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采用混烧法制备了WO3/γ-Al2O3催化剂,用于催化反应精馏两步合成ε-己内酯。考察了反应温度、反应时间、填料塔高、催化剂用量和原料用量对合成反应的影响。结果表明,两步反应温度分别为60℃和50℃、反应时间分别为4h和5 h、填料塔高为400 mm、m(WO3/γ-Al2O3)∶m(环己酮)=0.1、m(丙酸)∶m(环己酮)=7.3、m(30%H2O2)∶m(环己酮)=2.7时,过氧化氢的转化率和ε-己内酯的收率分别可达到95.8%和71.2%。
The WO3 / γ-Al2O3 catalyst was prepared by a mixed combustion method, which was used for two-step synthesis of ε-caprolactone by catalytic reactive distillation. The effects of reaction temperature, reaction time, packed tower height, amount of catalyst and amount of raw materials on the synthesis reaction were investigated. The results showed that the reaction temperature was 60 ℃ and 50 ℃ respectively, the reaction time was 4h and 5 h respectively, and the packing height was 400 mm. The mass ratio of WO3 / γ-Al2O3 to cyclohexanone = 0.1, m (Propionic acid): m (cyclohexanone) = 7.3, m (30% H2O2): m (cyclohexanone) = 2.7, the conversion of hydrogen peroxide and the yield of ε-caprolactone can reach 95.8 % And 71.2%.