Method for preparing L-methionine by using acetylated saponification solution

A technology of acetylmethionine and acetylmethionine, which is applied in the chemical industry, can solve the problems of increasing the cost of L-methionine, and achieve the effects of low production cost, high speed and high purity

Active Publication Date: 2013-10-09
NINGXIA UNISPLENDOUR TIANHUA METHIONINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, in the above-mentioned documents, the raw materials D and L-methionine for preparing L-methionine are all purified D, L-methionine commercial products, and their purity is above 98%, which will inevitably lead to an increase in the cost of L-methionine. However, there is no report on the direct use of the saponified liquid obtained from the hydrolysis of D,L-methylthioethylhydantoin (hydantoin) in the process of producing D,L-methionine to directly produce D,L-acetylmethionine.

Method used

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  • Method for preparing L-methionine by using acetylated saponification solution
  • Method for preparing L-methionine by using acetylated saponification solution
  • Method for preparing L-methionine by using acetylated saponification solution

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Experimental program
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Effect test

Embodiment 1

[0043] The 5-(2-methylthioethyl)-hydantoin (Ziguang Tianhua Methionine Co., Ltd.) was decolorized with activated carbon and then hydrolyzed with sodium hydroxide to obtain the saponified solution. For example, after adding sodium hydroxide, heat the hydrolysis reaction system to 130°C to 165°C to fully hydrolyze. The saponified solution obtained by hydrolysis is directly used in the following examples to produce D,L-acetylmethionine.

[0044] The saponification solution is composed of the following components: 17%±2% by mass of L,D-methionine sodium, 11%±2% by mass of sodium carbonate, and the rest of the water medium.

Embodiment 2

[0046] Get 200 kilograms of saponification liquid after the decolorization mentioned in embodiment 1, analyze the composition of saponification liquid: D, the content of L-sodium methionine is 15%, and sodium carbonate content is 10%, and surplus is water. The way of decolorization adopts activated carbon.

[0047] Slowly add 27 kg of acetic anhydride dropwise to the saponification solution to carry out the acetylation reaction, and control the reaction temperature at 45°C. During the reaction, the rate of addition is mainly controlled to avoid excessive bubbles. When the volume of acetic anhydride dropped to 1 / 2, a large number of carbon dioxide bubbles will be generated; the reaction time is 5 hours, and D,L-acetylmethionine sodium will be generated.

[0048] The reaction process was observed by thin-layer chromatography, the developer was n-butanol: water: acetic acid = 4:1:1, the chromogenic agent was ninhydrin chromogenic method, and the chromatographic plate was silica ...

Embodiment 3

[0050] Get 200 kilograms of saponification liquid after the decolorization mentioned in embodiment 1, analyze the composition of saponification liquid: D, the content of L-methionine sodium is 19%, and sodium carbonate content is 13%, and surplus is water.

[0051] Slowly add 27 kg of acetic anhydride dropwise to the saponification solution to carry out the acetylation reaction. Control the reaction temperature at 35°C. During the reaction, the rate of addition is mainly controlled to avoid excessive bubbles. When the volume of acetic anhydride dropped to 1 / 2, a large number of carbon dioxide bubbles will be generated; the reaction time is 5 hours, and D,L-acetylmethionine sodium will be generated.

[0052] The reaction process was observed by thin-layer chromatography, the developer was n-butanol: water: acetic acid = 4:1:1, the chromogenic agent was ninhydrin chromogenic method, and the chromatographic plate was silica chromatographic plate . The acetylation rate of D,L-me...

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Abstract

The invention relates to a preparation method of L-methionine aiming at the field of the chemical industry. The preparation method comprises the following steps of: adding acid into an acetylated saponification solution which is used as a production raw material to adjust the pH, cooling and then performing crystallization to obtain D,L-acetylmethionine crystals; and adding the obtained D,L-acetylmethionine into amino invertase to perform resolution reaction so as to obtain L-methionine, and recycling remainders. According to the method, links for refining D,L-methionine are reduced, the saponification solution for producing the D,L-methionine is directly used for performing acetylation reaction, and the yield is up to 99%; and besides, neutralization and separation steps for production of the D,L-methionine are reduced, the L-methionine obtained by performing enzymolysis on recrystallized D,L-acetylmethionine at an enzymolysis speed which is higher than that of the conventional method is better in crystal form and whiteness, the purity is more than 99.5%, and the total yield of the L-methionine is improved to 70%. The preparation method is a comprehensive cycle process which is reasonable in design and reduces the production cost.

Description

technical field [0001] The invention aims at the field of chemical industry and relates to a method for preparing L-methionine, in particular to a method for jointly preparing L-methionine by using D,L-methionine to produce saponification liquid. Background technique [0002] L-methionine, as a common reagent in biochemical research and a routine nutritional supplement, is also widely used in the adjuvant treatment of pneumonia, liver cirrhosis and fatty liver. At present, a variety of preparation methods of L-methionine have been reported, but most of the preparation methods are still in the laboratory stage, and only a few methods can be used in industrial production later. Among these methods, the commonly used means are enzymatic resolution or enzymatic cleavage, such as in the US patents of US6114163 and US6524837, enzymatic resolution of D, L-acetyl-methionine or enzymatic cleavage of D, L-methylthioethyl Hydantoin. [0003] In the prior art, the aminotransferase rou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/58C07C323/59C07C319/20
Inventor 吴传隆郑道敏姚如杰王用贵陈宏杨任星宇朱丽利
Owner NINGXIA UNISPLENDOUR TIANHUA METHIONINE CO LTD
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