1,4-双(2,4-二氨基苯氧基)苯的合成及其支化型聚酰亚胺薄膜

Synthesis of 1,4-Bis(2,4-diaminophenoxy) benzene and Branched Polyimide Film Therefrom

利用对苯二酚(HQ)、2,4-二硝基氯苯(24DNCB)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1,4-双(2,4-二硝基苯氧基)苯(14BDNPOB);随后,在Pd/C-水合肼的还原体系中进一步还原,得到了1,4-双(2,4-二氨基苯氧基)苯(14BDAPOB)。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1,4-双(2,4-二氨基苯氧基)苯(14BDAPOB)、4,4'-二氨基二苯醚(44ODA)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,得到了粘稠状的支化型聚酰胺酸(PMDA/44ODA/14BDAPOB-PAA)溶液,涂膜、热亚胺化,得到了相应的支化型聚酰亚胺(PMDA/44ODA/14BDAPOB-PI)薄膜,并对其性能进行了研究。

The polyimide monomer of 1,4-bis（2,4-diaminophenoxy）benzene（14BDAPOB） was obtained through the reducing reaction of the 1,4-bis（2,4-dinitrophenoxy）benzene（14BDNPOB） in the system of Pd/C-hydrazine hydrate.The compound of 14BDNPOB was synthesized by the condensation reaction between 2,4-dinitrochlorobenzene（24DNCB） and hydroquinone（HQ） 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 branched polyamic acid（PMDA/44ODA/14BDAPOB-PAA） solution was prepared by the reaction betweenpyromelltic dianhydride（PMDA） and amino-compounds including 4,4＇-diaminodiphenyl ether（44ODA） and 1,4-bis（2,4-diaminophenoxy）benzene（14BDAPOB） in the polar aprotic organic solvent,and the corresponding branched polyimide（PMDA/44ODA/14BDAPOB-PI） film was also manufactured by thermal imidization of PMDA/44ODA/14BDAPOB-PAA thin layer.The properties of the branched polyimide film was further studied.