硫化促进剂TBzTD合成工艺研究

Study on Synthesis Process of Vulcanization Accelerator TBzTD

研究以二苄胺、二硫化碳、氢氧化钠、硫酸为原料,过氧化氢为氧化剂,两步法合成促进剂TBzTD的工艺,采用正交试验法,研究过氧化氢用量、硫酸用量、氧化剂滴加速度和氧化反应温度对促进剂TBzTD收率的影响。结果表明:对促进剂TBzTD收率影响从大到小的因子顺序为氧化剂滴加速度,硫酸用量,氧化反应温度,过氧化氢用量;最佳氧化反应条件为过氧化氢/硫酸/二苄胺物质的量比0. 7/0. 7/1,氧化剂滴加速度3 mL·min^(-1),氧化反应温度50℃。在该氧化反应条件下,促进剂TBzTD收率为97. 4%,熔点为128. 6℃。

A two-step synthesis process of accelerator TBzTD was studied by using dibenzylamine,carbon disulfide,sodium hydroxide and sulfuric acid as raw materials,and hydrogen peroxide as oxidant.The effects of the amount of hydrogen peroxide and sulfuric acid,the dropping speed of oxidant and the oxidation reaction temperature on the yield of accelerator TBzTD were studied by orthogonal experiment.The results showed that the effect of factors affecting the yield of accelerator TBzTD decreased in the following order:the dropping speed of oxidant,the amount of sulfuric acid,the oxidation reaction temperature and the amount of hydrogen peroxide.The optimum oxidation reaction conditions were as follows:the mole ratio of hydrogen peroxide/sulfuric acid/dibenzylamine 0.7/0.7/1,the dropping speed of oxidant 3 mL·min-1,and the oxidation reaction temperature 50℃.Under the optimum oxidation reaction conditions,the yield of accelerator TBzTD was 97.4%,and the melting point was 128.6℃.