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机构地区:[1]黑龙江省科学院石油化学研究院,黑龙江哈尔滨150040
出 处:《化学与粘合》2008年第3期31-34,共4页Chemistry and Adhesion
摘 要:研究了在钛材反应器中液相空气氧化3,3',4,4'-四甲基二苯乙烷制备3,3',4,4'-二苯甲酮四羧酸的反应规律。通过采用Co-Mn-Br组成的高效催化体系以及低温引发、高温完成氧化的工艺,考察反应压力、反应温度和催化剂配比条件对3,3',4,4'-二苯甲酮四羧酸收率的影响,从而确定液相空气氧化3,3',4,4'-四甲基二苯乙烷制备3,3',4,4'-二苯甲酮四羧酸的最佳反应条件为n(Co)/n(Mn)/n(Br)/n(DXE)/n(HAc)=2/2/2/50/250、反应压力2.5MPa、开始反应温度为180℃、控制最终反应温度保持在220℃,酮酸的收率大于90%。该法具有收率高,生产工艺简单,反应溶剂容易回收,三废少等优点。The synthesis of 3,3′,4,4′- benzophenone tetracarboxylic acid by liquid phase air oxidation of 1,1 - bis ( 3,4 - dimethylphenyl) ethane in titanium reactor was studied. The effects of reaction pressure, temperature, proportion of catalyst on the yield of 3,3′,4,4′- benzophenone tetracarboxylic acid was investigated by applying Co - Mn - Br high performance catalyst system and oxidation process of initiating at low temperature and finishing at high temperature, then the optimum conditions for this reaction were obtained as follow : n(Co) : n(Mn) : n(Br) : n(DXE) : n(HAc) = 2: 2: 2: 50: 250, the reaction pressure was 2.5MPa, the initiation temperature was 180℃, the final reaction temperature was 220℃, and the yield of the product was more than 90%. This method had a lot of advantages such as high yield, simple process, easy recycling of reaction solvent and less wastes.
关 键 词:3 3′ 4 4′-四甲基二苯乙烷 液相空气氧化 3 3′ 4 4′-二苯甲酮四羧酸 催化体系
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