酰亚胺二羧酸的合成研究

以偏苯三酸酐(TMA)为原料,分别与4,4'-二氨基二苯醚、4,4'-二氨基二苯甲烷、1,6-己二胺反应,得到三种含酰亚胺结构的二羧酸产物(DIDA-a、DIDA-b、DIDA-c)。利用傅里叶红外光谱(FT-IR)、核磁共振氢谱(1H NMR)对酰亚胺二羧酸的结构进行表征。通过单因素实验,考察溶剂用量、反应时间、反应温度和反应物摩尔比对二酸产物收率的影响,得出DIDA-a的优化合成条件:偏酐起始浓度1.11mol/L,酰亚胺化反应时间6h,酰亚胺化反应温度140℃,TMA和二胺摩尔比2.05;DIDA-b的优化合成条件:偏酐起始浓度1.05mol/L,酰亚胺化反应时间5.5h,酰亚胺化反应温度145℃,TMA和二胺摩尔比2.02;DIDA-c的优化合成条件:偏酐起始浓度0.95mol/L,酰亚胺化反应时间5h,酰亚胺化反应温度135℃,TMA和二胺摩尔比2.03。

Research on Preparation of Diimide Dicarboxylic Acid

Three kinds of dicarboxylic acid containing imide group （ DIDA-a, DIDA-b, DIDA-c ） were prepared from trimellitic anhydride （ TMA ）, 4,4＇-diaminodiphenyether, 4,4＇-diaminodiphenylmethane and 1,6-diaminohex- ane. The structure of diimide diacids was characterized by means of FT-IR and 1H NMR. The effect of solvent amount, reaction time, reaction temperature and mole ratio of reactant on yield of diacids was observed through single factor experiment. The optimized condition for synthesis of DIDA-a is as followed： initial concentration of TMA 1. llmol/L,imidization reaction time 6h, imidization reaction temperature 140℃ ,mole ratio of TMA and diamine 2.05. The optimized condition for synthesis of DIDA-b is as followed：initial concentration of TMA 1.05mol/L, imidization reaction time 5.5h, imidization reaction temperature 145 ℃, mole ratio of TMA and diamine 2.02. The opti- mized condition for synthesis of DIDA-c is as followed：initial concentration of TMA 0. 95mol/L, imidization reaction time 5h,imidization reaction temperature 135℃ ,mole ratio of TMA and diamine 2.03.