高纯脱叶磷合成与杂质组成研究

Synthesis of Higher Pure Tribufos And Research of Its Impurity

脱叶磷是一种棉花脱叶剂。以三氯化磷与正丁基硫醇经硫代烷基化反应 ,得到的化合物被双氧水氧化即可得到该产品。用气相色谱—质谱联用仪对产品组成进行分析 ,共鉴定出 8个组分 ,确定出每一杂质组分产生的原因。对反应条件进行优化 ,控制反应温度 ,分段滴加正丁基硫醇 ,在氧化前蒸出未反应的正丁基硫醇 ,使其浓度小于 0 .1%。制备的脱叶磷产品纯度可达 97%以上 ,总收率为 80 %。

Tribufos is a defoliating agent. It is obtained by the reaction of the compound, which is prepared through the Thio-alkylation of PCl_3 with n-butane thiol, and hydrogen peroxide .The components of the product are analyzed using chromatography-mass spectrometry. 8 compounds are identified and given a reasonable explain for each one. The purity of the product can reach 97% by taking effective measure, such as controlling the reactive temperature when n-butane thiol is separated to drop, removing the extra n-butane thiol until its concentration is below 0.1% before Oxidation. The overall yield is 80%.