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在微波辐射条件下,将3,3′,4,4′-二苯酮四羧酸二酐(BTDA)、4,4′-二氨基二苯醚(ODA)和3,5-二氨苯甲酸(DABA)在少量非极性溶剂N,N′-二甲基甲酰胺(DMF)的存在下进行共缩聚反应,快速而高效地合成了聚酰胺酸(PAA)和聚酰亚胺(PI)。采用特性粘数、红外光谱(FT-IR)和核磁共振(1HNMR)对聚合物的结构进行了表征,利用热失重分析(TGA)对其热性能进行了测试,并测定了聚合物在多种溶剂中的溶解性。实验结果表明,微波辐射溶液聚合能够提高PAA的特性粘数及产率,微波的引入大大缩短了反应时间;FT-IR表明,在1779cm-1、1723cm-1、1239cm-1和1378cm-1处观察到聚酰亚胺特征峰;TG表明,PI在氮气中10%热失重温度(Td10%)为576℃。
Under microwave irradiation conditions, 3,3 ’, 4,4’-benzophenonetetracarboxylic dianhydride (BTDA), 4,4’-oxydianiline (ODA) and 3,5-diaminobenzene Formic acid (DABA) was copolycondensed in the presence of a small amount of N, N’-dimethyl formamide (DMF) to synthesize polyamic acid (PAA) and polyimide ). The structure of the polymer was characterized by FT-IR and 1HNMR. The thermal properties of the polymer were characterized by TGA, Solubility in solvents. The experimental results show that the microwave irradiation solution polymerization can improve the intrinsic viscosity and yield of PAA. The introduction of microwave greatly shortens the reaction time; FT-IR shows that at 1779cm-1, 1723cm-1, 1239cm-1 and 1378cm-1 The characteristic peak of the polyimide was observed. TG showed that the 10% weight loss temperature (Td10%) of PI in nitrogen was 576 ° C.