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Method for preparing glufosinate sylvite

A technology of glufosinate-ammonium hydrochloride and glufosinate-ammonium, which is applied in the field of organic chemical synthesis, can solve the problems of unfavorable target product glufosinate-ammonium potassium salt production, numerous synthesis method steps, reduced product yield and the like, and achieves product yield The effect of high, low equipment requirements and low synthesis cost

Inactive Publication Date: 2017-01-04
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the main component of products sold on the market is glufosinate-ammonium, and there are very few products related to glufosinate-ammonium potassium salt. Similarly, there are few patents on the preparation method of glufosinate-ammonium potassium salt. It is easy to absorb water, and its solubility in water is greater than 2000g / L, which is far greater than that of ammonium glufosinate (the solubility of glufosinate in water is 1370g / L), so potassium glufosinate will quickly absorb moisture when exposed to the air become pasty, which also puts forward higher requirements for the preparation of glufosinate-ammonium. If the existing preparation method is used to prepare glufosinate-ammonium potassium salt, it must be operated in anhydrous and dry environment, and now Some synthetic methods have many steps and complicated process, so the loss must be large in the process of preparing glufosinate-ammonium potassium salt, and the yield of the final product will also decrease accordingly
In contrast, the reaction of glufosinate-ammonium potassium salt in the water phase is an ideal method, which not only has a high yield, but also is green and pollution-free. However, the difficulty lies in that glufosinate-ammonium is prone to side reactions in the water phase. It is not conducive to the production of the target product glufosinate-ammonium potassium salt, and it is necessary to optimize the design of the reaction conditions; also because of the high solubility of glufosinate-ammonium potassium salt, use conventional separation operations such as alcohol precipitation and salting-out to obtain solid glufosinate-ammonium potassium salt poorly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] First weigh 35g of 90% potassium hydroxide and 400g of water, and then dissolve potassium hydroxide in water for later use; weigh 100g of 97% glufosinate-ammonium acid and add it to a 500ml four-neck flask, and then slowly dissolve the prepared potassium hydroxide solution Pour into a four-neck flask to stir the reaction, raise the temperature to 70°C and keep it warm for 1 hour, and filter to remove the insoluble solid impurities brought in from the raw materials. The filtrate was first concentrated under reduced pressure, and 241 g of water was evaporated. At this time, the content of glufosinate-ammonium potassium salt in the concentrated solution was 40%, and the concentrated solution was dehydrated by spray drying. The time is 5s; the crude product of glufosinate-ammonium potassium salt obtained by spray drying still contains more water, put the crude product in a vacuum drying oven for further drying, set the vacuum drying temperature to 90°C, and use a vacuum pump...

Embodiment 2

[0027] First weigh 35g of 90% potassium hydroxide and 400g of water, and then dissolve potassium hydroxide in water for later use; weigh 100g of 97% glufosinate-ammonium acid and add it to a 500ml four-neck flask, and then slowly dissolve the prepared potassium hydroxide solution Pour into a four-neck flask to stir the reaction, raise the temperature to 70°C and keep it warm for 1 hour, and filter to remove the insoluble solid impurities brought in from the raw materials. The filtrate was first concentrated under reduced pressure, and 300 g of water was evaporated. At this time, the content of glufosinate-ammonium potassium salt in the concentrated solution was 50%, and the concentrated solution was dehydrated by thin film evaporation, and the crude product of glufosinate-ammonium potassium salt was obtained after thin film evaporation. It also contains a lot of water, put the crude product into a vacuum drying oven for further drying, set the vacuum drying temperature at 90°C,...

Embodiment 3

[0029] First weigh 57g of 90% potassium hydroxide and 400g of water, then dissolve potassium hydroxide in water for later use; weigh 100g of 95% glufosinate-ammonium hydrochloride and add it to a 500ml four-neck flask, and then put the prepared potassium hydroxide solution Slowly pour it into a four-neck flask to stir the reaction, raise the temperature to 70°C and keep it warm for 1 hour, and filter to remove the insoluble solid impurities brought in from the raw materials. The filtrate passes through a membrane treatment device to separate potassium chloride and glufosinate-ammonium potassium salt solution. After removing potassium chloride, the glufosinate-ammonium potassium salt solution is first concentrated under reduced pressure, and part of the water is removed to reduce the content of glufosinate-ammonium potassium salt in the concentrated solution. About 50%, the concentrated solution is dehydrated by spray drying, the spray drying temperature is set at 150°C, and the...

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PUM

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Abstract

The invention provides a preparation method of glufosinate sylvite. The preparation method comprises slowly adding aqueous solution of potassium hydroxide or potassium carbonate to glufosinate or glufosinate hydrochloride, stirring at 0oC to 90 oC for 0-12h, after the reaction solution, purifying and concentrating to get glufosinate sylvite solution containing 30-70%, drying the glufosinate sylvite solution to obtain crude glufosinate sylvite, and drying the crude product in vacuum to obtain gulufosinate sylvite solids. The method for preparing glufosinate sylvite according to the invention has the advantages of environmental friendliness, simple process and suitability for industrial production, and has important significance.

Description

technical field [0001] The invention relates to a synthesis method of glufosinate-ammonium potassium salt, belonging to the field of organic chemical synthesis. Background technique [0002] Glufosinate-ammonium, commonly referred to as glufosinate-ammonium salt (the glufosinate-ammonium salt mentioned below refers to glufosinate-ammonium salt), is a broad-spectrum contact herbicide with weak systemic effect, which is different from glyphosate for root-killing , Glufosinate-ammonium kills leaves first, and can conduct transpiration in plant xylem through plant transpiration, and its quick-acting property is between paraquat and glyphosate. Glufosinate-ammonium has the characteristics of high efficiency, low toxicity, low residue, and safety. In recent years, with the increasing resistance to glyphosate, glufosinate-ammonium has also received more and more attention. [0003] At present, the main component of products sold on the market is glufosinate-ammonium, and there are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 秦龙陈静祝小红徐晓芳白俊玲蒋辉叶珊徐亚卿
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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