3,3’,4,4’-二苯甲酮四甲酸二酐制备和提纯的研究进展

Research Progress of Preparation and Purification of 3,3',4,4'-Benzophenonetetracarboxylic Dianhydride

综述了3,3’,4,4’-二苯甲酮四甲酸二酐的应用及其制备和提纯的方法。第一种是硝酸法,用邻二甲苯和乙醛作原料,硫酸作催化剂在较低温度下进行缩合反应合成3,3’,4,4’-四甲基二苯乙烷,采用硝酸分2步对其进行氧化得到3,3’,4,4’-二苯甲酮四羧酸(简称酮酸);第二种是采用液相空气氧化法制备酮酸。同时还分别介绍了提纯酮酸及酮酐的方法(1)醋酐法;(2)丙酮重结晶法;(3)硅胶吸附法;(4)乙醇洗涤法;(5)乙醚洗涤法;(6)升华法。

The application,preparation and purification of 3,3＇,4,4＇-benzophenonetetracarboxylic dianhydride are described.3,3＇,4,4＇Benzophenonetetracarboxylic acid（Keto acid）could be synthesized by two ways.One way is nitrate method,1,2-Bis（3,4-dimethyl phenyl）ethane was prepared by condensation under low temperature,using o-xylene and acetaldehyde with sulfate as the catalyst.With two steps 1,2-Bis（3,4-dimethyl phenyl）ethane was oxidated by nitrate,then Keto acid was prepared.The other way is the liquid phase air oxidation method.Meanwhile,the purification methods of keto acid and keto anhydride were introduced,including（1）Acetic anhydride method;（2） Acetone recrystallization method;（3）Silica gel adsorption method;（4）Ethanol washing method;（5）Ether washing method;（6）Sublimation method.