异丙醇溶剂中O-异丙基-S-十二烷基二硫代甲酸酯的合成工艺

Synthesis Process of S-Dodecyl O-Isopropyl Dithiocarbonate in the Isopropyl Alcohol

首先采用粉碱、二硫化碳在过量的异丙醇溶剂体系中合成了异丙基黄原酸盐,所得产物不经分离直接加入溴代十二烷合成O-异丙基-S-十二烷基二硫代甲酸酯(DIDTC)。实验考察了异丙醇用量、物料比例、反应时间和温度对产物收率的影响,并且研究了反应过程中溶剂异丙醇的回收循环利用。结果表明,在黄药与溴代十二烷物质的量比为1.05:1,反应温度45℃,溶剂用量为每摩尔溴代十二烷40mL异丙醇,反应时间为4h的较佳条件下,产物DIDTC基于溴代十二烷的收率可达94%。采用异丙醇为溶剂有效解决了溴代十二烷与黄药在水相中的反应效率低问题,而且异丙醇可循环利用,减小了环境污染。

S-dodecyl O-isopropyl dithiocarbonate （DIDTC） was synthesized by bromododecane and isopropyl xanthantes, which were firstly synthesized by using sodium hydroxide, carbon disulfide in the excessive isopropyl alcohol solvent. The effects of isopropyl alcohol dosage, molar ratio of materials, reaction time and reaction temperature on the yield of DIDTC were investigated experimentally. And the recycling of isopropyl alcohol was also investigated. The results showed that the yield of DIDTC based on the bromododecane could reach 94% under the conditions of 1.05 molar ratio of xanthante to bromododecane, the reaction temperature of 45℃, 40 mL isopropyl alcohol solvent for 1 mol bromododecane and the reaction time of 4 h. The problem of low conversion for the reaction of bromododecane and isopropyl xanthantes in water was solved by use of isopropyl alcohol as reaction solvent. There was little environmental pollution by the recycling use of isopropyl alcohol in the process.