields of most of the new towers in that company. The feature of better quality acids than the batch distillation process (8). these columns is the small hole size--8/le inch in diameterTrays are heated within the still by Dowtherm vapors. Continuous vacuum distillation is also the most economical method used on the trays. A 60-tray column with a diameter of 6.5 feet gave an efficiency 20% greater than an equivalent bubble-cap of fractionating tall oil (187). Considerations of pressure drop through bubble caps are column (89, ‘76). The bubble-cap tray used in this experimental comparison was not, however, designed to give maximum efstudied by Huitt and Huntington (55). They find that the surface tension of the liquid is an important variable a t low ficiency. Pilot plant perforated plate data are also given by flow rates. This appears to be a measure of the energy used to Arnold el al. (3). Turbogrid trays are being used in 80% of Shell’s new construcform a bubble. The behavior of gas bubbles in mass transfer varies with the size and velocity of the bubble (19). tion (15). These trays are essentially horizontal slot trays. Although admittedly less efficient than bubble-cap trays (66), The fluid dynamics of bubble trays is well reviewed by Houghthe use of the new structure permits reduced holdup, reduced land and Schreiner (54). Experience with rectangular caps is pressure drop, lower cost, and-by using close tray spacingincluded in this report. Slot opening of bubble-cap slots may lower towers. be correlated with air flow using a modified orifice equation with a coefficientof 0.57 (83). The Benturi tray was introduced last year. Performance data on these trays in commercia1 installations are given by Thornton Packed towers in laboratory, pilot plant, and commercial plant size continue to receive much attention. Packed tower (121). Increased throughput of 30% was not achieved by replacing bubble-cap trays by Benturi trays in a depropanizer. design is the topic of a new book by Leva (71), an article by A chart for sizing trays is included in this article. Williamson (132),and several articles by Pratt (99). All authors Behind this effort to replace the conventional bubble-cap find that a reflux distributor is eesential to optimum operation of tray with other contacting units lies the present cost of all types packed columns. The explanation of this is probably in the of p r o c e s s i n g equipment. need for complete wetting of Jandrisevits (68) indicates the packing before it is fully that preliminary cost estieffective. Pratt (100) finds mates for a 50-tray bubble a minimum effective liquid cap tower 18 inches in diamrate above which the mass eter should be $80,000 when transfer coefficient is indecarbon steel is satisfactory pendent of the liquid rate. and $160,000 when alloy steel Liquid rates in distillation is r e q u i r e d . T h e o r e t i c a l are generally below the ministudies by Gerster and others mum effective liquid rate; a t the University of Delaware thus the mass transfer co(37, 98) indicate that best efficient is generally a funcefficiencies will be obtained tion of the boilup rate. Norwhen the vapors are disman (85) found t h a t wetting tributed completely throughgreatly affects the performout the liquid on each tray. a n c e of g r i d - p a c k e d This distribution is not towers. On the other hand, achieved with the bubble-cap COURTESY NATIONAL CARSON. D I V I ~ I O N OF UNION C A R W O E B CARBON co Skulman and DeGroff tray. Figure 1. Ten-Inch Diameter Karbete Impervious Graphite Tray and (118) found that the effecBubble Caps Other data relating to the tive area of 1-inch Raschig performance of bubble-cap rings is greater than the trays in the form of efficiency correlations are given by Kondo wetted area. Kaufman and Thodos (64) express the effective area as the total area of the packing times a n effective and Fujita (68) and by Kamei and Takamatsu (61). Wetted-wall tube-plate columns give between 33 and 50% area factor that is a function of shape only. The effecplate efficiency when installed in a column a t 6.75-inch plate tive area factor is arbitrarily made equal to 1 for spheres and spacing (76). However, the column tested was small, only 3.75 varies from 0.52 for Raschig rings to 1.09for Berl saddles. inches in diameter. Wetted-wall columns are still inefficient on Stedman packing characteristics are a function of wetting a large scale. With 6 / ~ e inch between closest points on the outside and a distributor is necessary for best operation (80). The of tubes, a height equivalent to a theoretical plate of about 5 feet height equivalent to a theoretical plate of Stedman packing is reported by Lindsey et al. (73). in the distillation of hydrogen and its isotopes is about 1 inch
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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
(SO). D a t a on protruded packing is provided in a bulletin available from the Scientific Development Co. (116) and data on the new Octa-pak from Podbielniak, Inc. ( 9 7 ) . The chemical nature of a packing may be used to give a more efficient separation (55). The process is actually a combination of chromatographic separation and distillation. Thus, the boundary between the various diffusional operations continues t o break down. Standard tower sections of impervious graphite for use with any random type packing are offered b y the National Carbon Division of the Union Carbide and Carbon Corp. (83). Also available is a full line of bubble caps, sieve trays, and spray equipment. COMPUTING MACHINES
Many of the calculation techniques used in the past included approximations and assumptions but made for the sake of a solution. Such assumptions include negligible heat losses, ideal behavior, and constant relative volatility. The use of digital computers of the International Business Machines type t o solve batch distillation curves with appreciable holdup, variable relative volatility, variable overflow, and variable plate efficiency is described by Rose et al. (108). Plate efficiency considerations accounted for the main deviation of experimental and theoretical results. The use of the card programmed calculator for the solution of trial and error design calculations is outlined in another paper by Rose and coworkers at Pennsylvania State College (111).
