![]() Method of producing concentrated aqueous solution of sodium salt of methionine
专利摘要:
The invention relates to mercaptan derivatives and, in particular, the preparation of a concentrated solution of the NA salt of methionine used as additives to animal feed. The process is carried out by neutralizing the products of the saponification of 5- (β-methylmercaptoethyl) -hydantoin with sodium hydroxide, containing equimolar amounts of the NA salt of methionine and K 2 CO 3 , using H 2 SO 4 (taken in an amount necessary to neutralize the entire K 2 CO 3 ) at pH 10-12 and 100 ° C with removal of liberated CO 2 . The resulting solution is then concentrated to a methionine NA salt 45-55 g / 100 ml and the precipitated NA 2 SO 4 separated by filtration at 100 ° C to obtain a filtrate containing the NA salt of methionine and less than 1% mineral salts. These conditions provide a reduction in the content of mineral salts in the resulting target solution. 公开号:SU1503680A3 申请号:SU874202902 申请日:1987-07-16 公开日:1989-08-23 发明作者:Жиро Жан 申请人:Рон-Пуленк Нютрисьон Анималь (Фирма); IPC主号:
专利说明:
The invention relates to a method for producing an aqueous solution of methionine sodium salt used in animal husbandry as feed additives. The purpose of the invention is to reduce the concentration of mineral salts in an aqueous solution of the methionine sodium salt. Example 1. To 1000 g of the saponification products of 5 - (- methylmercaptoethyl) -hytantoin containing 164.6 g of methionine (or 1.105 mol) in the form of sodium salt and 98.32 g of sodium carbonate, sulfuric acid is added at 100 ° C. in an amount sufficient to neutralize sodium carbonate, at such a rate that the pH of the medium (measured at a temperature of about) was not lower than 10, carbon dioxide, which is released, is recovered. The resulting solution is concentrated so that the methionine sodium content is 46-55 g / 100 ml. The sodium sulfate which precipitates is separated by filtration at 100 seconds. In this way, a filtrate is obtained, the weight of which is 325 g and whose composition is as follows, g / 100 ml: methionine sodium 52; sodium sulfate 0.52. Carbon recovery rate gas 96% Example 2, To 1000 g of the product of 5- (p) methylmercaptoethyl) -hyndanone saphenis containing 164.3 g of methionyl about SA: O) 00 cm on (or I, 103 mol) in the form of the sodium salt and a total of 2, g-sodium atom, is slowly added with sulfuric acid in an amount sufficient to neutralize all the sodium. Recover carbon dioxide. Heat at for another 1 h to remove residual carbon dioxide. gas. Then, 62.5 cm of the hydantoin solution (sodium methionine and carbon monoxide of carbon dioxide) are added, for this it must be returned to the hydantoin synthesis stage, which complicates the technology. The method can also be carried out by neutralizing with sulfuric acid all sodium present in the saponification products of 5- (p-methylmercaptoethyl) ra hydroxide 50 g / 100 ml in sodium concentration of sufficient to neutralize methionine. The solution is concentrated so that the content of methionine sodium is 46 -15 52 g / 100 MP, the sodium sulphate which precipitates is separated by hot filtration. In this way, a filtrate is obtained, the weight of which is 342 g and whose composition is as follows, 20 g / 100 ml: methionine sodium 51.2; sodium sulfate 0.61. The degree of carbon dioxide recovery is 99%. As follows from the examples given, directly from the products of 5- (L-methylmercaptoethyl) -hydantoin saponification can be obtained an aqueous rast-Form thief methionium 1a sodium, containing Method 0.5-0.6 wt.% Mineral salts, then 30 aqueous solutions sodium salt 25 sodium), followed by treating the mixture with sodium hydroxide in an amount sufficient to form methionine sodium and mineral salts, and separating from solution after concentrating and recovering the carbon dioxide of the precipitated sodium sulfate, Thus, the practical use of concentrated solutions of methionine sodium salt instead of methionine solutions, the solubility of which in water is low, reduces the volume of liquids added to animal feed and facilitates methionine dosages of the required concentration. La invention of obtaining concentrated Yes, as in the known method, the amount of salt impurities reaches 2.9 wt.