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New method or preparing glufosinate ammonium salt

A technology of glufosinate-ammonium and ammonium chloride is applied in the field of preparation technology of glufosinate-ammonium salt, which can solve the problems of long route, cumbersome steps, increase cost and the like, and achieve the effects of high industrialization prospect, simple preparation process and economical cost.

Active Publication Date: 2016-04-13
ZHEJIANG XINAN CHEM INDAL GROUP
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AI Technical Summary

Benefits of technology

The technical effect of this new method described by this patented technology can be improved efficiency compared with current methods while also reducing costs associated therewith. This results from making it easier for people working at large scales or producing products that are safe without harmful chemicals like ethylene glycol (EG).

Problems solved by technology

This patented technical problem addressed in this patent relates to improving the efficiency at killing unwanted plants such as harmful vegetables or crops while reducing their resistance to other chemicals like glyphocide.

Method used

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  • New method or preparing glufosinate ammonium salt

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Embodiment 1

[0020] Take 34.5g (0.2mol) of methyl phosphonate, under stirring, add to the mixed solution containing 14.8g of sodium cyanide, 22.4g of ammonium chloride, 136g of 15% ammonia water, and react at a temperature of 15°C for 6 hour, then slowly add 120g of 37% hydrochloric acid, heat up to 95°C, react for 4 hours, concentrate the deacidified water under reduced pressure, add 125g of methanol, reflux esterification, the esterification temperature is 70°C, and the esterification time is 5 hours. After the end, cool down to 35°C, pass ammonia until the pH of the reaction solution is 6.5, react for 0.5 hours, then cool down to 10°C, separate and filter the insoluble ammonium chloride, and obtain a methanol solution of glufosinate-ammonium ester. Concentrate under reduced pressure to dealcoholize, add 34g of 10% ammonia water, and carry out ammoniation reaction. The reaction temperature is 5-10°C, and the reaction time is 3 hours. After the reaction, concentrate under reduced pressure,...

Embodiment 2

[0022] Take 34.5g (0.2mol) of methyl phosphonate, under stirring, add to the mixed solution containing 14.8g of sodium cyanide, 22.4g of ammonium chloride, 95g of 22.5% ammonia water, at a temperature of 10°C React for 5 hours, then slowly add 150g of 30% hydrochloric acid, heat up to 90°C, react for 4 hours, concentrate the deacidified water under reduced pressure, add 125g of methanol, reflux esterification, the esterification temperature is 70°C, and the esterification time is 5 hours. After the esterification, cool down to 35°C, pass ammonia until the pH of the reaction solution is 7, react for 0.5 hours, then cool down to 10°C, separate and filter the insoluble ammonium chloride to obtain a methanol solution of glufosinate-ammonium ester. Concentrate under reduced pressure to dealcoholize, add 44g of 8% ammonia water, and carry out ammoniation reaction. The reaction temperature is 5-10°C, and the reaction time is 3 hours. After the reaction, concentrate under reduced press...

Embodiment 3

[0024] Take 34.5g (0.2mol) of methyl phosphonate, under stirring, add to the mixed solution containing 14.8g of sodium cyanide, 22.4g of ammonium chloride, 136g of 15% ammonia water, and react at a temperature of 15°C for 6 hour, then slowly add 120g of 37% hydrochloric acid, heat up to 95°C, react for 4 hours, concentrate the deacidified water under reduced pressure, add 180g of ethanol, reflux esterification, the esterification temperature is 80°C, and the esterification time is 5 hours. After the end, cool down to 35°C, pass ammonia until the pH of the reaction solution is 6.5, react for 0.5 hours, then cool down to 10°C, separate and filter the insoluble ammonium chloride to obtain an ethanol solution of glufosinate-ammonium ester. Concentrate under reduced pressure to dealcoholize, add 34g of 10% ammonia water, and carry out ammoniation reaction. The reaction temperature is 5-10°C, and the reaction time is 3 hours. After the reaction, concentrate under reduced pressure, et...

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Abstract

The invention provides a method or preparing a glufosinate ammonium salt. The method comprises the following steps: 1, taking a proper amount of methylphosphonate, adding the taken methylphosphonate to a sodium cyanide, ammonium chloride and ammonia water mixed solution, and reacting at 5-45DEG C for 2-8h to generate aminonitrile phosphine ester; 2, slowly adding an acid to the aminonitrile phosphine ester, and reacting to obtain a glufosinate ammonium salt mixture; 3, adding R<1>OH to the glufosinate ammonium salt mixture, heating and refluxing the obtained solution, introducing ammonia gas after the above reaction ends, cooling after ammonia gas introduction ends, and filtering and separating out ammonium chloride to obtain an alcohol solution of glufosinate ammonium ester; and 4, carrying out reduced pressure alcohol removal on the obtained alcohol solution of glufosinate ammonium ester, adding an alkali, reacting, carrying out reduced pressure concentration after the reaction ends, carrying out alcohol precipitation, filtering the obtained solution, and drying the obtained precipitate to obtain the glufosinate ammonium salt. Cheap and easily available ammonia gas is used to substitute flammable, explosive and cancerigenic propylene oxide in traditional methods, so the method provided by the invention has the advantage of economy, safe operation and high industrialization prospect.

Description

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Claims

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Application Information

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Owner ZHEJIANG XINAN CHEM INDAL GROUP
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