The punch card calculation technique is also used by Opler and Heitz (86) for six-component distillations. Heat losses and deviations from ideality are handled by successive repetitions. These authors comment t h a t the engineers must still do the thinking for the machine but that more tedious calculations are justified using machine calculators. Analog computers of many kinds may be used to solve equilibrium problems of the flash vaporization type, such as dew point, bubble point, and vapor-liquid composition. Electrical analogs for the solution of multicomponent phase equilibrium problems are discussed by Wilson (134). 4 n electromechanical computer for the same purpose is offered by Morris (79). A commercial instrument of the electrical resistance bridge type is offered by Beckman Instruments (6). The literature of this company points out that the computers are capable of greater accuracy than the present knowledge of equilibrium constants justifies. A mechanical analog for steady-state separations of two stages is described by Franklin et al. (33). DISTILLATION THEORY
Steady-state distillation theories have not been changed during the year. Constant relative volatility is assumed in practically all of the theoretical developments. Murdoch and Holland (81, 86) present analytical analogs of Underwood equations in multicomponent distillation. Hirayama ( 5 2 ) rederives the Underwood equations using a matrix theory. Further study of the Underwood equation and a graphical solution are presented by Forsyth and Franklin ( 3 1 ) . A simplified equation is offered by Hirata ( 6 1 ) for the solution of design problems. The approach used here is a modified operating line. Ternary distillation problems may be solved on triangular diagrams. Kammermeyer and Lee ( 6 3 ) propose the use of the right triangular diagram for this purpose. Interrelations between distillation curves of the flash vaporization and true boiling point are developed by Bowman ( 1 0 ) from the composition distribution function. The approach is applied t o flash distillation problems of many components by Bowman and Edmister ( (I)and two applications of the concept are shown by Edmister and Buchanan (27).
Vol. 45, No.
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Vacuum distillations are discussed by Benedict ( 7 ) and by Peters and Cannon (95). Improvement in thermal efficiency, generally low, is studied by Freshwater (34). The absorption factor technique of distillation calculations has been revived and is presented in a series of papers given a t t h e Houston meeting of the Natural Gasoline Association of America (89, 7.4, 93). All of the usual simplifying assumptiom are made in this method. The theory of unsteady-state (batch) distillation has been greatly advanced during the last year. The pole height concept has been made more useful by the development of a relationship among the number of practical operating plates, actual reflux ratio, minimum number of theoretical plates, and the minimum reflux ratio as determined from the pole height (138). Differential equations for batch distillations are set up by Rose and Johnson (107). The equations cannot be integrated by standard analytical techniques. The only satisfactory solution a t the present time is through the solution of finite difference equations. The effect of holdup of a fractionating column on separation has been studied. Increasing the holdup is harmful in most cases but easy separations may be aided by an increase in holdup (109, 110). The effect of reflux ratio on intermediate fractions is less for actual columns than is predicted from no holdup calculations ( 9 6 ) . Hawkins and Brent ( 4 6 ) compared spiral screen and Raschig ring packings over a range of pressures for both steady-state and unsteady-state distillations. Their results indicate a n apparent increase in number of theoretical plates for a given column as the reflux ratio is decreased from infinity. This is caused by the use of a hIcCabe-Thiele calculation with a straight operating line for the distillations a t finite reflux ratios. Holdup in the column actually causes the operating line t o curve away from the equilibrium curve, giving a n easier separation and fewer theoretical plates than are calculated from the straight line. A theoretical comparison of continuous and batch distillations in the laboratory indicates that the batch distillation may have an advantage in giving greater yield (112). This does not include a consideration of thermal stability of the components. The general background of distillation may be reviewed in “Chemical Engineering Operations” by Rumford (113) or in a training article by Chu (16). The fourth annual review of analytical distillation by Rose (106) covers yearly progress in that field. VAPOR-LIQUID EQUILIBRIA DATA
