Патент USA US2259563код для вставки
2,259,563 Patented Oct. 21, 1941 UNITED STATES PATENT OFFICE 2,259,563 METHOD OF l'iIAKING GUANYL UREA SULPHAMATE William H. Hill, Mount Lebanon, Pa., assignor to American Cyanamid Company, New York, N. Y., a corporation of Maine No Drawing. Application December 30, 1939, Serial No. 311,939 4 Claims. (Cl. 260—553) The present invention relates to methods for ‘ producing guanyl urea sulphamate. * Example II Molar proportions of dicyandiamid, sulphamic The formation of this substance may be readily acid and water were slowly heated together. accomplished by hydrolyzing dicyandiamid with Suddenly, at about 80 to 100° C., a violent re sulphamic acid in the presence of water. As a 5 action took place, the contents of the beaker ris result of this reaction, a melt is formed con ing to the rim, then subsiding. The resultant taining guanyl urea sulphamate from which this product was a thick, glassy material, perfectly substance may be readily obtained in a purer clear, which gave with copper sulphate and so state by recrystallization from water. dium hydroxide a test indicating a mixture of Guanyl urea sulphonic acid may be obtained sulphonate and sulphamate since the solution from guanyl urea sulphamate by heating the was colored pink and contained a small amount latter to from 140 to 180° C. As a result of this of a pink precipitate. Continued heating in the reaction, there is evidence that some ammonium neighborhood of 160° C. and until no more am guanyl urea sulphonate is formed. The yields monia was evolved, resulted in a clear yellow of the free acid may, therefore, be increased by 15 melt which, when the same was leached with digesting the crude melt with water and a min water, was found to be substantially pure guanyl eral acid, such as sulphuric acid, or by protracted urea sulphonic acid contaminated with a mini heating of the melt until no more ammonia is mum amount of the ammonium-salt. This application is a continuation in part of evolved. ' 20 applicant's co-pending application Serial No. Example I 305,176, ?led November 18, 1939. 490 grams of sulphamic acid were mixed with While the invention has been described with 420 grams of dicyandiamid and 360 cc. of water particular reference to speci?c embodiments, it to form a thin paste. The mix was then heated, is to be understood that it is not to be limited during which time it assumed a yellow color and 25 thereto but is to be construed broadly and re became more ?uid. When the temperature stricted solely by the scope of the appended reached 75° C., it was evident that a reaction claims. was rapidly progressing and became violent at I claim: 95° C. At this point, the source of heat was re 1. A method of making guanyl urea sulpham moved, although the temperature continued to ate which comprises hydrolyzing dicyandiamid in rise to approximately 115° C. The reaction con the presence of sulphamic acid and water and tinued at this temperature for some time during recovering guanyl urea sulphamate therefrom. which period steam escaped and a clear yellow 2. The method of claim 1 in which molar pro melt resulted. After cooling, the solid product portions of sulphamic acid, dicyandiamid and was dissolved in water and a white crystalline 35 water are used. solid, identi?ed as guanyl urea sulphamate, re 3. The method of claim 1 in which sulphamic covered therefrom. acid, dicyandiamid and water are heated to sub Upon heating either the crude melt contain stantially 75° C. ing guanyl urea sulphamate or the recrystallized 4. The method of claim 1 in which the initial product to 160° C., the melt becomes foamy and 40 reaction mixture comprises essentially sulphamic ammonia escapes. After the reaction had sub acid, dicyandiamid and water in substantially sided, the product was found to contain substan the proportions of 4590;420:360, respectively, the tial quantities of guanyl urea sulphonic acid con mixture being heated to substantially 75° C. taining some of the ammonia salt thereof. A whereby a clear yellow melt results, treating the purer acid was obtained by digesting the crude melt with water and recrystallizing guanyl urea melt with water and a mineral acid such as sul phuric acid to liberate additional quantities of guanyl urea sulphonic acid. The latter was re covered in puri?ed form by recrystallization from 50 water. sulphamate therefrom. WILLIAM H. HILL.