TiSiW_(12)O_(40)/TiO_2催化合成2-异丁基-1,3-二硫杂环己烷

Synthesis of 2-Isobutyl-1,3-dithiocyclohexane with by TiSiW_(12)O_(40)/TiO_2 Catalyst

以TiSiW_(12)O_(40)/TiO_2为催化剂,研究了1,3-丙二硫醇和异戊醛直接缩合合成2-异丁基-1,3-二硫杂环己烷的方法。通过单因素工艺条件、正交试验和催化剂的连续催化试验确定优化工艺条件为:异戊醛和1,3-丙二硫醇物质的量比为1∶1.2,反应时间2h,反应温度60℃,催化剂的用量2%(催化剂质量占反应物总质量的百分数),收率87.6%。该方法反应条件温和,收率高,对环境友好。

2-Isobutyl-1,3-dithioc with isovaleraldehyde catalyzed yclohexane was synthesised by the condensation of 1,3-dimercaptopropanol by TiSiW12040/TiO2. The optimized reaction conditions were obtained by single factor experiments, orthogonal experiments and continuous catalytic experiments. TiSiWl2 O4o/TiO2 was found to be the best catalyst. The optimized reaction conditions were as follows, n（isovaleraldehyde） ： n（1, 3-dimercaptopropanol）=1 - 1.2, the reaction time and temperature were 2 h and 60℃,and the a- mount of catalyst was 2%. The best yield was 87.6%. This new method for preparing 2-isobutyl-1,3- di- thiocyclohexane has the advantages of mild conditions, good yield and environmental friendly.