Systems for which vapor-liquid equilibria data were reported during the year are indicated i n Table I. Interesting systems include propylene oxide-water which is a two liquid phase nonazeotrope (150). The system nitrogen-ammonia a t pressures above 1000 atmospheres shows two fluid phases (the so-called gas-gas equilibrium). The theoretical explanation of this phenomenon is discussed by Lindroos and Dodge ( 7 2 ) . Another type of unusual behavior is found in the dodecane-octadecene system. Here the activity coefficients are above 1 atmospheric pressure but shift to below 1a t low pressure (60). Use of equilibrium constants ( K ) for calculating vapor-liquid equilibria of hydrocarbon mixtures is a common practice in the petroleum industry, This technique has never been completely satisfactory, as the constants should be evaluated in terms of the composition of the mixture. The errors introduced by neglecting the composition effect are greatest for methane and ethane. Arnold ( 4 ) shows how these may be correlated in terms of a convergence composition. Amick et al. ( 8 ) point out that regularly evaluated constants do not fit the data for the methaneisobutane system. K a y and Nevens (66) show t h a t the equilibrium constant of ethane in ethane-benzene mixtures differs appreciably from t h a t of ethane in ethane-paraffin mixtures
January 1953
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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
a n d from that evaluated using fugacities a t the same pressure and temperature. Ethylene appears t o be the same type of substance, as fugacity data do not show agreement with experimental data for ethylene in mixtures with nitrogen, hydrogen, or ethane (39). Heavier hydrocarbons correlate better and K charts are presented for dodecane, hexadecane, and octadecane by Van Winkle (126). Solomon (119) shows that K's correlate better if the Watson characterization factor is included in the correlation. A nomograph presenting hydrocarbon vapor-liquid data in terms of temperature and pressure is presented by Winn (136)and methods of predicting equilibrium constants are presented by Organick and Brown (87)and by Rzasa et al. (114). Several azeotropes are included in the binary systems. The azeotrope in the methanol-methyl ethyl ketone is notable, a8 no azeotrope is reported for either methanol-methyl propyl ketone or for methanol-methyl isobutyl ketone (50). An azeotrope, boiling a t 866' C., consisting of 92% P4010and 8% water is reported by Brown and Whitt (12). Also interesting are three azeotropes of paraffins reported for the cyclohexanetriptane, cyclohexane-2,2,4-trimethylpentane,and cyclopentaneneohexane systems by Marschner and Burney (76). It now appears that azeotropism should be expected for any system on which data are not available. Tables of azeotropic data originally published in Analytical Chemistry are now available from the AMERICAN CHEMICAL SOCIETY (63). Vapor pressure data fundamental to the calculation of vaporliquid composition data by any method are given for many organic compounds in a new handbook by Dreisbach (24). The tables are calculated from Cox chart correlations using the convergence point approach. Vapor pressure data for light normal saturated hydrocarbons in the form of five constant equations are given by Perry and Thodos (94). Experimental data for some methyl esters of fatty acids presented by Scott et al. (117) indicate that methyl esters of successive even carbon atom saturated acids may be separated without great difficulty, but between 250 and 500 theoretical plates or the equivalent will be necessary to fractionate the methyl esters of the unsaturated C1g acids. The minimum amount of data necessary for establishing phase behavior and thermodynamic properties together with methods of measurement and means of expressing relationships are presented by Sage and Reamer (116). The limitations of thermodynamic formulas and semiempirical equations are pointed out by Nord (84) and a system of flexible equations amounting to an approximate equation of state is proposed by Redlich et al. (104). Equations and tests for vapor-liquid equilibria data under both isobaric and isothermal conditions together with methods of interpolation are discussed by Herrington (46-48) and by Yu and Coull(137). LABORATORY DISTILLATIONS AND EQUIPMENT
Correlation d laboratory data and commercial operation is frequently complicated owing to the impracticability of using the same type of equipment in the laboratory as in the plant. Methods of controlling small flows to make possible continuous distillation in the laboratory and descriptions of continuous stills as used in the laboratories of the Dow Chemical Co. are presented by Wilcox et al. (131). A laboratory adaptation of the pipe still is featured by Hands and Norman (43). The still is particularly recommended for the distillation of heat-sensitive materials. Heat is supplied to the feed stream using a rising film evaporator. An automatic pilot plant charging from 5 to 100 gallons is the series 400 Podbielniak Fractiopeer. This still may be fitted with columns of various diameter and either of the Podbielniak random packings-Heli-pak or Octa-pak. Pressure range is from 5 mm. of mercury t o 300 pounds per square inch, Reflux
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is controlled automatically a t ratios up to 100 to 1. The unit is describedin a brochure available from Podbielniak, Inc. (98). Other laboratory an$ pilot plant stills are also available commercially. Corning Glass offers parts for a 6-inch glass bubblecap column (20). Concentric tube semimicro columns are offered by Wheeler (128). The latter columns feature minimum holdup and up to 75 theoretical plates. Emil Greiner Co. (41) offers a flash-type equilibrium still originally described by Othmer et al. (90).
