含氟及苯环侧基的聚酰亚胺材料的制备及表征  

Preparation and Characterization of Polyimide Containing Fluorine and Benzene Ring Side Group

作　　者：熊兵[1] 徐敏 朱泽昊 肖丽萍 廖旭 Bing Xiong;Min Xu;Zhehao Zhu;Liping Xiao;Xu Liao(Department of Science and Engineering,College of Science and Technology,Nanchang University,Gong qingcheng 332020,China;Coalfield Geological Research Institute of Jiangxi,Nanchang330001,China)

机构地区：[1]南昌大学科学技术学院理工学科部,江西共青城332020 [2]江西省煤田地质勘察研究院,江西南昌330001

出　　处：《高分子材料科学与工程》2022年第1期19-26,共8页Polymer Materials Science & Engineering

基　　金：江西省教育厅自然科学基金资助项目(208704)。

摘　　要：由4-甲氧基二苯甲酮通过McMurry偶联反应得到(E)-1-甲氧基-4-(2-(4-甲氧基苯基)-1,2-二苯基乙烯基)苯(1),经过脱甲基,与邻氯对硝基三氟甲基苯进行亲核取代并还原得到(E)-4-(4-(2-(4-(4-氨基-2-三氟甲基苯氧基)苯基)-1,2-二苯基)苯氧基)-3-三氟甲基苯胺(APBA);采用上述二胺单体与4,4'-氧双邻苯二甲酸酐(ODPA)进行二元共聚,与4,4'-二氨基二苯醚(ODA)、ODPA按摩尔比15:85:100,45:55:100,75:25:100进行三元共聚,得到4种聚酰亚胺(PI)树脂及薄膜。然后对所得PI的结构、耐热性能、荧光性能、溶解性、吸水率等进行表征。研究结果表明,4种聚酰胺酸的特性黏度在0.91~1.91 dL/g之间,PI树脂在N,N-二甲基甲酰胺(DMF)、N,N-二甲基乙酰胺(DMAc)、间甲酚中都有不错的溶解性,在氯仿、四氢呋喃、二甲亚砜中的溶解性随着APBA含量的增加而增加;同时吸水率不断减低,分别为1.12%,0.68%,0.62%和0.39%;5%的热失重均在300℃以上,且稳定性随APBA含量的增加而增加,完全降解温度达到了630℃;另外,四苯乙烯型化合物的引入提高了荧光寿命,使其由单体的4.96 ns延长到了13.24 ns。To obtain(E)-1-methoxy 4-(2-(4-methoxyphenyl)-1,2-diphenylvinyl)benzene by McMurry coupling reaction,after demethylation,nucleophilic substitution and reduction with o-chloro-p-nitrotrifluoromethylphenyl phenyl,(E)-4-(4-(2-(4-(4-amino 2-(trifluoromethyl)phenoxy)phenyl)-1,2-diphenylvinyl)phenoxy)-3-(trifluoromethyl)benzenamine(APBA)was synthesized;the above diamine monomer was dually copolymerized with 4,4'-oxodiphthalic anhydride(ODPA),and the ternary copolymerization with 4,4-diaminodiphenyl ether(ODA)and 4,4'-oxodiphthalic anhydride(ODPA)was carried out at the mole ratio of 15:85:100,45:55:100,75:25:100 to obtain four kinds of polyimides(PI resins and films).Then,the structure,heat resistance,fluorescence properties,solubility and water uptake of the polyimides were characterized.The results show that the intrinsic viscosity of the four polyamic acids is 0.91~1.91 dL/g,PI resins have good solubility in DMF,DMAc and m-cresol,and the solubility in chloroform,THF and DMSO increases with the increase of APBA content;meanwhile,the water uptake decreases continuously,which are 1.12%,0.68%,0.62%and 0.39%,respectively;5%of the thermal mass loss is above 300℃,and the stability increases with the increase of APBA content,and the complete degradation reaches 630℃.In addition,the fluorescence lifetime of polyimide is prolonged from 4.96 ns of monomer to 13.24 ns of PI.

关 键 词：McMurry偶联 荧光性能 耐热性能 溶解性 吸水率 

分 类 号：TQ323.7[化学工程—合成树脂塑料工业]