水相法合成毒死蜱的清洁工艺改进

Improvement on Clean Process for Synthesizing Chlorpyrifos by Aqueous Phase Method

研究了以3,3,5,6-四氯-3,4-二氢吡啶-2-酮和O,O-二乙基硫代磷酰氯为主要原料,采用水溶液循环的清洁工艺合成毒死蜱的新方法。通过将反应物一次性加入水介质中,在三元复合催化剂作用下形成高度分散体系进行反应,反应时间大为缩短,经简单分离提纯即可得到目标产物毒死蜱。水溶液的循环套用,优化了工艺流程,降低了成本。同时,考察了工艺条件对毒死蜱含量和收率的影响,水溶液循环套用8次后毒死蜱质量分数和收率仍能分别达到98.0%和97.0%。

A new clean method for synthesizing chlorpyrifos using aqueous solution circulation was investigated with 3,3,5,6-tetrachloro-3,4-dihydropyridine-2-one and O,O-diethylthiophosphoryl chloride as major materials.In water medium,all reactants were added once only,and the reaction happened in a highly dispersed system formed by the three-way catalysts.The reaction time was much shorter and the target product could be obtained by simple separation and purification.The circulation of the aqueous solution not only optimized the process,but also reduced the cost.Meanwhile,the technological conditions were investigated to explore their effects on the purity and yield of chlorpyrifos.After eight rounds of aqueous solution recycling,the purity and yield of chlorpyrifos still reached 98.0% and 97.0%,respectively.