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以3,5-二硝基苯甲酰氯和邻氨基苯酚为原料合成了含苯并噁唑基团的二胺,然后将其与二氨基二苯醚(ODA)和二苯醚四甲酸二酐(ODPA)进行常温共聚合成聚酰胺酸,最后采用两步法合成了含苯并噁唑支链的可溶性聚酰亚胺(PI)。采用红外光谱(FT-IR)、差示扫描量热法(DSC)和热重分析(TGA)等测试手段分析了该PI的结构、热性能和在各溶剂中的溶解性能。实验结果表明,经300℃热处理1h后,聚酰胺酸转化为酰亚胺化比较完全;引入苯并噁唑支链基团可以提高PI的耐热性,其玻璃化转变温度(Tg)在300℃左右,初始热分解温度为552.5℃;该PI在强极性溶剂中溶解性能良好,但不溶于一般的极性溶剂中,说明其在提高加工性能的同时仍能保持耐一般溶剂的性能。
The 3,5-dinitrobenzoyl chloride and o-aminophenol were used as raw materials to synthesize the benzoxazole group-containing diamines, which were then mixed with diaminodiphenyl ether (ODA) and diphenyl ether tetracarboxylic dianhydride (ODPA) at room temperature to synthesize polyamic acid. Finally, the soluble polyimide (PI) containing benzoxazole branches was synthesized in two steps. The structure, thermal properties and solubility of the PI in each solvent were analyzed by means of FT-IR, DSC and TGA. The experimental results show that the polyamic acid is converted into imide completely after the heat treatment at 300 ℃ for 1 h. The introduction of benzoxazole branched groups can improve the heat resistance of PI. The glass transition temperature (Tg) ℃, the initial thermal decomposition temperature is 552.5 ℃. The PI has good solubility in strong polar solvents, but it is insoluble in common polar solvents, indicating that it can improve the processing performance while still maintaining the resistance to the general solvent.