BTDA型聚酰胺酸和聚酰亚胺的微波辐射合成

Microwave-radiated synthesis for BTDA type polyamic acid and polyimide

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℃。

Rapid and highly efficient synthesis of polyamic acid and polyimide was achieved under microwave irradiation by taking the co-polycondensation reactions of 3,3′ ,4,4′-benzophenonetetracarboxylic dianhydride （BTDA） with 4,4′-oxydianiline （ODA） and 3,5-diamino benzoic acid （DABA） in the presence of a small amount of a nonpolar organic medium-dimethylformamide （DMF）. Obtained polymers structure have been fully characterized by inherent viscosity, Fourier transform infrared spectroscopy （FT-IR）, proton nuclear magnetic resonance （IH NMR）. Heated properties were tested by thermal gravimetric analysis （TGA）,and solubility of polymer were determined in multi-solvent. The experimental results show that it can increase PAA′s inherent viscosity and yield via microwave-radiated solution polymerization method ,and shorten greatly the reactive time by drawing microwave. The FT-IR spectra of polymer show that there were PI＇s characteristic peaks around 1 779 cm^-1, 1 723 cm^-1, 1 239 cm^-1 and 1 378 cm^-1. Thermogravimetric（TG） curve indicates that its 10% thermal decomposition temperature under N2 is 576 ℃.