高等学校化学学报 ›› 2012, Vol. 33 ›› Issue (09): 2117.doi: 10.3969/j.issn.0251-0790.2012.09.042

• 高分子化学 • 上一篇    下一篇

耐高温交联侧基苯乙炔封端酰亚胺预聚体

杨明1, 白哲革2, 周宏伟2, 陈春海2, 党国栋2   

  1. 1. 中国航空工业集团北京航空材料研究院, 北京 100095;
    2. 吉林大学化学学院, 麦克德尔米德实验室, 长春 130012
  • 收稿日期:2011-10-18 出版日期:2012-09-10 发布日期:2012-08-14
  • 通讯作者: 党国栋,男,博士,副教授,主要从事聚酰亚胺和聚芳醚酮研究.E-mail:dgd_tong@jlu.edu.cn E-mail:dgd_tong@jlu.edu.cn
  • 基金资助:

    国家"九七三"计划项目(批准号: 2010CB631100)和国家科技支撑计划项目(批准号: 2011BAA06B03)资助.

Phenylethynyl-terminated Imide Oligomer of Having Pendent Phenylethynyl Group with Good Thermal Stability

YANG Ming1, PAEK Cholhyok2, ZHOU Hong-Wei2, CHEN Chun-Hai2, DANG Guo-Dong2   

  1. 1. Beijing Institute of Aeronautical Materials, Aviation Industy Corporation of China, Beijing 100095;
    2. Alan G. MacDiarmid Institiute, College of Chemistry, Jilin University, Changchun 130012, China
  • Received:2011-10-18 Online:2012-09-10 Published:2012-08-14
  • Contact: Guodong Dang E-mail:dgd_tong@jlu.edu.cn

摘要:

合成了含有苯乙炔基的二胺单体 3,5-二氨基-4'-苯乙炔苯甲酮(DPEB), 并与3,3',4,4'-联苯四酸二酐(s-BPDA)和1,4-双(4'-氨基苯氧基)-2-(苯基)苯(p-TPEQ)进行了缩聚反应, 以4-苯乙炔苯酐作为封端剂, 合成了交联侧基苯乙炔封端酰亚胺预聚体(n=4). DSC测试结果表明, 引入交联侧基后预聚体依然保持着较宽的加工窗口. 利用所合成的预聚体在370℃热压1 h制备了热固性薄膜. DMA测试结果表明, 引入交联侧基的预聚体树脂具有更高的玻璃化转变温度, 并且其储存模量在玻璃化转变后有很好的保持.

关键词: 聚酰亚胺, 预聚体, 苯乙炔, 交联侧基, 3,5-二氨基-4'-苯乙炔苯甲酮

Abstract:

A diamine monomer 3,5-diamino-4'-phenylethynylbenzophenone (DPEB) was synthesized and phenylethynyl-terminated imide oligomers having pendent phenylethynyl group (n=4) was prepared by the reaction of 3,3',4,4'-biphenylenetetracarboxylic dianhydride (s-BPDA), DPEB and 2,5-bis(4-aminophenoxy)-biphenyl(p-TPEQ), and end-capped with 4-phenylethynylphthalic anhydride (PEPA). The imide oligomer had low Tg and provided wide processing window. The cured films were prepared by molding the oligomer powder at 370℃ for 1 h under pressure. DMA results show the introduction of pendent phenylethynyl group increases Tg of the cured film and the retention of storage modulus beyond Tg is promoted.

Key words: Polyimide, Oligomer, Cross-linked pendent group, Phenylethyne, 3,5-Diamino-4'-phenyl ethynylbenzophenone (DPEB)

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