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A method for separating and purifying glufosinate-ammonium from hydrolysis reaction liquid

A hydrolysis reaction and glufosinate-ammonium technology, applied in the field of separation and purification of glufosinate-ammonium, can solve the problems of low yield and purity of glufosinate-ammonium, and low purification efficiency

Active Publication Date: 2020-07-07
HEBEI VEYONG BIO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Aiming at the problems of low yield, purity and low purification efficiency of glufosinate-ammonium in the existing glufosinate-ammonium purification process, the invention provides a method for separating and purifying glufosinate-ammonium from the hydrolysis reaction liquid

Method used

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  • A method for separating and purifying glufosinate-ammonium from hydrolysis reaction liquid
  • A method for separating and purifying glufosinate-ammonium from hydrolysis reaction liquid
  • A method for separating and purifying glufosinate-ammonium from hydrolysis reaction liquid

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Embodiment 1

[0045] A method for separating and purifying glufosinate-ammonium from hydrolysis reaction liquid:

[0046] Step 1. Take 1000 g of the hydrolysis reaction solution, stir, add sulfuric acid (mass content 92.5%) dropwise to pH = 1, the reaction releases a lot of heat, cool down with a water bath, keep the temperature at 15-70 ° C, and stir for 0.5 h after the dropwise addition is completed. Add ammonia water (20% by mass) dropwise to pH=6, stir for 0.5h, concentrate under reduced pressure to a thick state (mass about 700g) (solid content 80%), add 360g of methanol, stir at room temperature, take the clear liquid to measure the water content 20%, filtered at 15° C. for 4 h to obtain the mother liquor and the first filter cake, the first filter cake was washed with 230 g of methanol to obtain the washing filtrate, and the mother liquor and the washing filtrate were combined to obtain the first filtrate;

[0047] Step 2: Add 230 g of methanol to the first filtrate, adjust the water...

Embodiment 2

[0050] A method for separating and purifying glufosinate-ammonium from hydrolysis reaction liquid:

[0051]Step 1. Take 1000 g of the hydrolysis reaction solution, stir, add sulfuric acid (95% by mass) dropwise to pH = 2, the reaction releases a lot of heat, cool down with a water bath, keep the temperature at 15-70° C., and stir for 0.5 h after the dropwise addition is completed. Add ammonia water (mass content 25%) to pH = 8, stir for 0.5h, concentrate under reduced pressure to a thick state (mass about 930g) (solid content 60%), add methanol and ethanol with a volume ratio of 1:0.5 mixed alcohol 910g, stirred at room temperature, took the clear liquid to measure the moisture content of 25%, stirred at 30°C for 2h and filtered to obtain the mother liquor and the first filter cake. The first filter cake was washed with 580g methanol to obtain the washing filtrate, and the mother liquor and the washing Filtrate, get the first filtrate;

[0052] Step 2: Add 580 g of the above-...

Embodiment 3

[0055] A method for separating and purifying glufosinate-ammonium from hydrolysis reaction liquid:

[0056] Step 1. Take 1000 g of the hydrolysis reaction solution, stir, add sulfuric acid (98% by mass) dropwise to pH = 3, the reaction releases a lot of heat, cool down with a water bath, keep the temperature at 15-70° C., and stir for 0.5 h after the dropwise addition is completed. Add ammonia water (30% by mass) dropwise to pH = 7, stir for 0.5h, concentrate under reduced pressure to thick (mass about 800g) (solid content 70%), add methanol and ethanol with a volume ratio of 1:0.1 mixed alcohol 600g, stirred at room temperature, took the clear liquid to measure the moisture content of 23%, stirred at 70°C for 0.5h and filtered to obtain the mother liquor and the first filter cake. The first filter cake was washed with 280g methanol to obtain the washing filtrate, and the mother liquor and the first filter cake were combined. washing the filtrate to obtain the first filtrate; ...

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Abstract

The invention provides a method for separating and purifying glufosinate from a hydrolysis reaction solution. According to the method for purifying glufosinate, demineralization is conducted twice under the conditions of different water content by controlling the water content in the process of crystallization and demineralization, so that the problem of low yield and purity, caused by slow filtration and high content of residual glufosinate in salts during one-off demineralization, of the glufosinate product is solved. Through the method for purifying the glufosinate, the content of residualglufosinate in the final salts can be controlled at 0.2% or below, the purity of glufosinate can reach 98% or above, the yield reaches 96% or above, and the filtration time is shortened to 1 / 3 of theoriginal filtration time, and the purification efficiency is improved significantly; and the method has a simple process and requires no special equipment, high-efficiency purification of glufosinatecan be achieved through simple crystallization with alcohol, and therefore the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of pesticide production, in particular to a method for separating and purifying glufosinate-ammonium from a hydrolysis reaction liquid. Background technique [0002] Glufosinate-ammonium is a non-conductive herbicide with high efficiency, low toxicity, and environmental friendliness. It is easy to degrade in the soil, safe for crops, not easy to drift, has a wide spectrum of weeding, high activity, and low dosage, which is environmentally friendly. The pressure is small, and it is the world's largest tonnage pesticide variety. At present, the mature production process of glufosinate-ammonium mainly includes the addition of methyl phosphite diester and acrolein, followed by Strecker reaction, Bucherer-Bergs reaction, and hydrolysis reaction to obtain glufosinate-ammonium. The process route is as follows: [0003] Strecker route [0004] [0005] Bucherer-Bergs route [0006] [0007] In the two synt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 史秀肖范立攀马扩王双珠贾成国
Owner HEBEI VEYONG BIO CHEM
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