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采用正交设计试验法对乙酸锰催化环己烷液相亚硝化一步合成己内酰胺的新反应进行了研究。考察了反应温度、反应时间、催化剂用量和反应物配比等因素对环己烷转化率和己内酰胺选择性的影响。结果表明,最佳的合成条件为:在81℃反应36 h,催化剂乙酸锰用量为环己烷质量的2.5%,亚硝基硫酸与发烟硫酸的质量比为1∶3。在此优化的条件下,环己烷液相亚硝化反应的转化率为8.12%,目标产物己内酰胺的选择性达10.54%。
Orthogonal design test was used to study the new reaction of manganese acetate catalyzed one-step nitration of cyclohexane to caprolactam synthesis. The effects of reaction temperature, reaction time, amount of catalyst and the ratio of reactants on cyclohexane conversion and caprolactam selectivity were investigated. The results showed that the optimal reaction conditions were as follows: the amount of manganese acetate catalyst was 2.5% of the mass of cyclohexane and the mass ratio of nitrosyl sulfuric acid to fuming sulfuric acid was 1: 3 after reaction at 81 ℃ for 36 h. Under the optimal conditions, the conversion of cyclohexane liquid nitrosation was 8.12% and the selectivity of caprolactam was 10.54%.