%. This effect is achieved as a result of the formation in the proposed method of precipitation of sodium sulfate, which has low solubility, easily crystallizes and is separated by filtration even when, unlike sodium carbonate, which is necessary to separate in the known method. On the other hand, the proposed method makes it possible to obtain sodium sulfate as a by-product practically pure, which is directly sold without further purification, as well as simultaneous recovery of carbon dioxide released during the treatment of saponification products. According to a known method, sodium carbonate is obtained, which cannot be used directly for utilization. Compiler G Editor I. Gorn Tehred M. Dida The form Method of the aqueous solution of sodium salt sodium), followed by treating the mixture with sodium hydroxide in an amount sufficient to form sodium methionine and mineral salts, and separating from the solution after concentrating it and recovering the carbon dioxide of the precipitated sodium sulfate, Thus, the practical use of concentrated solutions of methionine sodium salt instead of methionine solutions, the solubility of which in water is low, reduces the volume of liquids added to animal feed and facilitates the methionine dosage of the required concentration. sodium salt solution In the invention of obtaining concentrated methionine from the 5- (ft-methyl mercapto-ethyl) -hydantoin saponification products with sodium hydroxide, containing equimolar amounts of sodium methionine and sodium carbonate, by heating, in order to reduce the content of mineral salts in solution, The saponification products are treated with sulfuric acid in an amount necessary to neutralize the whole sodium carbonate, at a pH of 10-12 and a temperature of 100 ° with the removal of the liberated carbon dioxide, then concentrate the resulting Solution To precipitate sodium sulphate to a sodium salt of methionine 46-55 g / 100 ml, the precipitated sodium sulphate is separated by filtration at 100 ° C and a filtrate is obtained containing 1% methionine sodium salt and less than 1% mineral salts. Proofreader N. King
权利要求:
Claims (1) [1] The form of the Method of an aqueous solution of methionine sodium salt from the saponification products of 5 (ft-methylmercaptoethyl) -hidantoin sodium hydroxide containing annular amounts of sodium thionine and sodium carbonate, heating, characterized in that, in order to reduce the content of mineral salts in the solution, the saponification products are treated sulfuric acid in the amount necessary to neutralize all sodium carbonate, at a pH of 10-12 and a temperature of 100 ° £ with the removal of carbon dioxide, then the resulting solution is concentrated methionine sodium salt 46-55 g / SОml, precipitated sodium sulfate is separated by filtration at 100 ° С and a filtrate, methionine lei, is obtained.
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同族专利:
公开号 | 公开日 DE3762967D1|1990-07-05| EP0253740A1|1988-01-20| JPS6327472A|1988-02-05| FR2601674B1|1988-09-23| ES2015074B3|1990-08-01| EP0253740B1|1990-05-30| CA1279329C|1991-01-22| KR950004048B1|1995-04-22| AT53202T|1990-06-15| KR880001586A|1988-04-25| JPH0681742B2|1994-10-19| FR2601674A1|1988-01-22| US4789686A|1988-12-06|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 FR934407A|1945-10-10|1948-05-21|Merck & Co Inc|Improved process for producing amino acids and resulting products| US2642459A|1948-12-08|1953-06-16|Dow Chemical Co|Production and purification of amino acids| FR1532723A|1966-07-02|1968-07-12|Sumitomo Chemical Co|Process for making an alpha-amino acid| DE1643480A1|1966-10-12|1972-02-17|Nippon Kayaku Kk|Process for the preparation of 2-amino-4-substituted butyric acids and their intermediates| JPS5314537B2|1972-04-27|1978-05-18| US3920737A|1973-10-25|1975-11-18|Kanegafuchi Chemical Ind|Recovery of free methionine| JPS5715837B2|1978-04-03|1982-04-01| US4272631A|1980-02-25|1981-06-09|Diamond Shamrock Corporation|Hydrolysis of 5--hydantoin| DE3105005A1|1981-02-12|1982-08-19|Degussa Ag, 6000 Frankfurt|Process for the preparation of aqueous sodium methioninate solutions | DE3105007A1|1981-02-12|1982-09-09|Degussa Ag, 6000 Frankfurt|METHOD FOR PRODUCING AQUEOUS SODIUM METHIONINATE SOLUTIONS | DE3104997A1|1981-02-12|1982-08-26|Degussa Ag, 6000 Frankfurt|METHOD FOR PRODUCING AQUEOUS SODIUM METHIONINATE SOLUTIONS |DE19822099A1|1998-05-16|1999-11-18|Degussa|Process for the preparation of aqueous sodium methioninate solutions and use of these solutions for the production of granules| IT1320794B1|2000-08-08|2003-12-10|Filozoo Aventis S R L|PROCEDURE AND SYSTEM FOR PROVIDING NATURALLY SIMILAR AMINO ACIDS AND LIQUID-DERIVED AMOIDS TO RUMINATED ANIMALS.| US7318943B2|2002-02-27|2008-01-15|Archer-Daniels-Midland Company|Feed supplement for increasing the plasma amino acid level of ruminant livestock and method of administration| ES2365849T3|2004-02-14|2011-10-11|Evonik Degussa Gmbh|PROCEDURE TO PRODUCE METIONIN.| CN103772246A|2014-03-03|2014-05-07|重庆紫光化工股份有限公司|Method and special equipment for preparing methionine employing ion-exchange acidification methionine salt|
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申请号 | 申请日 | 专利标题 FR8610399A|FR2601674B1|1986-07-17|1986-07-17|PROCESS FOR THE PREPARATION OF AN AQUEOUS SOLUTION OF METHIONINE SODIUM SALT| 相关专利
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