3,3’,4,4’-联苯四甲酸合成中偶联工艺的研究  

Coupling Reaction Conditions of 3,3',4,4'-Biphenyltetracarboxylic Acid

作　　者：李永真[1] 陈玉红[1] 王贵珍[1] 孙娜[1] 邸青[1] 

机构地区：[1]河北化工医药职业技术学院,石家庄050026

出　　处：《绝缘材料》2011年第5期24-26,共3页Insulating Materials

基　　金：河北省教育厅项目(Z2010239)

摘　　要：以苯酐为原料经氯化、脱氯偶联两步反应合成了3,3',4,4'-联苯四甲酸,研究了中间产物4-氯邻苯二甲酸(4-CPA)脱氯偶联生成3,3',4,4'-联苯四甲酸的偶联反应工艺条件,并通过红外、液相色谱等对产物进行了表征。结果表明:Pd/C催化剂的用量及钯含量、氢氧化钠加入量、温度对产率及纯度影响较大,偶联反应最佳工艺条件为:5%Pd/C催化剂中Pa/4-CPA的配比为6.47 mg∶1 g,OH-/4-CPA的摩尔比为3.5,反应温度90℃,此时偶联收率达到66.7%,纯度高于98%。3,3＇,4,4＇-biphenyltetracarboxylic acid（s-BPTA） was prepared with phthalic anhydride as raw material through two-step reaction of chloridization and dechloridization coupling,and thecoupling reaction condition of the intermediate 4-chloro-phthalic acid（4-CPA） was studied.The product s-BPTA was analyzed by FTIR and liquid chromatography.The results show that the Pd/C catalyst and Pd content,the sodium hydroxide content and temperature have great influence on the yieldand purity of the s-BPTA.The optimum coupling reaction condition is： 5% Pd/C catalyst,Pd/4-CPA=6.47 mg∶1 g,OH-/4-CPA=3.5 and 90 ℃ of reaction temperature in which the yield reaches 66.7% and the purity is higher than 98%.

关 键 词：聚酰亚胺 3 3' 4 4'-联苯四甲酸 4-氯-邻苯二甲酸 偶联 

分 类 号：TM215.1[一般工业技术—材料科学与工程] TQ323.7[电气工程—电工理论与新技术]