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
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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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