4,4'-双(4-氨基苯氧基)-3,3',5,5'-四甲基联苯及其聚酰亚胺的合成与性能研究

Synthesis and Property Study of 4,4'-Bis(4-aminophenoxy)-3,3',5,5'-tetramethyl Biphenyl and Polyimide Therefrom

4,4'-二羟基-3,3',5,5'-四甲基联苯(TMBP)、4-氯硝基苯(4CNB)和碳酸钾在N,N-二甲基甲酰胺(DMF)和甲苯的混合溶剂体系中回流反应,合成得到了4,4'-双(4-硝基苯氧基)-3,3',5,5'-四甲基联苯(BNTMBP);随后,在Pd/C-水合肼的还原体系中,被进一步还原,得到了4,4'-双(4-氨基苯氧基)-3,3',5,5'-四甲基联苯(BATMBP)。利用差示扫描量热计(DSC)、傅立叶转换红外光谱仪(FT-IR)等仪器,对其进行了表征。另外,将所得到的4,4'-双(4-氨基苯氧基)-3,3',5,5'-四甲基联苯(BATMBP)与均苯四甲酸二酐(PMDA)在强极性非质子有机溶剂中进行聚合反应,得到了粘稠状的聚酰胺酸(BATMBP/PMDA-PAA)溶液,涂膜、热亚胺化,获得了相应的聚酰亚胺(BATMBP/PMDA-PI)薄膜,并对其性能进行了研究。

The polyimide monomer of 4, 4＇-bis（4-aminophenoxy）-3, 3＇, 5, 5＇-tetramethylbiphenyl（BATMBP） was obtained through the reducing reaction of the 4, 4＇-bis（4-nitrophenoxy）-3, 3＇, 5, 5＇ -tetramethyl biphenyI（BNTMBP） in the system of Pd/C-hydrazine hydrate. The compound of BNTMBP was synthesized by the condensation reaction between 4-chloronitrobenzene（4CNB） and 4, 4＇-dihydroxy） -3, 3＇,5,5＇-tetramethyl biphenyl（TMBP） in the presence of potassium carbonate in the mixture solvents of N,N-dimethylformamide（DMF） and tolune（Tol）. Then, the obtained compounds were characterized by differential scanning calorimeter（DSC） and Fourier transfer infrared spectrometer（FT-IR）. Moreover, the viscous polyamic acid（BATMBP/PMDA-PAA） solution was prepared by polycondesation reaction betweenBATMBP and pyromelltic dianhydride（PMDA） in the polar aprotic organic solvent, and the corresponding polyimide （BATMBP/PMDA-PI） film was also obtained by thermal imidization of BATMBP/PMDA-PAA thin layer. The properties of the film was further studied.