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    对二乙苯液相氧化制对二乙酰苯工艺研究

    Research on Liquid Oxidation of p-Diethylbenzene to Prepare p-Diacetylbenzene

      摘要
    • 摘要: 对二乙酰苯是一种重要的化工原料,可用于生产医药、农药和染料等。今以对二乙苯为原料,30%过氧化氢为氧化剂,四水合乙酸钴为催化剂,溴化钾为助剂,研究液相氧化合成对二乙酰苯工艺及条件。实验考察了氧化剂、催化剂和助剂用量以及反应温度和反应时间对对二乙酰苯选择性的影响;采用L8(27)正交试验对对二乙苯液相氧化制备对二乙酰苯反应工艺条件进行优化。结果表明:催化剂、氧化剂和助剂用量对对二乙酰苯选择性有显著影响;适宜的反应条件为:四水合乙酸钴与对二乙苯摩尔比为0.25,对二乙苯与过氧化氢摩尔比为0.08,溴化钾与对二乙苯摩尔比为1.8,反应温度82℃,反应时间6.38 h;对二乙苯转化率接近100%,对二乙酰苯的选择性为80.81%。通过分析(GC-MS)产物组成,探讨了过氧化氢氧化对二乙苯制对二乙酰苯反应历程为:对二乙苯首先被氧化为对乙基苯乙酮,然后进一步氧化为对二乙酰苯。研究为开发对二乙苯氧化制备对二乙酰苯新工艺提供了基础。

       

      Abstract: p-Diacetylbenzene (PDAB) is an important organic material in fine chemical engineering. Liquid oxidation of p-diethylbenzene (PDEB) to prepare p-diacetylbenzene was studied using Co(Ac)2·4H2O as a catalyst, H2O2 as an oxidant and KBr as an additive. Reaction conditions were optimized by an L8(27) orthogonal design. The results show that catalyst, oxidant and additive dosages are the main factors that affect PDAB selectivity. The optimum conditions are as follows: molar ratios of Co(Ac)2·4H2O:PDEB, H2O2:PDEB and KBr:PDEB are 0.25, 0.08 and 1.8, respectively. The conversion rate is ~100% and PDAB selectivity reaches to 80.81% at 82℃ for 6.38 h. GC-MS results show that PDEB is first oxidized to p-ethylacetophenone (EAP), and then EAP is converted to PDAB. The principle and pathway of oxidation reaction from PDEB to PDAB was also discussed. This paper provides fundamental ideas in developing PDEB oxidation processes to prepare PDAB.

       

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