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United States Patent Office Patented July 28, 1964

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United States Patent Office Patented July 28, 1964 3,142,638 United States Patent Office Patented July 28, 1964 2 3,42,638 been carried through pipe, conduit, or sewers. In some PROCESS FOR SEPARATING SOLIDS embodiments of our invention, the concentrations of FROM SEWAGE wastes of significance to the application at hand may be Donald Stapf Blaisdeil, 780 Sanamit Ave., St. Paul, Minn., only a few parts per million, and in other embodiments and Ruth Elizabeth Barry Klaas, 353 Ridgewood the concentrations may be as high as 10,000 parts per Road, Ardeia Sis, Miinae. milion or even higher. Unless otherwise defined in this a. No Drawing. Fied June 29, 1962, Ser. No. 265,184. specification, the definitions of the terms and tests we 7 Cains. (C. 250-52) use are those set forth in the book, "Standard Methods for the Examination of Water, Sewage, and Industrial This invention relates to the treatment of sewage, and 10 Wastes,' Tenth Edition, published in 1955 by the Ameri this application is a continuation-in-part of application can Public Health Association, of New York City, and for U.S. Letters Patent Serial Numbers 724,785 (filed such standard handbooks and textbooks of chemistry March 31, 1958, now abandoned) and 786,906 (filed as: Lange, "Handbook of Chemistry,” Handbook Pub January 15, 1959 now abandoned) by the present in lishers, Inc., Sandusky, Ohio, 1944; Latimer and Hilde ventors. More specifically, this invention relates to novel 5 brand, “Reference Book of Inorganic Chemistry,” Re compositions useful as additives for sewage, and to novel vised Edition, The Macmillan Company, New York, processes for the treatment of sewage. 1940; Hildebrand, “Principles of Chemistry,” Fifth Edi It is an object of this invention to provide novel sewage tion, The Macmillan Company, New York, 1947; Fuson compositions from which suspended solids settie and and Snyder, "Organic Chemistry,” John Wiley & Sons, can be removed rapidly in treating mechanisms of simple 20 inc., New York, 1942; and Glasstone, “Textbook of design and modest size. Physical Chemistry,” Second Edition, D. Van Nostrand It is a principal object of this invention to provide a Co., Inc., New York, 1946. Thus, for example, the novel type of clarifying agent in the treatment of sewage, term "water-dispersible synthetic organic cationic poly which type of clarifying agent causes rapid flocculation electrolytic flocculating material' will be understood to and sedimentation of solids, either suspended, dissolved, 25 exclude (as being polyampholytic rather than cationic) or both, in said sewage, and makes said solids adapted even polyacrylamide-type polymers that under some con for easy and rapid removal from the major aqueous ditions may actually be anionic by reason of a minor component of Such sewage, at low cost in treating mecha content of carboxylic groups. (Compare Dow, "Separan nisms of simple design and modest size. 2610 In Waste and Sewage Treatment,” October 1956, It is a further principal object of this invention to 30 Dow Chemical Company, Midland, Michigan, and Chem provide novel processes for the treatment of sewage, ical Week, September 17, 1960, page 6.) In other words, wherein chemical additives may be employed to produce we regard an organic polyelectrolytic flocculating ma a treated water of relatively high degree of purity from terial as cationic only if the main bodies of the polymer aqueous liquors containing wastes, such as fecal matter molecules bear overall positive charges at pH levels or other contaminants, in treating mechanisms of simple 35 commonly encountered in sewage; since the ionization design and modest size. constant of the amine groups is polyacrylamide is about Another object is to provide a sewage slude of relatively 10-15, and the ionization constant of carboxylic groups higher solids content, and of relatively lower Volume per is about 10, a modified polyacrylamide polymer con unit volume of sewage treated, than obtained in present taining even a very low percentage of carboxylic groups chemical methods of treating sewage conventionally used. 40 would be anionic at some levels of pH commonly en Another object is to provide a sludge of modified countered in sewage, or the like, and such modified characteristics (e.g. filtration, dispersion, digestion charac polyacrylamide polymers are intended to be excluded teristics), as compared to the characteristics of sludges specifically from the class of materials defined in this obtained in conventional chemical methods of treating specification as "water dispersible synthetic organic cat sewage or such like liquors. 