Table
1.
Equilibria Data
System 1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
11.
12.
13. 14. 15. 16. 17. 18. 19.
Literature Cited
Acetic acid-water Eth 1alcohol-water MetKane-isopentane Acetone-carbon tetrachloride Methane-nitrogen Hydrazine-water Pfopane-propylene Methanol-propanol; Methanol-butanol Methanol-pentanol Methanol-methyl ethyl ketone Methanol-methyl propyl ketone Methanol-methyl isobutyl ketone Ethane-benzene Dodecane-hexadecane Propane-water Nitrogen-ammonia Cyclopentane-neohexane Cyclopentane-triptane
20. Cyclopentane-2,2,4-trimethylpentane 21. Acetone-water 22. Acetone-methyl ethyl ketone 23. Water-methyl ethyl ketone 24. Propane-carbon dioxide 25. n-Butane-water 26. Benzene-furfuraldehyde 27. Cyclohexane-furf uraldehyde Benzene-cyclohexane Benzene-methyl Cellosolve 30. Cyclohexane-methyl Cellosolve 31. Iso-octane-toluene 32. Iso-octane-furfuraldehyde 33. Toluene-furfuraldehvde 34. Toluene-n-hexane 35. Propylene oxide-water
2:
36. 37. 38. 39. 40. 41. 42. 43* 44. 45. 46. 47. 48. 49. 60. 51.
rhlnrodiflnoromethane-monochlorodifluoromethane
.ifluoromethane-l,1,2,3,
2-Propanol-water n-Decane-trans-Deoalin n-Hexadecane-n-heptylbenzoate Pvridinn-water
Benzene-cyclohexane-methyl Cellosolve Toluene-iso-octane-furfuraldeh yde
A high pressure equilibrium still of stainless steel is described by Othmer et al. (89) and a polyethylene still for the preparation of pure hydrofluoric acid by Coppola and Hughes (19). An improved equilibrium still featuring nearly adiabatic operation and a short time of approach to equilibrium is described by Altsheler et al. ( 1 ) . A maximum relative volatility, a, in the ethyl alcohol-water system a t 0.4% (weight) of ethyl alcohol is also reported in this paper. An equilibrium flash still and data for four crude petroleum fractions are discussed by Johnson and Mills (69). The treatment of data from multiplate equilibrium stills is discussed by Reed and Myers (105). A three-sample method and a two-sample method are proposed. A graphical solution is recommended as the significance of the data is not immediately obvious. The behavior of laboratory columns of the Vigreux and of the spinning band type over a wide range of pressure was studied by Zuiderweg (140). The Vigreux column lost about 25% of its atmospheric pressure efficiency and the spinning band column lost about 70% as the pressure was reduced.
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INDUSTRIAL AND ENGINEERING CHEMISTRY
Techniques of laboratory operation involved the use of the alcohol chaser technique for the routine determination of butanes in furfural or absorber oil (5'7). The synthetic samples prepared to test the method showed good agreement, although one sample indicated a n error of 2 parts in 15. Caution should be exercised when using this technique, as ethyl alcohol is known to form azeotropes with hydrocarbons boiling in the butane range. Batch differential vacuum distillation has been recommended as a means of evaluating heavy stocks t h a t cannot be distilled without decomposition a t atmospheric pressures. A theoretical analysis indicates that the vacuum distillation may be used if fundamentals can be clarified (70). The experimental curves have a greater slope than the calculated curves, indicating t h a t the reflux is increasing during the distillation. A corrected vapor pressure-temperature correlation is proposed for adjusting measured temperatures to atmospheric boiling points. Column auxiliaries to simplify the construction or operation of a distillation unit are described in several articles. Miller ('78) proposes a constant reflux ratio head of the Corad type with the tapered joint by which the head is attached to the column inverted (the female section attached to the head) and improved drip tips on the bottom of the condensing sections. A vapor split condensing head with th? vapor flow controlled through a rotating valve located in the cold zone is suggested by Payne and Perrins (92). Control of coolant flow for still heads operating at low temperatures by use of a relay working on alternating current is illustrated by Stokes and Hauptschein (120).
