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以对二甲苯为原料,通过溴代、偶合、硝化和还原反应成功合成了2,2’,5.5’-四甲基联苯-4,4'-二胺(TMBPDA).TMBPDA分别与4,4’-双酚A型二醚二酐(BPADA)和4,4’-双酚AF型二醚二酐(FBDA)通过高温-步法缩聚生成聚肫亚胺PLA和PI—AF。结果表明,两种聚酰亚胺不仅在N-甲基-2-吡咯烷酮(NMP),N,N-二甲基甲酰胺(DMAc)中展示出良好的有机可溶性,同时拥有优良热性能,由差示扫描量热仪(DSC)测得玻璃化转变温度(Tg)分别为251℃、和255℃。此外,两种聚酰亚胺薄膜在可见光范围内具有良好的透明性,在450nm处的透光率均超过了88%。

ABSTRACT : A biphenyl diamine, 2,2', 5,5'-tetramethylbiphenyl-4,4'-diamine (TMBPDA), was synthesized from p-xylene via bromination, Ni(0) catalytic coupling reaction, nitration and reduction. Polyimides (PI-A and PI-AF) were synthesized from TMBPDA with 4,4'- (4,4'-isopropylidenediphenoxy) bis - ( phthatic anhydride) (BPAI)A) arid 4,4'-(4,4'-hexafluoroisopropylidenediphenoxy) bis-( phthalic anhydride) (FBDA) respectively, by one step high temperature potycondensation. The polyimides show the good solubility in N-methyl-2-pyrrolidone (NMP), N, N- dimethylacetamide (DMAc). PI-A and PI-AF also exhibit excellent thermal stability, the glass-transition temperature (Tg) of PI-A and PI-AF measured by differential scanning calorimetry(DSC) is 251℃ and 255 V respectively. Moreover, the polyimides show the good transparency in the visible light region, the transparency at 450nm is higher than 88 % . Keywords : synthesis ; polyimide; transparency; diamine; thermal stability

参考文献

[1] Yang, C.-P.;Chen, Y.-C.;Hsiao, S.-H.;Guo, W.;Wang, H.-M. .Optically transparent and colorless poly(ether-imide)s derived from a phenylhydroquinone bis(ether anhydride) and various trifluoromethyl-substituted bis(ether amine)s[J].Journal of Polymer Research,2010(6):779-788.
[2] Jang W;Shin D;Choi S;Park S;Han H .Effects of internal linkage groups of fluorinated diamine on the optical and dielectric properties of polyimide thin films[J].Polymer: The International Journal for the Science and Technology of Polymers,2007(7):2130-2143.
[3] Yang CP;Chiang HC .Organosoluble and light-colored fluorinated polyimides based on 9,9-bis[4-(4-amino-2-trifluoromethylphenoxy)phenyl]fluorene and aromatic dianhydrides[J].Colloid and polymer science,2004(12):1347-1358.
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