45 ionic polyelectrolytic flocculating material.” Still a further object is to provide waters of a relatively Chemical treatment of sewage, of course, is well known high degree of purity by chemical treatment of aqueous to those versed in the prior art. The voluminous litera liquors containing such wastes as sanitary sewage, in ture of this field mentions the use of the following ma dustrial wastes or other contaminants. terials, among others, in the treatment of sewage or raw Various other objects, advantages, and features of this 50 water: ferric chloride, ferric sulfate, ferrous sulfate, invention will become apparent to those skilled in the chlorinated copperas, calcium oxide, calcium hydroxide, art upon reading the specification and appended claims. aluminum sulfate, alkali hypochlorites, soda ash, activated A broad field of utility for our invention is, of course, silica, calcium carbonte, coal, diatomite, activated carbon, the treatment of municipal sewage. ammonium sulfate, sodium aluminate, sodium silico Sewage ordinarily is a dilute aqueous mixture of the 55 fluoride, sodium flouride, caustic, sulfuric acid, activated wastes from household and industry that is convenient glue, rosin size, pine oil, kerosense, copper sulfate, chlor and economical to carry away by water. As used in amine, sulfur dioxide, sodium sulfite, nitric acid, carbon this specification and the appended claims, the term dioxide, hydrochloric acid, oxygen, ozone, and chlorine. sewage refers to any of the ordinary types of aqueous In the prior art, iron and aluminum salts have been liquors containing significant amounts of wastes, such 60 used as coagulants or flocculants for sewage, and indeed as fecal matter, domestic wastes, industrial wastes, and have a limited degree of effectiveness for removing col such like, and is not to be construed as being limited loidal solids and very finely divided suspended matter. to meaning only aqueous liquors which in lay terms are Both the iron and aluminum salts sometimes used (ferric ordinarily called sewages, nor should it be construed as chloride, alum, and the like) have the property of form being limited to mean aqueous liquors which have actually 65 ing relatively insoluble flocs that enmesh suspended ma 3,142,638 as 4. terial in the sewage, some of which material is swept sued October 25, 1960); Chemical Week, 87 (August out of the sewage as the floc matrix is removed. Fron 6, 1960), pages 26-28; Chemical Week, 87, (September and aluminum salts have been used also in the coagula i7, 1960), page 16; Plant Management and Engineer tion of sewage sludge, particularly in the preparation ing, 23, (March 1961), pages 2 and 3; Aimone and of the sludge for dewatering. (Our compositions are Booth, U.S. Patent 2,740,522 (issued April 3, 1956); also useful in some degree for this purpose.) Contois, U.S. Patent 2,847,403 (issued August 12, 1958); Water-insoluble synthetic organic polyelectrolytes (ion Chemical Engineering, June 1956, page 148; Dow, “Sep exchange resins) have been used in the prior art in the aran. 2610 In Waste and Sewage Treatment,” (October conditioning of certain aqueous liquors, as described in 1956), Dow Chemical Co., Midland, Michigan; "Co the literature by one of us, and by many others in numer 0. agulant Aids,' Bulletin 410-12-2 (1957), Hagan Chem ous references. The performance of carboxylic ex icals & Controls, Inc., Pittsburgh, Pennsylvania; "Hagan changers in the removal of material from certain types Coagulant Aids Nos. 7, 11, and 18 Safe for Drinking of aqueous liquors, for example, has been described by Waters,” Hagan Bulletin 4104-1-12:#HC-5652, Hagan Kunin and Barry, in Industrial and Engineering Chem Chemicals & Controls, Inc., Pittsburgh, Pennsylvania; istry, 41, 1269-72 (1949); by Winters and Kunin, in 5 French Patent 1,123,970 (October 2, 1956); Australian Industrial and Engineering Chemistry, 41, 460 (1949); by Patent 200,883 (April 21, 1955); Uytenbogaart, U.S. McGarvey and Thompson, Industrial and Engineering Patent 2,236,930 (issued April 1, 1941); Ralston and s Chemistry, 43, 741 (1951); and by others. Such water Pool, U.S. Patent 2,315,734 (issued April 6, 1943); insolubie ion exchangers have never found widespread Wilson, U.S. Patent 2,419,930 (issued April 29, 1947); commercial usage in the treatment of municipal sewage, 20 McDonald, U.S. Patent 2,647,084 (issued July 28, 1953); by reason of their relative ineffectiveness especially in the Stautzenberger and MacLean, U.S. Patent 2,903,438 (is light of their high initial and operating costs, and the sued September 8, 1959); Suen and Schiller, Canadian general operational difficulties associated with the use Patent 589,309 (issued December 22, 1959); Weidner and of insoluble ion exchangers in aqueous liquors contain Dunlap, U.S. Patent 2,995,512 (issued August 8, 1961); ing suspended solids. British Patent 10,050 (October 30, 1906); and multi In the separation of suspended inorganic solids from tudinous other references.) Even relatively cheap ani aqueous liquors, of course, certain chemical coagulants onic organic polyelectrolytic coagulants diluted with have been found to be effective at least to some degree. massive amounts of inexpensive anionic polyelectrolytic (See, for example, British Patent 760,869.) flocculant aid such as clay (see Henry, U.S. Patent 2,296,- To date, however, no really satisfactory chemical clari 30 523, issued September 22, 1942, and Ryznar, U.S.
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