高温法合成甲基二氯化磷

High Temperature Synthesis of Methyldichlorophosphine

介绍了一种高温法合成甲基二氯化磷的方法,以甲烷和三氯化磷为起始原料,四氯化碳为引发剂,考查了反应温度、物料流量、反应停留时间和四氯化碳用量对反应的影响。结果表明,当反应温度为590℃,甲烷和三氯化磷的流量比为1 000∶1,停留时间为0.7 s,四氯化碳用量为6%mol时,反应条件最佳,三氯化磷转化率达到30.5%,甲基二氯化磷含量为25.6%,收率为95.0%(甲基二氯化膦收率按照转化的三氯化磷来计算)。

This paper describes a method for the synthesis of methyldichlorophosphine from a high temperature process using methane and phosphorus trichloride as starting materials and carbon tetrachloride as the initiator. The effects of reaction temperature, material flow rate, reaction residence time, and carbon tetrachloride dosage on the reaction were investigated. The results show that when the reaction temperature is 590℃, the flow ratio of methane and phosphorus trichloride is 1 000∶1, the residence time is 0.7 s, and the amount of carbon tetrachloride is 6% mol, the reaction conditions are the best. The phosphorus trichloride conversion reached 30.5%, the methyldichlorophosphine content was 25.6%, and the yield was 95.0%(the yield of methyldichlorophosphine chloride was calculated from the converted phosphorus trichloride).