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Method for preparing methylthioamino acid or alkali salts thereof

A technology of methionine and alkali metal salts, applied in the field of preparation of D, can solve the problems of easy formation of lumps, poor fluidity, crystal cakes cannot be washed thoroughly, and achieve good stability

Inactive Publication Date: 2005-01-12
EVONIK DEGUSSA GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This makes the product difficult to filter and the crystal cake cannot be washed thoroughly, moreover, the resulting D,L-methionine has poor fluidity and tends to form lumps

Method used

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  • Method for preparing methylthioamino acid or alkali salts thereof
  • Method for preparing methylthioamino acid or alkali salts thereof
  • Method for preparing methylthioamino acid or alkali salts thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-4

[0076] Example of the preparation of 5-(2-methylthioethyl)-hydantoin

Embodiment 1

[0079] Use the equipment in accompanying drawing 1. At the beginning, water was heated to 90°C and circulated; a solution containing 10.5 moles of hydrogen cyanide in 10 moles of 3-methylthiopropanal and 6.8 liters of ammonium carbonate aqueous solution containing 9.6 wt.% ammonia and 15.2 wt.% carbon dioxide Added to the cycle every 1 hour. The circulation volume in the circulation system is 300 liters per hour. The reaction temperature was kept at 90°C and the pressure was 1.4×10 6 Pa. A volume of reaction mixture corresponding to the volume entering the recycle is removed from the recycle system and passed to the secondary reaction. The average residence time in the circulation system is 10 minutes and in the secondary reaction is 2 hours. The yield of 5-(2-methylthioethyl)-hydantoin or the compound saponifiable to methionine was 99.8%, based on the amount of 3-methylthiopropanal used. (Specifically, it is counted as 100% based on 3-methylthiopropanal).

Embodiment 2

[0081] The same procedure as Example 1 was followed, except that a saturated ammonium carbonate solution containing 9.6 wt.% ammonia and 15.2 wt.% carbon dioxide at room temperature was circulated initially instead of water. The yield is 99.7%.

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PUM

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Abstract

A process for the preparation of methionine or a salt of methionine by reaction of the components 3-methylmercaptopropionaldhyde, hydrogen cyanide, ammonia and carbon dioxide or components from which the above-mentioned components can be prepared, optionally in the presence of water, to 5-(2-methylmercaptoethyl)-hydantoin and further reaction thereof to methionine or the salt thereof, characterised in that the reaction of the components is initiated by means of at least one premixture in such a way that a first mixture is formed containing at least the predominant proportion (at least 5 / 10) of the 3-methylmercaptopropionaldeyde and at least 1 / 10 of the hydrogen cyanide component or corresponding quantities of components from which these components can be prepared, and less than 5 / 10 of one of the components ammonia, carbon dioxide or of the components from which ammonia or carbon dioxide can be prepared, and in that this first mixture is combined with the other component(s) for the reactive conversion to 5-(2-methylmercaptoethyl)-hydantoin, wherein this (these) latter component(s) may be premixed in one or more other mixtures.

Description

technical field [0001] The present invention relates to preparation D, the preparation method of L-methionine or D, L-methionine salt, this method can component 3-methylthio propionaldehyde, hydrogen cyanide, ammonia and carbon dioxide or 5-( Starting from the salts of 2-methylthioethyl)-hydantoin or methionine, it is also possible to start with the preparation of the above-mentioned components, water optionally being present in the process. [0002] The synthetic steps can be represented by the following reaction formula: [0003] Formation of 5-(2-methylthioethyl)-hydantoin: [0004] [0005] D, Formation of L-methionine salt: [0006] [0007] D, Release of L-methionine: [0008] [0009] M represents an alkali metal, alkaline earth metal, ammonium, preferably potassium. Preferably, the steps of 5-(2-methylthioethyl)-hydantoin formation, D,L-methionine salt formation and D,L-methionine release are carried out continuously, preferably in Subsequent steps are in...

Claims

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Application Information

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IPC IPC(8): C07C319/20C07C319/28C07C323/58C07D233/76
CPCC07C319/28C07C319/20C07D233/76C07C323/58
Inventor F·盖吉B·哈斯伯格H-J·哈塞尔巴赫K·亨茨彻尔K·霍斯马彻M·科弗S-P·曼斯费尔德H·坦纳F·塞森J·宛罗贝斯K·威利吉罗特
Owner EVONIK DEGUSSA GMBH