ION EXCHANGE ROBERT KUNIN ROHM & HAAS CO., PHILADELPHIA, PA.
During 1951, the interest in ion exchange reached a new peak. The utilization of this unit operation on a large industrial scale has been widespread, ranging from the commercial production and use of water having an electrical resistivity of conductivity water to the recovery of antibiotics. Pharmaceutical and medical acceptance of ion exchange resins as a new form of internal therapy has been one of the new outstanding developments.
I
N T H E 1950 review of the developments in ion exchange, an analysis of the interest in this unit operation since 1900 was presented. The basis for this analysis was a survey of the number of articles appearing in Chemical Abstracts. It was quite evident t h a t the “interest index” indicated a marked and increasing interest in the new unit operation, ion exchange. The present review confirms this trend in t h a t the total number of ion exchange publications and the widespread distribution have not diminished. It must be recognized, however, t h a t any new development usually stimulates interest in many fields initially, and then finds its own level based on true utility rather than on curiosity. REVIEWS
Deuel and Hostettler (109)prepared an excellent review of ion exchange tracing the development from the early work of Way until the very recent work of the present day ion exchange resins. Other interesting general reviews have been prepared by Heinrich (189),Lesser (266),Sancho and Carpena (367),Walton (ado), and Fortune (1G). More fundamental summaries were prepared by Glueckauf (169,161),Pepper (333), and Ryabchikov and Terent’era (363). Recent developments of ion exchange applications have been reviewed by Austerweil (99,23) and others (9, 19,98,306,358).Reports (84,113) from the governmental laboratories of England and India stress the important role ion exchange is playing in their research programs. THEORY
Although considerable advances have been made in formulating a n ion exchange equilibrium relationship, inability t o account rigorously for the ion activities in the solid phase and inhomogeneity of most ion exchangers have presented formidable difficulties t h a t have not been overcome. Several attempts have been made in app1,ying rigorously the law of mass action. The more noteworthy attempts have been those of Argersinger, Davidson, and Bonner (17),Lowen (962,263), Austerweil @ I ) , Gregor (166),Reichenberg, Pepper, and McCauley (3&), Gapon and Gapon (152),Ekedahl, Hogfeldt, and Sillen (128), Stoenner (4Or),Hogfeldt, Ekedahl, and Sillen (190),Holm (191)’ and Cosgrove and Strickland (93). Donnan distribution studies on cation exchange resins have been conducted by Eriksson (132), Gregor (164),and Cassel (69)and a statistical thermodynamic study has been presented by Hamada (177). The acid-base equilibria of several cation exchange and anion exchange resins have been studied by Honda (199),Gupta (171),and Shah and Bafna (876). The relationship between the capacity of both anion exchangers and cation exchangers has been studied by Shukow and Brodska ja-Moskow (383). The adsorptive properties of several phenol formaldehyde-type resins have been studied by Bhatnagar (40,41) and Mukherjee and coworkers (179,302). The selectivity of the phenolic group for cesium has been conaidered as being the reason for the difference in behavior between
a sulfonic- and a phenol sulfonictype cation exchange resin (291). Other exchange ~- equilibrium studies have been made on silicates (161, S o l ) , bone (137),and charcoal (160). The rate of exchange in ion exchangsresins has been considered by Boyd, Adamson, and Myers (61)as being controlled primarily by either film diffueion or solid diffusion depending upon the nature and composition of the resin, temperature, and external concentration. Hiester (186) and Nelson (308) consider t h e rate of exchange as obeying a second-order reaction mechanism. Other rate studies have been made by Stach (400),Selke and Bliss (X?), and Samuelson, Gartner, and Johansson (366). Further advances in the development of the theory of ion exchange columnar operation6 have been made by Glueckauf and Duncan (166) and Sillen and his coworkers (386487). Displacement chromatographic studies have been conducted by Partridge and his coworkers (396,326). Various miscellaneous theoretical studies on ion exchange and related phenomena have been presented during the year. Barrer (99)has presented a study on the porosity of zeolite minerals. Adsorption of nonelectrolytes has been reported by Kipling (934)and polyelectrolyte studies have been presented by Deuel et al. (110)and Huizenga, Grieger, and Wall (901). An interesting note on electromigration in ion exchange resins Bas been published by Spiegler and Coryell(398). Fundamental studies on the nature of sulfonic acid-cation exchange resins have been reported by Gregor et d.(166). P r o p erties of strongly basic anion exchange resins have been presented by Wheaton and Bauman (447). The operating chsracteristics of these latter resins have been studied by Lindsay and D’Amico (267). An interesting paper on the adsorptive properties of cellulose has been presented by Davidson (97). Methods on the measurement of-the capacity of various exchangers have been proposed by Dbdek et al. (106),Gapon and Zhupakhina (153),Martinez (980),and Ongaro (318). Methods for studying the external volumes and swelling of ion exchange resins have been studied by Gregor et al. (167,168). WATER SOFTENING
