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以四氯邻氨基苯甲酸和蒽经Diels-Alder反应得到1,2,3,4-四氯三蝶烯,再经硝化、还原得到2,6-二氨基-13,14,15,16-四氯三蝶烯二胺单体.该二胺与双酚A二酐(BPADA)、六氟二酐(6FDA)和3,3’,4,4’-二苯甲酮四羧酸二酐(BTDA)经两步法缩聚得到系列聚酰亚胺.对2,6-二氨基-13,14,15,16-四氯三蝶烯二胺单体进行了1H-NMR,13C-NMR,FTIR表征,对所合成聚酰亚胺进行了1H-NMR、FTIR结构表征及溶解性、热性能、特性粘度、BET等测试.结果表明,含四氯三蝶烯结构的聚酰亚胺具有优异的溶解性,能溶于DMAc、DMF、NMP、THF、吡啶、间甲酚等有机溶剂,其中基于双酚A二酐和六氟二酐的聚酰亚胺在室温下能溶于氯仿中.聚合物具有良好的热性能,在0~300℃之间没有发现其玻璃化转变温度以及10%的热失重温度均高于500℃.聚合物可形成颜色较浅的透明薄膜,其中基于双酚A二酐的聚酰亚胺薄膜为无色透明.基于六氟二酐的聚酰亚胺BET比表面积为370 m2/g,是一种新型多孔聚合物.
Tetrachloro-anthranilic acid and anthracene by Diels-Alder reaction 1,2,3,4-tetrachloro-triptycene, followed by nitration and reduction to give 2,6-diamino-13,14,15,16- Tetrachlorostyrenediamine monomer, the reaction between the diamine and bisphenol A dianhydride (BPADA), hexafluoro dianhydride (6FDA) and 3,3 ’, 4,4’-benzophenonetetracarboxylic dianhydride (BTDA) to obtain a series of polyimides by two-step polycondensation.H2-NMR, 13C-NMR, FTIR, 1H-NMR, FTIR, characterization of solubility, thermal properties, intrinsic viscosity, BET, etc. The results show that the polyimide containing tetrachlorotetracycline structure has excellent Soluble in organic solvents such as DMAc, DMF, NMP, THF, pyridine and m-cresol. The polyimide based on bisphenol A dianhydride and hexafluoro dianhydride can be dissolved in chloroform at room temperature. The polymer has good thermal properties with no glass transition temperature found between 0 and 300 ° C and a 10% weight loss temperature of above 500 ° C. The polymer can form a light-colored, clear film with a bisphenol A dianhydride polyimide film is colorless and transparent based on hexafluoro dianhydride Polyimide BET specific surface area of 370 m2 / g, is a new type of porous polymer.