杀虫环合成工艺研究

Study on Synthetic Process of Thiocyclam

研究了硫化钠路线生产杀虫环的合成工艺,探讨了影响产品收率的主要因素,获得了优惠的反应条件。实验证明:环化反应取氯化物与硫化钠的配比为1:1.0(mol),温度控制在0℃时反应效果最好;成盐反应选用新配制的草酸溶液于25℃时缓慢滴加到三硫杂环烷的甲苯溶液中,控制反应液pH=5时结束反应,所得产品外观松散易分离,且收率稳定。

In this paper,the synthetic process of thiocyclam by sodium sulfide was studied.The effect of the important factor on the product yield is discussed,the excellent reaction conditions could be obtained.The experiment results showed:the molar rate of chloride to sodium sulfide is1.0in cyclization reaction;the reaction result is best at0℃,the solution of oxalic acid produced newly is slowly added to the solution toluence of tri-thiacyclohexane at25℃in the salifiable reaction;the reaction is finished at pH5,the appearance of the product is loose and the product separation is easy,the product yield is stable.