草铵膦的合成新工艺

New Process for Synthesis of Glufosinate

文章以羟基亚磷酸二乙酯为原料,与丙酰氯反应生成1-二乙氧基-3-(乙氧基羟基膦酰基)丙烷气,经稀碱水解得到3-(羟甲基膦酰基)丙醛,然后用Bucherer-Bergs反应将其与硝酸钾和氰化氢环合。氢氧化钙水解反应后,二氧化碳进入反应溶液中,除去钠离子,得到草铵膦铵盐。结果表明:水解反应进料量的最佳标准:羟基亚磷酸二乙酯、氢氧化钙、水的摩尔比为1:2:35,反应温度为140℃,速度10 h,草铵膦铵盐的总收率可达70%。以这种方式生产草铵膦的后处理过程很简单,这反映出转化后的副产物碳酸氢钙可以在燃烧和分解后以氢氧化钙的形式注入,转化后的二氧化碳也可以回收利用、重用。该加工技术可防止浪费和固体,并且可以完成草铵膦的绿色生产和制造。

In this paper,1-diethoxy-3-(ethoxy hydroxyphosphonyl)propane was synthesized from diethyl phosphate and propionyl chloride,and 3-(hydroxymethyl phosphonyl)propionaldehyde was obtained by dilute alkaline hydrolysis,it was then cyclized with potassium nitrate and hydrogen cyanide by the Bucherer-Bergs reaction.After the calcium dihydroxide hydrolysis,the carbon dioxide enters the reaction solution and removes the sodium ion to obtain ammonium glufosinate.The results showed that the best feed standard of hydrolysis reaction is:the molar ratio of diethyl hydroxyphosphite,calcium dihydroxide,water is 1:2:35,the reaction temperature is 140℃,the total yield of ammonium glufosinate could reach 70%in 10 hours.The reprocessing of glufosinate in this way is simple,reflecting the fact that the by product technology can prevent waste and solid,and can complete the green production and manufacture of glufosinate.