One of the more interesting developments in water softening has been the use of resinous exchangers for the softening of the effluent of a hot-lime process. Reviews of this application including operational performance on a large scale have been published Kemmer (926), Lindsay, Wirth, and Durinski by Applebawn (16), (268),and Wirth and Butler (468). Banks (28)and Howson (196)have prepared economic studies on the ion exchange-water softening operation. Other aspects of water conditioning connected with ion exchange water softening have been presented in publications and patents ( l g , 14, $3, 136, 1-40,147, 197, 226, 280, 324, 341, 360,419,446). DEIONIZATION
The deionization of water by means of ion exchange resins
has achieved a new degree of importance due t o the development of the strongly basic anion exchange resins and the mixeci bed and
79
INDUSTRIAL AND ENGINEERING CHEMISTRY
80
Monobed deionization technique. These developments have found increased importance in the television, electric power, and other fields. The mixed bed and Monobed deionization technique has led to the commercial usage of water having the quality of conductance water. This technique has been studied by Kunin and McGarvey (250),Reents and Kahler (342)) Wesly and Gilwooci (158). The economics and plant performance of several deionization systems have been discussed by Argent (16), Kohler and Morrison (2381, Showell (383), Wade (434))Yoder (464), and Osmun and Wirth (322). Various miscellaneous aspects of deionization have been discussed in a series of publications (86, 108, 118,200,255,264,295,342,399). Included are regeneration techniques, apparatus, and sterilization detaiIs. Specific applications for deionization have been nylon (83), alcoholic beverfound in the fields of television (2?06), ice manufacture (130),oil (448,455), and sea water ages (35,82), treatment (8, 85). The use of ion exchange in the purification of sugar is still under active consideration by most investigators in the fields of corn, beet, and cane sugar refining. Several discussions applicable t o several fields of sugar refining have been published by Blann (43))Dymond ( l 2 6 ) , D u Toit et al. (l25),Jordan (216), Koviz (242),Mindler (292),Smit (389-591),and van Doormal (117). Many studies and notes on the specific use of ion exchange in beet sugar refining appeared during the past year (36,48, 55, 56, 103, 104, 112, 268, 269, 402, 410, 421, 467). Discussions and recommendations were made during the year covering the use of ion exchange in the treatment of molasses or the reduction of molasses formation (9,31, 101,311,351,364,S76), inversion of sucrose (389,391), decolorization of raw sugar (l73),and recoveryof by-products (58,94,138,141,274).
(w),
RECOVERY, PURIFICATION, AND P R E P A R A T I O N
Ion exchange resins are playing an important role in the recovery and purification of various metals and organic constituents and in the preparation of various products. The use of ion exchange for concentrating dilute solutions has been studied by Durant (123), Guntz (l70),Kot (241))and Sueta (4lf). Ion exchange has played an important role in the recovery of copper (439),tin (293),chromium (80), rhodium (88), and zirconium and hafnium (26). Purification of phosphoric acid (79,226,327) and hydrochloric acid (88)has been aided by a cation exchange resin. Other purifications include chemicals, such as formalin (81), methanol (393), hydrocarbons ( 1 7 6 ) , antibiotics (106, 139, 195,209,254,347,417),alkaloids (361,433),organic acids (202)) lactose (265,436-438),wine (169,319, 349, 362, 363), milk (8?,154,155), glycerol ( a l l ,466),and greases and fats (379). Ion exchange resins have been employed in the manufacture of free acids (l24,236,994), alkali (406,Cog),sodium bicarbonate (428),phosphates (ZOJ),colloids ( I 78, 180,296),gallium citrate (@), cobalt amines (3%)) tartrates (336), lubricants (217,218), dyes (3.48),and in flotation (181). BIOCHEMISTRY
The ion exchange resins have become of considerable importance in the study, isolation, and recovery of several biological and biochemical substances: proteins (37,157, 233, 346, @O), amino acids (7,39,66, 96,99,107,115,131, 249,427,429,&6), peptides (57),acids (l27), enzymes (71,72, 156, 415, 416), flavonoids (150, 300), cytochrome (324),carbohydrates (18, 95, 136, 377, 461, 462),vitamins (61,206, 219, 220, 230, 231, 240,264,329),hemin (306),hormones (328),glucose phosphates (287,371),lignin (349),hyaluronic acid (211, 212, ZZ4),blood (5,73,345,435),virus (84,244, 299),pectin ( I S ) , phthiotic acid (68), nucleic acids (89-91, 179, 187, 194, 203,227, 829,232, 239, .%?4O,266,270,271,290,307, 343, 426,430-432,443,463))and related materials (60, 60, 243,276,30.9,310,321,323, 388,401,441).