At the other end of the column, Feldrnan and Pantages (88) describe a n adapter for inserting heating coils directly into a distilling flash through the flash neck. The coils are claimed to give smooth boiling even under conditions of high vacuum. , The laboratory column proper must be insulated t o ensure substantially adiabatic operation or the natural tendency t o lose heat must be compensated by heating the outside of the column. The latter is simplified by the use of Corning's conducting glass tubes. These permit the application of 5 n atts per square inch a t 115 volts. The temperature may be raised to 350' C. and is limited by the coating used on the glass. The conducting glass is chemically resistant but should not be used in a reducing atmosphere @ I ) . Glas-eo1 has also added t o its line of heating mantles, with mantles for fractionating columns and heating bands for wrapping transfer lines (40). An automatic product collector and meter for batch distillation operation in which the volume of each sample activates the turntable receiving mechanism is described by Crook and Datta (28). EXTRACTIVE DISTILLATION
Extractive distillation is that type of nonideal distillation in which the solvent used is not vaporized in the column. The design and application of extractive distillation equipment are discussed by Chambers (14). The column should be considered in two sections with the extractant florring countercurrent to the first key in one section and concurrent to the second key in the other section. Plate efficiencies in extractive distillation columns are generally low but may be correlated with the viscosity of the fluid phase (62). A plant using phenol as a n extractive distillation solvent for the recovery of high purity benzene and toluene from petroleum fractions is described by Dunn and Liedholm (26). The selection of solvents for extractive distillation and the prediction of ternary equilibrium data from binary data are considered by Garner and Ellis (36). A new equilibrium still is apparently needed, as the binary data do not allow calculation of the ternary equilibria with a n accuracy better than 10%. The best solvents for the separation of n-butane from butencs are aniline and furfural-water (49).
Vol. 45, No. 1
BIBLIOGRAPHY
Altsheler, W. B., Unger, E. D., and Kolachov, P., ISD.ENG, CHEM.,43, 2559 (1951). Amick, E. H., Jr., Johnson, W. B.. and Dodge, B. F., Chem. Eng. Progr., Symposium Ser., 48;No. 3, 65 71952). Arnold, D. S., Plank, C. A., and Schoenborn, E. M., paper presented a t meeting Am. Inst. Chem. Engrs., Atlanta, .Ga., March 1952. iirnold, J. H., Chem. Eng. Progress,Sumposium Ser., 48, E o . 3, 82 (1952). Bachman, K. C., and Simons, E. L., IKD.ENG.CHEM,,44, 202 (1952). Beckman Instruments, Inc., Chem. Eng., 59, No. 6, 224 (1952). Benedict, Q. E., Petroleum RefineT, 31, No. 1, 103 (1952). Berger, R. W., paper presented at meeting Am. Oil Chemists' SOC.,Chicago, Ill., October 1951; Wurster and Sanger, Inc., 5201 Kenwood Avo., Chicago, Ill., Bull. 25. Bloomer, 0. T., and Parent, J. D., Inst. Gas Technol., Research Bull. 17 (April 1952). Bowman, J. R., ISD.EXG.CHEW,43, 2622 (1951). Bowman, J. R., and Edmister, W. C., Ibid., 43, 2625 (1951). Brown, E. H., and Whitt, C. D., lbid., 44, 615 (1952). Burtle, J. D., Ibid., 44, 1675 (1952). Chambers, J. M., Chem. Eng. Progr., 47, 555 (1951). Chem. Eng. A7ews, 30, 4164 (1952). Chu, J. C., J . Inst. Petroleum, 37, 605 (1951). Cines, M. E., Roach, J. T., Hogan, R. J., and Roland, C. H., paper presented a t meeting Am. Inst. Chem. Engrs., atlantic City, N.J., December 1951. Coppock, P. D.., and hfeiklejohn, G. T., Trans. Inst. Chem. Engrs. (London),29, 75 (1951). Coppola, P. P., and Hughes, R. C., Anal. Chem., 24, 768 (1952). Corning Glass Works, Corning, N. Y., Bull. PE-9. Corning Glass Works, Corning, N. Y.,Supplement 1 to Catalog LP-31. Crook, E. M., and Datta, S. P., Chemistry & Industru, 1951, 718. Cross, C. A., and Ryder, H., J. A p p l . Chem., 2, 51 (1952). Dreisbach, R. R., "Pressure-Volume-Temperature Relationships of Organic Compounds," Sandusky, Ohio, Handbook Publishers, Inc. Dunn, C. L., and Liedholm, G. E., Petroleum Engr., 24, KO.9, C-7 (1952). Dwyer, 0. E., and Gleioh, TV. P., Chem. Eng. Progr., S y m p o sium Ser., 48, No. 2, 80 (1952). Edmister, W. C., and Buchanan, D. H., paper presented a t meeting -4m. Inst. Chem. Engrs., Atlantic City, N. J., December 1951. (28) Feldman, J., and Pantages, P., Anal. Chem., 24, 432 (1952). (29) Ferro, B. J., Lcgatski, H. R., and Hachmuth, K. H., paper presented at meeting Natural Gasoline Assoc. of america, Houston, Tex., 1952. (30) Fookson, A , , Pomerantz, P., and Rothberg, S., J . Research A'atl. Bur. Standards, 47, 449 (1951). (31) Forsyth, J. S., and Franklin, K.L., Trans. Inst. Chem. Engrs. (London),27, 223 (1949). (32) Fowler, R. T., J . AppZ. Chem. (London),2, 246 (1952). (33) Franklin, N. L., Forsyth, J. S.,and Winning, H., Jr., Tmns. Inst. Chem. Engrs. (London),29, 63 (1951). (34) Freshwater, D. C., Ibid., 29, 149 (1951). (35) Fuchs, O., Chem. Ing. Tech., 43,2932 (1951). (36) Garner, F. H., and Ellis, S. R. M., Trans. Inst. Chem. Enws. (London),29, 45 (1981). (37)'Gerster, J. A,, and Bonnet, W.E., Chem. Eng. P T O Q 47, ~ . , 523 (1951). (38) Gerster, J. A., Bonnet, W. E., and Hess, I., Ihid., 47, 621 (1951). (39) Gilliland, E. R., and Sullivan, T. E., Ibid., Symposium Ser., 48, No. 2, 18 (1952). (40) Glas-col Apparatus Co., Inc., 711 Hulman St., Terre Haute, Ind., Bull. 4. (41) Greiner, Emil, Co., 20 North Moore St., New York 13, S . Y . , Lahitems, 2, No. 1, March 1952. (42) Giiswold, J., and Wong, S.Y . , Chem. Eng. Progr., Symposium Ser., 48, Xo. 3, 18 (1952). (43) Hands, C. H. G., and Korman, TV, S., Trans. Inst. Chem. Engrs. (London),27, 71 (1949). (44) Hanson, G. H., Hogan, R. J., Nelson, W. T., and Cines, AI. R., I N D . ESQ. CHEXf., 44, 604 (1952). (45) Hawkins, J. E., and Brent, J. A , , J r . , Ibid., 43, 2611 (1951). (46) Herrington, E. F. G., J . Appl. Chem. (London),2, 1 1 (1952). (47) Ibid., p. 19. (48) Herrington, E. F. G., J . Inst. Petroleum, 37, 457 (1951).
January 1953
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INDUSTRIAL AND ENGINEERING CHEMISTRY
