Purification method for glufosinate-ammonium

A purification method and glufosinate-ammonium technology are applied in the purification field of chemicals, which can solve the problems of low yield, long process route, and product quality decline, and achieve the effects of low inorganic salt content, good industrialization prospect and simple steps.

Active Publication Date: 2016-05-04
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The crude product of glufosinate-ammonium hydrochloride contains a large amount of inorganic salt by-products such as ammonium chloride and produces viscous organic impurities. There are also relevant reports on the purification process of glufosinate-ammonium hydrochloride in China. For example, patent CN103819503 mentions that glufosinate-ammonium Phosphine hydrochloride is ammonified into salt, and then mixed with carbon dioxide to obtain glufosinate-ammonium acid. This process introduces ammonium bicarbonate during the reaction process, which needs to be removed by thermal decomposition in the final product, which will easily lead to a decline in product quality, and a large amount of carbon dioxide is used , low utilization
In patent CN201110160129, glufosinate-ammonium hydrochloride is sequentially subjected to esterification reaction, hydrolysis reaction and neutralization reaction with ethylene oxide to obtain glufosinate-ammonium acid, and finally ammonia gas is passed to obtain glufosinate-ammonium ammonium salt. The process route is long and consumes Large, low yield, ethylene oxide is used in the neutralization reaction, the operation risk factor is large, and the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 80 grams of crude glufosinate-ammonium hydrochloride (purity about 80%) into 100 grams of water, add ammonia water to adjust the pH to 8 at room temperature, remove 30 grams of water by vacuum distillation, and filter to remove ammonium chloride and other insolubles. Then add 30 grams of concentrated hydrochloric acid to adjust the pH value to 1, crystallize, filter, and dry to obtain 50 grams of off-white solids with a yield of 94% and a purity of 95%.

Embodiment 2

[0034] 80 grams of crude glufosinate-ammonium hydrochloride (purity about 80%) was added to 100 grams of methanol and water mixed solvent (1:1), 15 grams of sodium hydroxide was added at room temperature to adjust the pH to 9, and the pressure was reduced. 30 grams of mixed solvent was removed by distillation, ammonium chloride and other insolubles were removed by filtration, then 14 grams of concentrated sulfuric acid was added dropwise to adjust pH=1, crystallized, filtered, washed with methanol, and dried to obtain 49 grams of off-white solids with a yield of 92%. , 94% purity.

Embodiment 3

[0036] Add 80 grams of crude glufosinate-ammonium hydrochloride (purity about 80%) to 100 grams of water, add 30 grams of potassium carbonate at room temperature to adjust the pH to 7, remove 30 grams of water by vacuum distillation, and filter to remove ammonium chloride and other insolubles, dropwise added formic acid to adjust pH=3, crystallized, filtered, and dried to obtain 47 grams of off-white solids with a yield of 89% and a purity of 95%.

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Abstract

The invention relates to a purification method for glufosinate-ammonium. The method comprises the following steps that a glufosinate-ammonium hydrochloride crude product is dissolved into a solvent, then, alkaline is added to be subjected to a reaction, the pH value is adjusted to be 7-10, reduced pressure distillation is performed to remove some solvent, then filtering is performed to remove ammonium chloride and other undissolved substances; acid is added into the reaction solution to be subjected to a reaction, the pH value is adjusted to be 1-4.5, and then filtering and drying are performed to obtain glufosinate-ammonium acid; the glufosinate-ammonium acid is dissolved into the solvent, then, ammonia gas is introduced to be subjected to a salt forming reaction, glufosinate-ammonium solid is separated out, and filtering and drying are performed to obtain high-purity glufosinate-ammonium. According to the purification technology, fatty amine hard to remove and high-risk ethylene oxide and epoxypropane are prevented from being used, the steps are simple, the obtained glufosinate-ammonium is low in inorganic salt content and high in purity, yield and safety, water or alcohol is used as the solvent in the technological process, ammonium hydroxide and inorganic base are used for being subjected to a neutral reaction, the glufosinate-ammonium conforms to the environment-friendly and economical principle, and the good industrial prospect is achieved.

Description

technical field [0001] The invention belongs to a purification method of chemicals, in particular to a purification method of glufosinate-ammonium. Background technique [0002] Glufosinate-ammonium is a biocidal contact herbicide with the characteristics of high efficiency, low toxicity, low residue and safety. Its quick-acting property is between paraquat and glyphosate. It is widely used in agricultural production. The structural formula of glufosinate-ammonium is as follows : [0003] . [0004] The crude product of glufosinate-ammonium hydrochloride contains a large amount of inorganic salt by-products such as ammonium chloride and produces viscous organic impurities. There are also relevant reports on the research of glufosinate-ammonium hydrochloride purification process in China. For example, patent CN103819503 mentioned that glufosinate-ammonium hydrochloride was first Phosphine hydrochloride is ammoniated into a salt, and then combined with carbon dioxide to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 姜宇华周志豪丁菲徐洪喜薛红芬
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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