Vol. 44, No. 1
A N A L Y T I C A L CHEMISTRY
The use of ion exchange techniques in analytical chemistry continues to grow quite rapidly. Reviews of this application have been contributed by Futterknecht (147),Honda (195), Wickbold (452),Davies (99),and Stein and Moore (404). The chief utility for ion exchange appears to be that of separating ionic species (62,111, 148,236,314,366,424, 427). Analytical separations have included the separation of samarium and promethium (64),titanium and iron (465),iron and aluminum (418),radium and barium (425),rare earths (141,184, 186, 199,215, 228, 183, 396, 39?),zirconium and hafnium (198,245, 409), tantalum, niobium, and proactinium (214,24.4, 246, 247))vanadium (221)) rhenium ( 7 , do), alkali ions (63, 223, 450, 463),and cobalt and copper (304). The use of ion exchange resins for determining the concentration of electrolyte solutions has been further investigated (237, 267, 279, 320, 350, 451). Miscellaneous analytical applications of ion exchange include methods for the analysis of iron and copper in wine (163), complex studies (49, 174, 367), determination of potasbium (102, 149, 554), analysis of fluorides (BO), halogenh (59))streptomycin (406))lactic acid (385), thiamin and riboflavin (288), nicotinamide (222),aldehydes and ketones (169),gelatin (no), viscose (355))fruit acids (456), purines (3, 4),soils (340),and activity coefficients (92,285,366). Lecture experiments utilizing ion exchange have also been reported (70,213,338, 368). WASTE TREATMENT
Because of increased activity in the prevention of stream pollution, the use of ion exchange is being actively considered for the treatment of wastes. Several general reviews (74,146) have discussed the general possibilities for ion exchange in this field. Bloodgood and his coworkers (46,46,261) studied the use of ion exchange resins for treating cyanide and chromium wastes. Lauderdale and Emmons (252)and Ayres (24)proposed the use of ion exchange for the treatment of radioactive wastes. Mellor (286)investigated the use of ion exchange resins for the removal of trace elements from water and Mulvavy et al. (303) studied the use of ion exchange on sulfite waste liquors. CATALYSIS
Fundamental studies on the catalytic activity of ion exchange resins have been reported by Smith and Amundson (392), Bodamer and Kunin (47),Mariani (272, 27S),and Lawrence and Moore (253). I n addition, Runge (352)reviewed the applications for ion exchange resins as catalysts. Several patents and publications have appeared on the use of sulfonic acid-cation exchange resins as catalysts for reactions, such as sucrose inversion (&), esterification (359),preparation of acetals (116, 448), extraction of glycerol (4M),uronoside formation (349), dehydration of alcohols (281),condensations (78), ester hydrolyses (275), and vulcanization of rubber (374). ION E X C H A N G E RESIN P R E P A R A T I O N S
A considerable number of patents and a relatively small number of papers on the preparation of ion exchange resins appeared during 1951. It would be beyond the scope of this review to discusa these other than to merely list the references. The work of P e p per (331,332) on the sulfonated polystyrene-divinylbenzene copolymers has been outstanding. The remainder of the literature refers to patents on cation exchange resin syntheses (1,10, 11, 26, 27, 52, 100, 121, 134, 145, 183, 284, 298, 312, 2313, 316, 31 7,330,381, 422) and anion exchange resin syntheses (25,34, 65,83,119, 120, 122, 135, 188,207, 208, 248, 851,269, 282,M8, 315,316,336,337,369,370,449). Although still in an early developmental stage, membranes possessing ion exchange properties are now being studied by several investigators (6, 61,7'5, 188, 584 394,3996).
January 1952
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 MEDICAL APPLICATIONS
The medical applications of ion exchange resins are still of considerable interest and are now being extensively studied. Martin (877) has reviewed quite thoroughly the use of ion exchange resins as therapeutic agents. The use of cation exchange resins in the sodium reduction therapy for cardiac edema and hypertension (38, 77, i i 4 , i89, i33, 178, 860) and the use of an anion exchange resin for the treatment of peptic ulcers (68, 64, 148, i76, 278, 878,4O8,418 469,480)have received considerable attention. In addition, ion exchange resins have been suggested as a model for the production of gastric hydrochloric acid (414) and in the removal of fluorides as a preventative for fluorosis
(76). APPARATUS
There have been but a few papers and patents on new advances in equipment design for ion exchange apparatus (30,334, 339, 878, 464). ACKNOWLEDGMENT
The author wishes t o thank Frank McGarvey and Helen Tucker for their assistance in assembling many of the references and in obtaining many of the publications cited. BIBLIOGRAPHY
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. ,
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83
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