(49) Hess, H. V., Naragon, E. A., and Coghlan, C. A,, Chem. Eng. Progr., Symposium Ser., 48, No. 2, 72 (1952). (50) Hill, W. D., and Van Winkle, M., IND. ENG.CHEM.,44, 205 (1952). 151) Hirata. M.. Chem. Eno. [Javan).15,267 (1951). . . i52j Hirayama,’S., Ibid., 16, i72 (1952); (53) Horsley, L. H., et al., Advances in Chem. Ser., No. 6 (1951). (54) Houghland, G. S., and Schreiner, W. C., Proc. Natl. Con$ Ind. Hydraulics, IV, 75 (1950). (55) Huitt, J. L., and Huntington, R. L., Petroleum Refiner, 30, No. 8, 111; No. 10, 153 (1951). ENG.CHEM.,44, No. 9, 15 A (1952). (56) Hull, W. Q., IND. (57) Hyzer, R. E., Anal. Chem., 24, 1093 (1952). (58) Jandrisevits, P., IND. ENG.CHEM.,43,2299 (1951). (59) Johnson, P. H., and Mills, K. L., Jr., Ibid., 44, 1624 (1952). (60) Jordan, B. T., and Van Winkle, M., Ibid., 43, 2908 (1951). (61) Kamei. S..and Takamatsu, T., Chem. Eng. (Japan),16, 178 (1952). (62) Kammermeyer, K., and Lee, Ibid., “Graphical Interpretation in Ternary Distillation,” paper presented at meeting of Am. Inst. Chem. Engrs., Chicago, Ill., September 1952. (63) Kammermeyer, K., and Lee, K. T., Ibid, “Plate Efficiencies in an Extractive Distillation Column.” (64) Kaufman, D. J., and Thodos, G., IND.ENG.CHEM.,43, 2582 (1952). (65) Kay, W. B., and Nevens, T. D., Chem. Eng. Progr., Symposium Ser., 48, No. 3, 108 (1952). (66) Keistler, J. R., and Van Winkle, M., IND.ENG.CHEM.,44, 622 (1952). (67) Kobayashi, R., and Katz, D. L., paper presented before Division of Petroleum Chemistry a t the 121st Meeting of the AMERICAN CHEMICAL SOCIETY, Milwaukee, Wis., March 1952. (68) Kondo, S., and Fujita, S., Chem. Eng. (Japan),16, 186 (1952). (69) Kreg, D. R., Chem. Eng., 59, No. 6, 174 (1952). (70) Lamb, G. G., and Sitar, I. J., Chem. Eng. Progr., Symposium Ser., 48, No. 3, 99 (1952). (71) Leva, M., “Tower Packings and Packed Tower Design,” United States Stoneware Co., Akron, Ohio, November 1951. (72) Lindroos, A. E., and Dodge, B. F., Chem. Eng. Progr., Symposium Ser., 48, No. 3, 10 (1952). (73) Lindsey, E. E., Kiefer, J. M., and Huffine, C. L., IND.ENG. CHEM:,44, 225 (1952). (74) McIntire, R. L., Shelton, R. O., and Hachmuth, K. H., annual meeting Natural Gasoline Assoc. of America, Houston, Tex., 1952. (75) Marschner, R. F., and Burney, D. E., IND.ENQ.CHEM.,44, 1406 (1952). (76) Martin, J. J., Ibid., 44, 920 (1952). (77) Mayfield, F. D., Church, D. L., Jr., Green, A. C., Lee, D. C., Jr., and Rasmussen, R. W., Ibid., 44, 2238 (1952). (78) Miller, G. H., J . Chem. Educ., 29, 73 (1952). (79) Morris, W. L., IND.ENG.CHEM.,43, 2473 (1951). (80) Morton, F., Trans. Inst. Chem. Engrs. (London), 29, 240 (1951). (81) Murdoch, P. G., and Holland, C. D., Chem. Eng. Progr., 48, 2.54 (1952). (82) Ibid.: p’: 287: (83) National Carbon Division, Union Carbide and Carbon Corp., 30 East 42nd St., New York 17, N. Y., Catalog Section S-7350. (84) Nord, M., Chem. Eng. Progr., Symposium Ser., 48, No. 3, 55 (1952). (85) Norman, W. S., Trans. Inst. Chem. Engrs. (London),29, 226 (1951). ENQ.CHEM., 43, 2465 (1951). (86) Opler, A., and Heitz, R. G., IND. (87) Organick, E. I., and Brown, G. G., Chem. Eng. Progr., Symposium Ser., 48, No. 2, 97 (1952). (88) Othmer, D. F., Chugar, M. M., and Levy, S. L., IND.ENG. CHEM.,44, 1872 (1952). (89) Othmer, D. F., Silvis, S. J., and Spiel, A., Ibid., 44, 1864 (1952). (90) Othmer, D. F., Ten Eyck, E. H., and Tobias, S., Ibid., 43, 1607 (1951). (91) Otsuki, H., and Williams, F. C., paper presented at meeting Am. Inst. Chem. Engrs., Atlantic City, N. J., December 1951. (92) Payne, N., and Perrins, L. E., J. Appl. Chem. (London), 2 208 (1952). (93) Pennington, E. N., Poetmann, F. H., and Hachmuth, K. H., Annual Meeting Natural Gasoline Assoc. of America, Houston, Tex., 1952.
