可溶性聚酰亚胺的合成和性能研究

Copolymerization of Soluble Fluorinated Polyimides

采用低温两步法对1,4-双(1,4-二氨基)苯氧基苯(TPEQ)和4,4′-二氨基二苯醚(ODA)(含醚二胺)与4,4′-六氟亚异丙基-邻苯二甲酸酐(6FDA)(含氟二酐)分别进行了二元共聚和三元共聚,而且对共聚物分别进行了高温环化和化学环化,考察了其物性并采用FT-IR、1H-NMR、DSC、TGA对其进行了表征。结果表明,所有产品都具有良好地溶解性、耐热性和加工性能;不仅溶于DMF,还能很好的溶于低沸点溶剂三氯甲烷、四氢呋喃;Tg在220.9℃以上,Td在429℃以上,5%热损失的温度多在462℃以上,Tm在550℃以上。其中经高温环化的的三元共聚物(n(TPEQ)∶n(ODA)=3∶1)具有最好的综合性能:粘度1.065,Tg241.7℃,Td506℃,T5%488℃,拉伸强度108.81 MPa,可适用于激光约束聚变(ICF)实验用靶的自支撑膜材料。

In this study,a group-containing polyimides based on two kinds of diamine of TPEQ and ODA with 6FDA were polymerized and copolymerized.And these polyimides were synthesized by a two-step method,reactive dehydration at low temperature and high temperature dehydration.The experimental results were compared for viscosity,solubility,T-IR1,H-NMR,DSC,and TGA.The results show that all of the resulting polyimides are heat-resistant and have a preferable solubility.They were soluble in common solvents such as DMF,and in lower boiling point solvents,such as chloroform and THF.The polyimides also exhibited a good thermo-stability with glass transition temperatures of above 220.9℃,decomposing temperatures of above 429℃,5% weight-loss temperatures of above 462℃,and melting points of above 550 ℃.The seventh sample（n（TPEQ）∶n（ODA）=3∶1）by high temperature dehydration） has the best general capabilities of all samples.Its viscosity is 1.065,glass transition temperature 241.7 ℃,decomposing temperature 506 ℃,temperature of 5% weight-loss 488℃,melting point of 557.9 ℃,and tensile strength 108.81 MPa.These polyimides are better sustainable films used as the self-supporting laser targets in initial controlled fusion（ICF） experiments.