Post-treatment method of L-glufosinase hydrolysate

A technology of glufosinate-ammonium and hydrolyzate, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of low yield and low purification efficiency of L-glufosinate-ammonium , to achieve the effects of reducing the amount of three wastes produced, simple operation and low cost

Pending Publication Date: 2020-08-25
HEBEI VEYONG BIO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention provides a post-treatment method for L-glufosinate-ammonium enzyme hydrolyzate, so as to solve the problems of low yield and low purification efficiency in the preparation of L-glufosinate-ammonium by biological method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 1L L-glufosinate-ammonium enzyme hydrolyzate, which is composed of: L-glufosinate-ammonium, phenylacetic acid, N-phenylacetyl-D-glufosinate-ammonium, ammonium salt, sodium salt, etc., wherein the content of L-glufosinate-ammonium is 49.5 g / L, concentrated under reduced pressure at 70°C to about 250mL, added concentrated sulfuric acid to adjust the pH value of the solution to 1-2, stirred and crystallized at 15°C, filtered to remove most of the phenylacetic acid and N-phenylacetyl-D glufosinate-ammonium in the solution, The filtrate is the pretreatment liquid; in the pretreatment liquid, add 150 mL of n-butanol at a time, extract twice, and extract the residual phenylacetic acid and N-phenylacetyl-D-glufosinate-ammonium in the solution into the n-butanol phase, statically After liquid separation, collect the water phase; add 30g of 20% ammonia water to the water phase to adjust the pH value to 7-8, concentrate under reduced pressure at 80°C to a residual weight of 10...

Embodiment 2

[0025] Take 1L L-glufosinate-ammonium enzyme hydrolyzate, which is composed of: L-glufosinate-ammonium, acetic acid, N-acetyl-D-glufosinate-ammonium, ammonium salt, sodium salt, etc., wherein the content of L-glufosinate-ammonium is 40.2g / L, concentrated under reduced pressure at 70°C to about 400mL, added concentrated sulfuric acid to adjust the pH value of the solution to 1-2, stirred and crystallized at 15°C, filtered to remove most of the acetic acid and N-acetyl-D glufosinate-ammonium in the solution, and the filtrate was the pre- Treatment solution: Add 130 mL of n-butanol to the pretreatment solution each time, extract twice, extract the residual phenylacetic acid and N-phenylacetyl-D-glufosinate-ammonium in the solution to the n-butanol phase, and let it stand for liquid separation , collect the water phase; add 22g of 20% ammonia water to the water phase to adjust the pH value to 7-8, concentrate under reduced pressure at 80°C until the residual weight reaches 75g, ad...

Embodiment 3

[0027] Take 1L L-glufosinate-ammonium enzyme hydrolyzate, which is composed of: L-glufosinate-ammonium, phenylacetic acid, N-phenylacetyl-D-glufosinate-ammonium, ammonium salt, sodium salt, etc., wherein the content of L-glufosinate-ammonium is 49.5 g / L, concentrated under reduced pressure at 70°C to about 250mL, added concentrated sulfuric acid to adjust the pH value of the solution to 1-2, stirred and crystallized at 15°C, filtered to remove most of the phenylacetic acid and N-phenylacetyl-D glufosinate-ammonium in the solution, The filtrate is the pretreatment liquid; in the pretreatment liquid, add 150 mL of benzyl alcohol each time, extract twice, and extract the remaining phenylacetic acid and N-phenylacetyl-D-glufosinate-ammonium in the solution to the benzyl alcohol phase, stand and separate After liquid, collect the water phase; add 30g of 20% ammonia water to the water phase to adjust the pH value to 7-8, concentrate under reduced pressure at 80°C until the residual w...

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Abstract

The invention discloses a post-treatment method of an enzymatic hydrolysate of L-glufosinate-ammonium. The enzymatic hydrolysate of L-glufosinate-ammonium prepared by a biological enzyme resolution method is treated by four steps of pretreatment, extraction, desalination and crystallization; impurities such as unreacted D-glufosinate-ammonium derivatives, generated organic acids, ammonium salts and sodium salts are removed, and L-glufosinase of which the yield is greater than 98%, the content is greater than 98%, and the ee value is greater than 99% is obtained. According to the method, a traditional cation exchange resin passing mode is replaced with an extraction mode so that the method is simpler, more convenient and feasible, the purification efficiency is high, the extraction agent can be recycled, and the yield of three wastes is greatly reduced.

Description

technical field [0001] The invention relates to the field of biochemical industry, in particular to a post-treatment method of L-glufosinate-ammonium enzyme hydrolyzate. Background technique [0002] At present, the methods for preparing L-glufosinate-ammonium at home and abroad mainly include the synthesis of L-glufosinate-ammonium with natural amino acids as chiral raw materials, asymmetric reactions catalyzed by chiral catalysts, chemical-biological methods and the synthesis of glufosinate-ammonium racemates. Chiral resolution of these four methods. Among them, the three methods of synthesizing L-glufosinate-ammonium using natural amino acids as chiral raw materials, asymmetric reactions catalyzed by chiral catalysts, and chemical-biological methods all have the disadvantages of long reaction steps and low overall yields. The biological method is to use biological enzymes to selectively catalyze the reaction of L-glufosinate-ammonium derivatives to obtain L-glufosinate-a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 范立攀史秀肖贾成国范朝辉
Owner HEBEI VEYONG BIO CHEM
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