论文部分内容阅读
以o-羟基苯乙酮、对氯硝基苯和苯甲醛为原料,通过亲核取代反应、改进的Chichibabin反应以及水合肼催化还原合成了一种新型含邻位取代单元及吡啶环的芳香二胺4-苯基-2,6-双[3-(4-氨基苯氧基)苯基]吡啶(o,p-PAPP).以N,N-二甲基甲酰胺(DMF)为溶剂,将o,p-PAPP分别与3,3’,4,4’-二苯醚四羧酸二酐(ODPA)、2,2-双[4-(3,4-二羧基苯氧基)苯基]丙烷二酐(BPADA)、3,3’,4,4’-二苯酮四甲酸二酐(BTDA)及均苯四甲酸二酐(PMDA)通过常规的两步法,合成了4种聚酰亚胺.用FTIR、DSC、TGA、XRD、溶解性测试、UV-Vis和荧光光谱对聚合物的结构和性能进行了表征.FTIR结果表明,所得的聚合物在1780,1720和1380cm-1左右出现了聚酰亚胺的特征吸收峰.实验所得的PI能很好地溶解于常见有机溶剂(如DMF,DMAC,DMSO,NMP,THF,CHCl3),在氮气氛中,PI的10%失重温度(T10)为444.2～467.5℃,800℃时的残余质量(Rw)为49.6%～58.3%.同时PI分子主链中的吡啶环结构使其具有良好的紫外光吸收性能,经HCl质子化后,在460 nm附近出现非常强的荧光发射峰.
Using o-hydroxyacetophenone, p-chloronitrobenzene and benzaldehyde as raw materials, a novel bis (2-naphtho) -benzaldehyde substituted with ortho-substituted units and pyridine ring was synthesized by nucleophilic substitution reaction, modified Chichibabin reaction and hydrazine hydrate catalytic reduction Amine 4-phenyl-2,6-bis [3- (4-aminophenoxy) phenyl] pyridine (o, p-PAPP) The o, p-PAPP was mixed with 3,3 ’, 4,4’-diphenyl ether tetracarboxylic dianhydride (ODPA), 2,2-bis [4- (3,4- dicarboxyphenoxy) benzene (BPDA), 3,3 ’, 4,4’-benzophenonetetracarboxylic dianhydride (BTDA) and pyromellitic dianhydride (PMDA) were synthesized by the conventional two-step method The structures and properties of the polymers were characterized by FTIR, DSC, TGA, XRD, solubility test, UV-Vis and fluorescence spectroscopy.The FTIR results showed that the polymers obtained at 1780, 1720 and 1380 cm- 1 appeared characteristic absorption peak of polyimide.The PI obtained experimentally dissolved in common organic solvents (such as DMF, DMAC, DMSO, NMP, THF, CHCl3), in a nitrogen atmosphere, PI 10% The weight loss temperature (T10) was 444.2 ~ 467.5 ℃, and the residual mass (Rw) was 49.6% ~ 58.3% at 800 ℃ .At the same time, Ring structure it has a good ultraviolet absorption properties, HCl after protonation, it appears very strong emission peak in the vicinity of 460 nm.