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以9,9-双(4-氨基苯基)芴(BAF)为二胺,分别与6种二酐单体——均苯四甲酸二酐(PMDA)、3,3’,4,4’-二苯醚四甲酸二酐(ODPA)、3,3’,4,4’-二苯甲酮四甲酸酐(BTDA)、3,3’,4,4’-联苯四甲酸二酐(BPDA)、4,4’-(六氟异丙烯)二酞酸酐(6FDA)和1,2,3,4-环丁烷四甲酸二酐(CBDA),经室温溶液缩聚反应得到聚酰胺酸溶液,再经化学酰亚胺化反应得到芴基聚酰亚胺(PI)。采用红外光谱、差示扫描量热分析、热重分析、溶解性测试及气体分离性能测试等手段对PI的结构和性能进行了表征。所合成的PI在N-甲基吡咯烷酮(NMP)等强极性溶剂中均具有良好的溶解性,且表现出良好的热性能,玻璃化转变温度(Tg)均在300℃以上,芳香族PI的起始热分解温度也均超过500℃,经600℃热处理的芴基PI,表现出了较好的气体渗透性能,但PI-CBDA膜的气体通量最小。
In this paper, 6 kinds of dianhydride monomers, such as pyromellitic dianhydride (PMDA), 3,3 ’, 4, 4’ - diphenyl ether tetracarboxylic dianhydride (ODPA), 3,3 ’, 4,4’-benzophenone tetracarboxylic anhydride (BTDA), 3,3’, 4,4’-biphenyl tetracarboxylic dianhydride BPDA), 4,4 ’- (hexafluoroisopropene) phthalic anhydride (6FDA) and 1,2,3,4-cyclobutanetetracarboxylic dianhydride (CBDA) were synthesized by polycondensation reaction at room temperature to obtain polyamic acid solution , Followed by chemical imidization fluorene polyimide (PI). The structure and properties of PI were characterized by infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis, solubility test and gas separation performance test. The synthesized PI has good solubility in strong polar solvents such as N-methylpyrrolidone (NMP), and shows good thermal properties, the glass transition temperature (Tg) is above 300 ℃, the aromatic PI The thermal decomposition temperature of the PI-CBDA film also exceeded 500 ℃, and the fluorene PI treated by heat treatment at 600 ℃ showed better gas permeability, but the gas flux of PI-CBDA film was the smallest.