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以马来酸酐为原料与水合肼反应得到哒嗪酮,再与三氯氧磷反应制备3,6-二氯哒嗪中间体,哒嗪中间体与间氨基苯酚通过亲核取代反应合成了一种新的二胺单体——3,6-二(3-氨基苯氧基)哒嗪.通过1HNMR,FTIR及HPLC-MS确证了哒嗪二胺及中间体的结构.这种哒嗪二胺单体与6种芳香二酐单体——均苯四甲酸二酐(PMDA)、3,3’,4,4’-联苯四甲酸二酐(BPDA)、4,4-六氟异丙基邻苯二甲酸酐(6FDA)、3,3’,4,4’-二苯甲酮四甲酸二酐(BTDA)、3,3’,4,4’-二苯醚四甲酸二酐(ODPA)和双酚A型二醚二酐(BPADA)通过两步法聚合制备了一系列的聚酰亚胺,并对其结构和性能进行了研究.结果表明,聚酰胺酸的比浓对数黏度为0.37~0.50 dL/g,该系列聚酰亚胺膜具有良好的热稳定性和机械性能,玻璃化温度(Tg)为188~241℃,氮气氛围下5%和10%热失重分别为421~448℃和447~473℃,拉伸强度(TS)高达102 MPa,断裂伸长率(EB)为2.0%~6.5%.紫外可见光谱测试得到的截止波长(λcut-off)为367~389 nm.
The reaction of maleic anhydride with hydrazine hydrate to obtain pyridazinone, and then with phosphorus oxychloride 3,6-dichloropyridazine intermediates, pyridazine intermediates and m-aminophenol by nucleophilic substitution reaction was synthesized The new diamine monomer, 3,6-bis (3-aminophenoxy) pyridazine, was confirmed by 1HNMR, FTIR and HPLC-MS.The structures of pyridazindi Amine monomer and six kinds of aromatic dianhydride monomers - pyromellitic dianhydride (PMDA), 3,3 ’, 4,4’-biphenyl tetracarboxylic dianhydride (BPDA), 4,4-hexafluoroiso Propyl phthalic anhydride (6FDA), 3,3 ’, 4,4’-benzophenone tetracarboxylic dianhydride (BTDA), 3,3’, 4,4’-diphenyl ether tetracarboxylic dianhydride (ODPA) and bisphenol A diether dianhydride (BPADA) were prepared by a two-step polymerization process and their structures and properties were studied.The results showed that the concentration of polyamic acid Viscosity of 0.37 ~ 0.50 dL / g, the series of polyimide film has good thermal stability and mechanical properties, glass transition temperature (Tg) of 188 ~ 241 ℃, 5% and 10% weight loss under nitrogen atmosphere, respectively The tensile strength (TS) was as high as 102 MPa and the elongation at break (EB) was 2.0% ~ 6.5% at 421 ~ 448 ℃ and 447 ~ 473 ℃. Cutoff wavelength spectrum measurement obtained (λcut-off) is 367 ~ 389 nm.