Method for separating and extracting L-glufosinate from enzymatical reaction liquid

A technology of glufosinate-ammonium and enzyme conversion is applied in the field of chemical-enzymatic production of amino acids, which can solve the problems of many acid-base solvents, high operation cost, complicated operation, etc., and achieve the effects of good product quality, low reagent cost and simple operation.

Active Publication Date: 2018-09-04
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method consumes more acid-base solvents, and the yield is lower, less than 80%.
[0005] In summary, there are few existing separation and purification methods about L-glufosinate-ammonium, and most of them are about the separation and extraction of racemic glufosinate-ammonium solution produced by chemical methods.
Moreover, most of the existing reported glufosinate-ammonium separation methods have problems such as complicated operation and high operating cost.

Method used

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  • Method for separating and extracting L-glufosinate from enzymatical reaction liquid
  • Method for separating and extracting L-glufosinate from enzymatical reaction liquid
  • Method for separating and extracting L-glufosinate from enzymatical reaction liquid

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Effect test

Embodiment 1

[0035] Embodiment 1: a kind of method for separating and extracting L-glufosinate-ammonium from enzyme conversion liquid, concrete steps are as follows:

[0036] (1) Enzyme conversion solution

[0037] Add 160g of N-phenylacetyl-D, L-glufosinate-ammonium into 900mL of water, adjust the pH of the solution to 8.5 with 17% ammonia water to dissolve N-phenylacetyl-D, L-glufosinate-ammonium, then dilute the solution to 1000mL , add 780U amidase (under optimal conditions, the amount of enzyme needed to catalyze the substrate to produce 1 μmol of product per minute, that is, 1 enzyme activity unit U, the same below), and react at 35°C for 8 hours. After the reaction, the obtained enzyme conversion solution mainly contains 50g / L L-glufosinate-ammonium, 36g / L phenylacetic acid, 80g / L N-phenylacetyl-D-glufosinate-ammonium and ammonium salt.

[0038] (2) Separation and purification

[0039] 1) Take 1L of the enzyme conversion solution and concentrate it under reduced pressure at 60°C u...

Embodiment 2

[0042] Embodiment 2: a kind of method for separating and extracting L-glufosinate-ammonium from enzyme conversion liquid, concrete steps are as follows:

[0043] (1) Enzyme conversion solution

[0044] Add 120g N-acetyl-D, L-glufosinate-ammonium into 900mL water, adjust the pH of the solution to 8.5 with 17% ammonia water to dissolve N-acetyl-D, L-glufosinate-ammonium, then dilute the solution to 1000mL, add 2400U acylase, react at 37°C for 48 hours. The enzyme conversion solution obtained after the reaction mainly contains 50g / L L-glufosinate-ammonium, 15g / L acetic acid, 59.7g / L N-acetyl-D-glufosinate-ammonium and ammonium salt.

[0045] (2) Separation and purification

[0046] 1) Take 1L of the enzyme conversion solution, and concentrate it under reduced pressure at 60°C until the volume of the enzyme conversion solution is 500ml. The ammonium salt and part of the acetic acid can be removed during the rotary evaporation process to obtain the L-glufosinate-ammonium concentr...

Embodiment 3

[0049] Embodiment 3: a kind of method for separating and extracting L-glufosinate-ammonium from enzyme conversion liquid, concrete steps are as follows:

[0050] (1) Enzyme conversion solution

[0051] Add 100g (R,S)-2-amino-4-(hydroxymethylphosphono)-butyramide to 900mL water, adjust the pH of the solution to 8.5 with 17% ammonia water, and make (R,S)-2-amino-4 -(Hydroxymethylphosphono)-butyramide was dissolved, then the solution was adjusted to 1000 mL, 500 U of amidase was added, and the reaction was carried out at 28° C. for 15 hours. After the reaction, the enzyme conversion solution obtained mainly contained 50g / LL-glufosinate-ammonium, 49.3g / L R-2-amino-4-(hydroxymethylphosphono)-butyramide, and ammonium ions.

[0052] (2) Separation and purification

[0053] 1) Take 1L of the enzyme conversion solution and concentrate under reduced pressure at 55°C until the volume of the enzyme conversion solution is 500ml. The ammonium salt and part of the acetic acid can be remove...

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Abstract

The invention discloses a method for separating and extracting L-glufosinate from enzymatical reaction liquid. When an enzyme catalysis method is adopted for producing the L-glufosinate, enzyme catalysis liquid contains not only the L-glufosinate, but also impurities including enzyme or thalli, byproducts(normally organic matters), unreacted D-type substrates, ammonium salt and the like, and due to the fact that the L-glufosinate has such characteristics as being soluble in water and insoluble in organic solvent, separation and extraction difficulty levels are high; the method for separating and extracting the L-glufosinate mainly includes the following three steps of (1) pre-treatment, (2) an ion exchange method and (3) crystallization; the purity of the product finally obtained reaches 98% or above, and the yield reaches 98% or above. According to the method, the technological process is short, operation is simple, the application range is wide, the cost is low, the yield of the L-glufosinate is high, and the product quality is high.

Description

technical field [0001] The invention relates to a method for separating and extracting L-glufosinate-ammonium from an enzyme conversion liquid, and belongs to the technical field of chemical-enzymatic production of amino acids. Background technique [0002] Glufosinate ammonium, also known as glufosinate, is an organophosphorus herbicide developed by Hearst AG (now Bayer AG) of Germany. The chemical formula of glufosinate-ammonium is C 5 h 12 NO 4 P, easily soluble in water, not easily soluble in organic solvents, stable to light. Glufosinate-ammonium has the characteristics of high efficiency, low toxicity, broad-spectrum, killing, etc., and with the delisting of paraquat, and more and more difficult-to-kill weeds resistant to glyphosate and paraquat, glufosinate-ammonium With its unique weeding mechanism, it has broad market prospects. Currently commercially available glufosinate-ammonium is a racemic mixture, but only the L-configuration glufosinate-ammonium has herb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 薛亚平郑裕国郭宇星徐建妙程峰
Owner ZHEJIANG UNIV OF TECH
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