微波辐射合成含三苯胺结构的超支化聚酰亚胺及其表征

Microwave-Assisted Synthesis and Characterization of Hyperbranched Polyimides containing Triphenylamine Structure

在微波辐射条件下,采用两步法以3,3′,4,4′-二苯酮四羧酸二酐(BTDA)和4,4′,4″-三氨基三苯胺(TAPA)为单体,先合成出含三苯胺结构的氨基封端和酐基封端的超支化聚酰胺酸,再经化学亚胺化和热亚胺化分别制得了相应的超支化聚酰亚胺(AM-HBPI和AD-HBPI)。FT-IR和1H-NMR验证了所得AM-HBPI和AD-HBPI的分子结构。TG测试表明此两种芳香族HBPI具有优异的热稳定性,N2中10%热失重温度(Td10%)在540℃以上。溶解性测试发现化学亚胺化得到的HBPI具有优良的溶解性能,可以溶于常见的强极性非质子溶剂。此外,它们还具有极佳的紫外-可见光吸收性能和荧光发射性能。

A series of hyperbranched polyimides （HBPIs） containing triphenylamine structure were successfully obtained by two-step process,which included synthesis of intermediates,amine-terminated and anhydride-terminated hyperbranched polyamic acids with a dianhydride monomer,3,3＇,4,4＇-benzophenonetetracarboxylic dianhydride （BTDA） and a triamine monomer,4,4＇,4＂-tris（4-aminophenyl）amine （TAPA） by controlling the monomer molar ratio and monomer addition order under microwave irradiation. It is found that the chemical structure of such HBPIs are confirmed by FT-IR spectra and 1H-NMR spectra. The TG curves indicate that the HBPIs performe admirable thermal stability with 10% mass loss above 540 ℃ in an N2 atmosphere. The solubility testing shows that the HBPIs are soluble in several polar aprotic solvents. What is more,such HBPIs were approved to have excellent UV-vis absorption property and fluorescence property from UV-vis spectra and fluorescence spectra respectively.