基于大体积芴侧基热固性聚酰亚胺的合成及性能研究  

Preparation and properties of thermoset polyimide with bulky side groups of fluorene

作　　者：贾子辰 马臣俣 汪毅 汪贵梅 彭万 黄琦睿 潘丽静 韩敏 胡一鸣 宇平 JIA Zichen;MA Chenyu;WANG Yi;WANG Guimei;PENG Wan;HUANG Qirui;PAN Lijing;HAN Min;HU Yiming;YU Ping(School of Environmental and Chemical Engineering,Jiangsu Ocean University,Lianyungang 222005,China;Changzhou JME Advanced Materials Co,Ltd,Changzhou 213000,China;State Key Laboratory for Modification of Chemical Fibers and Polymer Materials,Donghua University,Shanghai 201620,China)

机构地区：[1]江苏海洋大学环境与化学工程学院,江苏连云港222005 [2]常州杰铭新材料科技有限公司,江苏常州213200 [3]东华大学,纤维材料改性国家重点实验室,上海201620

出　　处：《中国塑料》2023年第7期22-26,共5页China Plastics

基　　金：江苏省先进功能材料调控技术重点实验室开放基金(jsklfctam202109);江苏省高校大学生创新创业训练计划项目(202211641178T、202311641637004);产学研合作项目(HKK2022038)。

摘　　要：在二元酐2,3,3’,4’-二苯醚四甲酸二酐(a-ODPA)基础上,利用二元胺9,9-双(4-氨基苯基)芴(BAFL)共聚合成耐高温的苯乙炔苯酐封端的聚酰亚胺树脂,采用傅里叶变换红外光谱、差示扫描量热、热失重分析等方法,研究了其化学结构与溶解度、固化特性、耐热性能的关系及其影响机理。结果表明,该预聚体在有机溶剂中具有较高溶解度;玻璃化转变温度随着芴基引入而增加,提高了41℃,达到356℃;固化后的树脂具有高的热稳定性,氮气下,5%热失重温度大于520℃,800℃的残炭率高达62%,本研究进一步提升了热固性聚酰亚胺树脂的耐温等级,有望在海工装备、国防军工等领域得到较好应用。In this paper,a type of high-temperature-resistant polyimide(PI) resins terminated with phenylethynyl groups was prepared by using 2,3,3',4'-diphenyl ether tetracarboxylic acid dianhydride and 9,9-bis(4-aminophenyl) fluorene as raw materials.The relationships between the chemical structure of the as-prepared products and their solubility,curing properties,and heat resistance were investigated by using Fourier-transform infrared spectroscopy,differential scanning calorimetry,and thermogravimetric analysis,and the relevant influencing mechanisms were studied.The results indicated that the oligomers had high solubility in organic solvents.The as-prepared PI resin samples exhibited a maximum glass transition temperature of 356 ℃,which increased by 41 oC with increasing the fluorenyl content.The cured PI resins presented a high thermal stability with a 5 wt% thermogravimetric temperature of above 520 ℃ in nitrogen,and their residual char yields were as high as 60 wt% at 800 ℃.The thermoset PI resins gained an improvement in temperature resistance and were expected to be applied in marine engineering equipments,national defense,military industry,and other fields.

关 键 词：热固性聚酰亚胺 苯乙炔苯酐 芴基 耐热性能 

分 类 号：TQ323.7[化学工程—合成树脂塑料工业]