混合氧化法合成硫化促进剂CBS的新工艺研究

Process for synthesis of vulcanization accelerator CBS with mixed oxidant

对以2-巯基苯并噻唑(促进剂M)和环己胺为初始原料,经双氧水和次氯酸钠"混合"氧化合成硫化促进剂N-环己基-2-苯并噻唑次磺酰胺(简称CBS)进行了研究。采用混合氧化法,即反应前期采用双氧水氧化,后期采用次氯酸钠氧化的工艺,不仅克服了双氧水氧化法产率低的缺点,同时有效的降低了产生废水的含盐量。考察了工艺条件对产品的影响,优化得到适宜的工艺条件,使产品的平均产率达95.0%(以M计),纯度为99.0%,产品为优级品。混合氧化法产生废水含盐量较次氯酸钠法减少67%。

N-cyclohexyl-2-benzothiazolesulfenamide (rubber vulcanization accelerator CBS) is prepared from 2-mercaptobenzothiazole (vulcanization accelerator M) and cyclohexylamine with hydrogen peroxide and sodium hypochlorite as mixed oxidizing agents.This preliminary oxidation method is achieved with hydrogen peroxide,and then sodium hypochlorite as oxidant is used in the later period,not only solves low yield with hydrogen peroxide as oxidant,but also reduces the salinity in the wastewater effectively.Effects of reaction factors on the yield and quality of CBS are studied.Under the optimal conditions the average yield and the purity of CBS can be about 95.0% and 99.0%,respectively.The salinity in the wastewater with mixed oxidants can be diminished by about 67% as compared with sodium hypochlorite oxidation.