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United States Patent (19) 11 Patent Number: 4,808,406 Brinkman (45) Date of Patent: Feb

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United States Patent (19) 11 Patent Number: 4,808,406 Brinkman (45) Date of Patent: Feb United States Patent (19) 11 Patent Number: 4,808,406 Brinkman (45) Date of Patent: Feb. 28, 1989 54 PREPARATION OF CUPRC HYDROXDE 3,194,749 7/1965 Furness ................................. 204/96 COMPOSITIONS 3,231,464 1/1966 Dettwiler et al. .................. 424/140 3,428,731 2/1969 Furness ............................... 424/40 (75) Inventor: Norman C. Brinkman, Houston, Tex. 3,628,920 12/1971 Barker ................................... 23/315 3,635,668 1/1972 Barker ................................... 23/147 73 Assignee: Kocide Chemical Corporation, 4,418,056 11/1983 Gonzales ............................. 424/142 Houston, Tex. 4,490,337 12/1984 Richardson ..................... 423/604X (*) Notice: The portion of the term of this patent subsequent to Dec. 25, 2001 has been OTHER PUBLICATIONS disclaimed. Merck Index-9th ed, 1976, pp. 2631 & 1484. Butts-"Copper, The Science & Technology of Metal, (21) Appl. No.: 901,965 its Alloys & Cpds', pp. 813-815 (1970). 22 Filed: Aug. 28, 1986 Mellor-Comprensive Treatise of Inorganic & Theoreti cal Chemistry, vol. 3, pp. 142-146, 267-268, (1973). - Related U.S. Application Data Primary Examiner-Leonard Schenkman (63) Continuation of Ser. No. 678,291, Dec. 5, 1984, aban Attorney, Agent, or Firm-Kenneth H. Johnson; Richard doned. L. Moseley (51) Int. Cl* ............................................ A01N 59/20 57 ABSTRACT 52 U.S. C. ...................................... 424/140; 423/42; 423/43; 423/604; 424/143 A method for producing finely divided stable cupric 58) Field of Search ......................... 424/140; 423/604 hydroxide composition of low bulk density comprising contacting solutions of an alkali metal carbonate or 56) References Cited bicarbonate and a copper salt, precipitating a basic cop U.S. PATENT DOCUMENTS per carbonate-basic copper sulfate to a minimum pH Re, 24,324 5/1957. Furness ................................. 23/147 in the range of greater than 5 to about 6, contacting the l,800,828 4/1931 Furness ............................... 423/604 precipitate with an alkali metal hydroxide and convert 1,867,357 7/1932. Furness ... ... 423/604 ing basic copper sulfate to cupric hydroxide, within the 2,525,242.10/1950. Rowe .................................... 23/147 pH range of 7 to 11. 2,666,688 ll/1954 Furness ................................. 23/147 2,924,505 2/1960 Page et al. .............................. 23/14 31 Claims, No Drawings 4,808,406 1. 2 is treated, ammonia may be a biological poison, which PREPARATION OF CUPRICHYDROXIDE damages the effectiveness of the bacteria in the pond. COMPOSITIONS The ammoniacal process is further complicated in waste water treatment in that ammonia solubilizes the cupric This application is a continuation of application Ser. 5 hydroxide to a significant extent, thus further contami No. 678,291, filed 12-5-84 abandoned. nating the waste water with copper and reducing the copper content of the product. BACKGROUND OF THE INVENTION Historically unstable copper hydroxide has been pre 1. Field of the Invention pared and used in the "Bordeaux' and "Burgundy' The present invention relates to a method for produc 10 mixtures (named for the regions of France where the ing chemically and color stable cupric hydroxide com mixtures were first used as fungicides for grapes). The positions, suitable for use as a fungicide. In particular, Bordeaux mixture is obtained by adding copper sulfate the method employs a class of carbonate compounds as to a suspension of hydrated lime. The product is unsta intermediates and may be characterized as carbonate ble copper hydroxide. The Burgundy, mixture is ob process cupric hydroxide and is an improvement on 15 tained by adding sodium carbonate to a solution of similar types of processes by providing for control of copper sulfate to produce unstable basic copper carbon particle size and bulk density of the resultant product. ate (CuCO3Cu(OH)2). 2. Related Art In commonly owned U.S. Pat. No. 4,490,337 issued Cupric hydroxide, depending to a large extent on its Dec. 25, 1984 a carbonate process is disclosed wherein method of production may not be a stable material. For 20 an alkali metal carbonate is reacted with a soluble cop example, when a base such as sodium hydroxide, is per salt and the precipitate (copper carbonate) then added to a solution of water soluble copper salts, e.g., treated with alkali hydroxide to convert a major portion copper sulfate, a blue, gelatinous precipitate is formed of the precipitate to cupric hydroxide. The alkali metal that gradually turns black in color. This material is hydroxide regenerates the alkali carbonate. The process unstable and contains cupric oxide hydrate and cupric 25 is continued by alternately adding copper sulfate and oxide in addition to cupric hydroxide. alkali metal hydroxide. The alkali carbonate is an inter U.S. Pat. No. Re 