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3,3′,4,4′-二苯甲酮四羧酸的工艺研究
引用本文:张春荣,于明慧.3,3′,4,4′-二苯甲酮四羧酸的工艺研究[J].化学与粘合,2008,30(3):31-34.
作者姓名:张春荣  于明慧
作者单位:黑龙江省科学院石油化学研究院 黑龙江哈尔滨150040
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。

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

Study on Synthesis Technique of 3,3',4,4'-Benzophenone Tetracarboxylic Acid
ZHANG Chun-rong,YU Ming-hui.Study on Synthesis Technique of 3,3',4,4'-Benzophenone Tetracarboxylic Acid[J].Chemistry and Adhesion,2008,30(3):31-34.
Authors:ZHANG Chun-rong  YU Ming-hui
Affiliation:ZHANG Chun - rong , YU Ming - hui ( Institute of Petrochemistry, Heilongjiang Academy of Science, Harbin 150040, China)
Abstract: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.
Keywords:1  1-bis(3  4-dimethylphenyl)ethane  liquid phase air oxidation  3  3'  4  4'-benzophenone tetracarboxylic acid  catalyst system
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