高等学校化学学报 ›› 2013, Vol. 34 ›› Issue (11): 2650-2654.doi: 10.7503/cjcu20130785

• 高分子化学 • 上一篇    下一篇

含磷聚酰亚胺纤维的制备与性能

丁祥1,2, 邱雪鹏1, 马晓野1, 李国民1, 高连勋1   

  1. 1. 中国科学院长春应用化学研究所, 高分子物理与化学国家重点实验室, 长春 130022;
    2. 中国科学院大学, 北京 100049
  • 收稿日期:2013-08-14 出版日期:2013-11-10 发布日期:2013-09-13
  • 作者简介:高连勋,男,博士,研究员,博士生导师,主要从事聚酰亚胺方面的研究,E-mail:lxgao@ciac.jl.cn
  • 基金资助:

    国家高技术研究发展计划(批准号:2012AA03A211)、国家重点基础研究发展计划(批准号:2014CB643604)、国家自然科学基金(批准号:51173178)和国家自然科学基金重点项目(批准号:51233001)资助.

Preparations and Properties of the Phosphorus-containing Polyimide Fibers

DING Xiang1,2, QIU Xue-Peng1, MA Xiao-Ye1, LI Guo-Min1, GAO Lian-Xun1   

  1. 1. State Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China;
    2. University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2013-08-14 Online:2013-11-10 Published:2013-09-13

摘要:

合成了一种含磷二胺单体, 二(4-胺基苯氧基)苯基膦氧(DAPOPO). 该单体与4,4'-二胺基二苯醚(ODA)、 均苯四酸二酐(PMDA)和3,3',4,4'-联苯四酸二酐(BPDA)共聚得到聚酰胺酸溶液, 通过干喷湿纺法纺丝得到聚酰胺酸纤维, 聚酰胺酸纤维经过热亚胺化和热牵伸得到含磷的聚酰亚胺纤维. 利用纤维强度仪、 扫描电子显微镜、 热失重分析仪和氧指数测定仪等研究了含磷聚酰亚胺纤维的力学性能、 形貌、 热稳定性能和阻燃性能. 结果表明, 随着含磷量的增加, 纤维的热稳定性明显提高, 而极限氧指数从35上升到了45, 说明纤维的阻燃性能得到很大提高.

关键词: 含磷聚酰亚胺纤维, 热失重分析, 阻燃性能, 极限氧指数

Abstract:

The phosphorus-containing diamine compound, bis(4-aminophenoxy)-phenyl phosphine oxide(DAPOPO) was synthesized. The solutions of polyamic acid(PAA) prepared from DAPOPO and 4,4'-oxydianiline(ODA) with pyromellitic dianhydride(PMDA) and 3,3',4,4'-biphenyl tertracarboxylic dianhydride(BPDA) were used for PAA fiber spinning with two-step process by dry-jet wet spinning. The polyimide(PI) fibers were obtained from PAA fibers by the process of the thermal imidization and hot dra-wing. The morphologies, mechanical properties, thermal properties and flame retardant properties of PI fibers were systematically investigated by the scanning electron microscopy(SEM), fiber mechanical property tester, thermogravimetric analyzer(TGA) and limiting oxygen index(LOI) value tester, respectively. The results indicate that thermal stability of the PI fibers is obviously enhanced with increasing phosphorus content. The value of LOI is increased from 35 to 45. These powerfully demonstrate that the flame retardant of PI fibers have been significantly enhanced.

Key words: Phosphorus-containing polyimide fiber, Thermogravimetric analysis, Flame retardant property, Limiting oxygen index(LOI)

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