24,324 disclosed a method for the mediate and alternating the additions may be repeated preparation of stable cupric hydroxide. This procedure 15 to 20 times in this manner. In this process the carbon comprised reacting substantially equal molar amounts ate radical must be preserved to provide the intermedi of copper sulfate and trisodium phosphate, to obtain a 30 ate for the alternating copper reaction and regeneration. copper containing precipitate. The precipitate is then The present invention is much simpler in that it is a one treated with sodium hydroxide in an amount sufficient step process and the liberation of carbon dioxide from to convert a major portion of the precipitate to cupric the reaction medium is encouraged and desirable. Fur hydroxide. The sodium hydroxide regenerates the triso thermore it has been found that the pH range is critical dium phosphate. The process is continued by alter 35 to produce stable cupric hydroxide composition. nately adding copper sulfate and sodium hydroxide. The present method has a significant advantage over The trisodium phosphate is an intermediate and the the related art in that neither ammonia, copper, nor alternating additions may be repeated 15 to 20 times in phosphate are introduced into waste water. Another this manner. A solid product is obtained by separating advantage is the presence of carbonate in the waste solids, washing and drying the precipitate. 40 water, which is a practiced and accepted method of Other methods of preparing phosphate-process cu buffering industrial effluents. A feature of the present pric hydroxide are disclosed in U.S. Pat. Nos. 2,924,505 invention is absence of pollutants in the waste water and 3,628,920. stream. Another advantage of the present method is the A particularly effective fungicidal and bactericidal production of much finer particles and much lower bulk copper material is disclosed in U.S. Pat. No. 3,428,731 45 density than presently available for similar materials. A wherein a stable dispersion of phosphate-process cupric further advantage is the use of aqueous dispersions of hydroxide is obtained in an aqueous medium by having the carbonate process cupric hydroxide directly as fo a pH in the range of about 7 to 9.5. This phosphate liage sprays without stickers (adhesive aids, such as stabilized cupric hydroxide is suitable for use as a fungi starch). cide because of its fine particle size and high surface 50 area, but is not suitable for most industrial applications SUMMARY OF THE INVENTION because of the phosphate ion which has been incorpo Briefly, the present invention relates to the method of rated in the final product and the resulting insolubles producing stable cupric hydroxide-cupric carbonate that are found in the reaction medium. composition which is suitable for use as an agricultural Another approach to producing stable cupric hy 55 fungicide, and provides a means to control particle size droxide is the ammonia-process cupric hydroxide, dis and bulk density of the cupric hydroxide-cupric car closed in U.S. Pat. Nos. 1,800,828; 1,867,357; 2,525,242; bonate product. The present method comprises a pro and 3,635,668. These materials are suitable for use as cess whereby a solution of alkali metal carbonate is chemical intermediates, however, the individual parti reacted with a solution of soluble copper sulfate salt cles are relatively course and exhibit varying degrees of 60 taken to a pH of greater than 5 to about 6 to form an fungicidal activity. The ammoniacal process also tends insoluble basic copper carbonate (also called cupric to produce cupric hydroxide of higher bulk density and carbonate)-basic copper sulfate intermediate with the lower surface area than the present method, hence evolution of carbon dioxide. The insoluble basic copper lower reactivity per unit time compared to the present carbonate-basic copper sulfate intermediate is then carbonate process cupric hydroxide. 65 reacted with an alkali metal hydroxide and taken to a Furthermore, inherent in an ammoniacal process is pH of 7 to 11 preferably from about 10.0 to about 10.8 the problem of further processing the effluent. For ex (more preferably 10.4 to 10.8) to form insoluble cupric ample, in the so called "bug ponds" where waste water hydroxide-cupric carbonate composition. The reac 4,808,406 3 4. tion is carried on in an aqueous medium. The pH con to the carbonate solution. The copper solution may be trol and alkali metal hydroxide (sodium hydroxide) either dilute or concentrated, however, a concentrated serve to increase the copper hydroxide ratio in the pres solution is preferred. When copper sulfate is prepared ent composition and to stabilize the azurite (blue copper by dissolving copper wire in sulfuric acid the presence carbonate) and inhibit its conversion to malachite. of free acid in the copper solution may prevent this The temperature of reaction would be generally in amount of copper from being added, since it is the ulti the range of 5 C. to 32° C. Cupric hydroxide-cupric mate pH (not less than 5) which controls this step.
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