O,O-二乙基硫代磷酰氯的合成工艺优化

Process Improvement on Preparation of O,O-Diethyl Thiophosphoryl Chloride

对O,O-二乙基硫代磷酰氯的生产工艺进行了优化。利用第一步五硫化二磷与无水乙醇反应中产生的硫化氢副产物通入到第二步硫代磷酰酯(乙基硫化物)的氯化母液中,以硫化氢替代传统工艺中的硫化碱消除反应母液中的氯化硫,达到精制O,O-二乙基硫代磷酰氯的目的。相比传统工艺,该路线不仅缩短了工艺流程,同时废水量大幅减少为0.2t/t产品,且高收率得到了易于回收的疏松颗粒物单质硫,提高了目标化合物O,O-二乙基硫代磷酰氯的含量。

The process improvement on preparation of O,O-diethyl thiophosphoryl chloride was intrcduced.The sulfuretted hydrogen by product obtained from the reaction step one between phosphorus pentasulfide and absolute alcohol was utilized to replenish the mother solution of chlorinated O,O-diethyl dithiophosphate obtained from reaction step two.In order to purify O,O-diethyl thiophosphoryl chloride,sulfuretted hydrogen was utilized to dispel sulfur chloride instead of sodium sulfide in traditional process.Compared with the traditional process,this method can greatly simplify the process flow,sharply reduced the wasted water quantity to 0.2t/t of products,and finally obtain loosened sulfur particle and eligible O,O-diethyl thiophosphoryl chloride.