相转移催化剂上环戊烯选择氧化制备戊二酸

以双氧水为氧化剂,采用反应控制相转移催化剂催化环戊烯选择氧化制备戊二酸,考察反应条件的影响和催化剂回收。结果表明,催化剂最佳反应条件为催化剂用量为环戊烯质量的10%,双氧水和环戊烯物质的量比为4. 15∶1,反应温度90℃,反应时间5 h,最佳反应条件下戊二酸收率95. 67%,催化剂回收率66. 78%。通过高温分解反应液中残余双氧水可提高催化剂回收率。最佳分解温度为105℃,分解时间为6 h,分解反应后催化剂回收率79. 42%。实验室工艺条件下进行20 L放大试验,结果与小试无明显差别。

Preparation of glutaric acid by oxidation of cyclopentene over phase transfer catalyst

Catalyst recovery and effect of reaction conditions on selective oxidation of cyclopentene to glutaric acid over reaction-controlled phase-transfer catalyst with hydrogen peroxide as oxidant were investigated.Results showed that the optimum amount of catalyst was 10% of cyclopentene mass,molar ratio of hydrogen peroxide and cyclopentene was 4.15∶1,reaction temperature was 90 ℃ and reaction time was 5 h.Under this condition,yield of glutaric acid was 95.67%, and recovery of the catalyst was 66.78%.Catalyst recovery could be further increased by pyrolysis of residual hydrogen peroxide in the reaction solution.Under the optimum decomposition temperature of 105 ℃ and decomposition time of 6 h,catalyst recovery reached 79.42%.20 L scale-up tests which were conducted using the laboratory process conditions were not significantly different from the results of the small test.