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(94) Perry, R. E., and Thodos, G., IND.ENG. CHEM.,44, 1649 (1952). (95) Peters, M. S., and Cannon, M. R., Ibid., 44, 1452 (1952). (96) Pigford, R. L., Tepe, J. B., and Garrahan, C. J., Ibid., 43, 2592 (1951). (97) Podbielniak, Inc., 341 East Ohio St., Chicago 11, Ill., “OctaDak” Announcement. (98) Pddbielniak, Inc., Brochure 10. (99) Pratt, H. R. C., Ind. Chemist, 26, 291, 470 (1950); 27, 3, 51, 152 (1951). (100) Pratt, H. R. C., Trans. Inst. Chem. Engrs. (London),29, 195 (1951). (101) Reamer, H. H., Sage, B. H., and Lacey, W. N., IND.ENG. CHEM.,43, 2515 (1951). (102) Ibid., 44, 609 (1952). (103) Ibid., p. 1671. (104) Redlich, O., Kister, A. T., and Turnquist, C. E., Chem. Eng. Progr., Symposium Ser., 48, No. 2, 49 (1952). (105) Reed, T. M., and Myers, H. S., IND.ENG.CHEM.,44, 914 (1952). (106) Rose, A., A n d . Chem., 24, 60 (1952). (107) Rose, A,, and Johnson, R. C., paper presented a t meeting Am. Inst. Chem. Ennrs.. Atlanta. Ga.. March 1952. (108) Rose, A., Johnson, R. C., and Williams, T. J . , IND. ENQ. CHEM.,43, 2459 (1951). (109) Rose,.A., Johnson, R. C., and Williams, T. J., paper presented a t meeting Am. Inst. Chem. Engrs., Atlanta, Ga., March 1952. (110) Rose, A,, and O’Brien, V. J., Jr., IND.ENG.CHEM.,44, 1480 (1952). (111) Rose, A., Williams, T. J., and Kahn, H. A,, Ibid., 43, 2502 f 1951). (112) Ibid., p.‘2608. (113) Rumford, F., “Chemical Engineering Operations,” London, Constable and Co., Ltd., 1951. (114) Rzasa, M. J., Glass, E. D., and Opfell, J. B., Chem. Eng. Progr., Sumposium Ser.. 48, No. 2. 28 (1952). . . (115) Sage, B . H., and Reamer, H. H., Ibid., 48, No, 2, 3 (1952). (116) Scientific Development Co., Box 795, State College, Pa., Bull. 12. (117) Scott, T. A , , Jr., MacMillan, D., and Melvin, E. H., IND. ENG.CHEM.,44, 172 (1952). (118) Skulman, H. L., and DeGroff, J. J., Jr., Ibid., 44, 1915 (1952). (119) Solomon, E., Chem. Eng. Proor., Symposium Ser., 48, No. 3, 93 (1952). (120) Stokes, C..S., and Hauptschein, M., Anal. Chem., 24, 1526 (1952). (121) Thornton, D. P., Jr., Petroleum Processing. 7, 623 (1952). (122) Thornton, J. D., and Garner, F.H., J. Appl. Chem. (London), 1, Supplement No. 1, S61 (1951). (123) Ibid., p. 568. (124) Ibid., p. S74. (125) Van Winkle, M., Petroleum Refiner, 31, No. 2, 111 (1952). (126) Watson, L. M., and Dodge, B. F., Chem. Eng. Progr., Symposium Ser., 48, No. 3, 73 (1952). (127) Wheeler, D. H., Foster, R. J.,and Berry, A. P., paper presented before the Division of Industrial Chemistry a t the 122nd Meeting of the AMERICAN CHEMICAL SOCIETY,Atlantic City, N. J. (128) Wheeler, E. L., “All Glass” Wheeler Fractionating Columns, Univ. Minnesota, Minneapolis, Minn. ENQ.CHEM.,44, 1664 (1952). (129) Whipple, 0. H., IND. (130) Wickert, J. N., Tamplin, W. S., and Shank, R. L., Chem. Eng. Progr., Symposium Ser., 48, No. 2, 92 (1952). (131) Wilcox, A. C., Coulter, K. E., and Lloyd, L. E., Petroleum Refiner, 31, No. 2. 134 (1952). . . (132) Williamson, G. J., Trans. Inst. Chem. Engrs. (London), 29, 215 (1951). (133) Wilson, A., and Simons, E. L., IND.ENG.CHEW,44, 2214 (1952). (134) Wilson, C. L., Petroleum Refiner, 31, No. 6 , 131 (1952). (135) Wilson, R. Q., Munger, H. P., and Clegg, J. W., Chem. Eng. Progr., Symposium Ser., 48, No. 3, 115 (1952). (136) Winn, F. W., Ibid., 48, No. 2, 121 (1952). (137) Yu, K. T., and Coull, J., Ibid., 48, No. 2, 38 (1952). (138) Zuiderweg, F. J., Chem. Eng. Sci., 1, 8 (1951). (139) Ibid., 1, 164 (1952). (140) Ibid., p. 174.
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