正丁基硫代磷酰三胺的绿色合成工艺

Synthesis of N-(n-butyl)Thiophosphoric Triamide

以甲苯为溶剂,硫代磷酰氯与过量的正丁胺进入管式反应器中反应,滤出正丁胺盐酸盐后,滤液进入氨化反应釜,通入氨气进行氨化反应,过滤生成的氯化铵,滤液回收大部分甲苯,再经结晶、过滤、干燥即得最终产物正丁基硫代磷酰三胺,总收率达89.8%。正丁胺盐酸盐则在无水条件下回收得正丁胺甲苯溶液,套用于反应,正丁胺回收率大于95%。该工艺操作简单、产生的三废少、生产成本低、收率高且适合工业化生产。

Using toluene as a solvent, thiophosphoryl chloride react with excess n-butylamine in tubular. The filtrate was added to ammoniated reactor after the butylamine hydrochloride filtered. Pass into the amina-tion, then remove the generation of ammonium chloride. Reclaim most of the solvent of the filtrate, through crystallization, filtration, drying to obtain the final product NBPT, the total yield was 89.8%. Butylamine hy-drochloride was recovered under anhydrous conditions. The obtained toluene solution of the n-butylamine ap-plied in the rreaction. The n-butylamine recovery was more than 95%. The process is simple, produce less waste, low production cost, high yield and is suitable for industrialized production.