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  • ISSN 1006-3080
  • CN 31-1691/TQ

新型耐高温热固性苯并噁唑树脂的合成与性能研究

汪文涛 刘小云 姜正涛 庄启昕

汪文涛, 刘小云, 姜正涛, 庄启昕. 新型耐高温热固性苯并噁唑树脂的合成与性能研究[J]. 华东理工大学学报(自然科学版). doi: 10.14135/j.cnki.1006-3080.20210405001
引用本文: 汪文涛, 刘小云, 姜正涛, 庄启昕. 新型耐高温热固性苯并噁唑树脂的合成与性能研究[J]. 华东理工大学学报(自然科学版). doi: 10.14135/j.cnki.1006-3080.20210405001
WANG Wentao, LIU Xiaoyun, JANG Zhengtao, ZHUANG Qixin. Study on the Synthesis and Performance of High Temperature Resistant Thermosetting Benzoxazole Resins[J]. Journal of East China University of Science and Technology. doi: 10.14135/j.cnki.1006-3080.20210405001
Citation: WANG Wentao, LIU Xiaoyun, JANG Zhengtao, ZHUANG Qixin. Study on the Synthesis and Performance of High Temperature Resistant Thermosetting Benzoxazole Resins[J]. Journal of East China University of Science and Technology. doi: 10.14135/j.cnki.1006-3080.20210405001

新型耐高温热固性苯并噁唑树脂的合成与性能研究

doi: 10.14135/j.cnki.1006-3080.20210405001
基金项目: 国家自然科学基金(52073091, 51773060);上海市自然科学基金(20ZR1414600);上海市先进聚合物材料实验室开放基金
详细信息
    作者简介:

    汪文涛(1994-),男,湖北人,硕士生,研究方向:耐高温高性能材料。E-mail:786922483@qq.com

    通讯作者:

    庄启昕,E-mail:qxzhuang@ecust.edu.cn

    刘小云,E-mail:liuxiaoyun@ecust.edu.cn

  • 中图分类号: O63

Study on the Synthesis and Performance of High Temperature Resistant Thermosetting Benzoxazole Resins

  • 摘要: 通过水介质反应法合成四种热固性苯并噁唑树脂(DAR-C、DAR-N、DAR-lN和LAR-N),对其进行了表征。研究了它们的溶解性,以及利用DSC研究了树脂的固化行为,用TGA分析和宽频介电谱仪研究了树脂耐热性和介电性能。结果表明:热固性苯并噁唑的加工性能较长链聚苯并噁唑更佳,且聚苯并噁唑的耐热性和介电性能也保持的较为完好,PLAR-N在空气中的Td5达到了612 ℃,1k Hz下介电常数为2.24,介电损耗低至0.008,表明新型苯并噁唑树脂在耐高热低介电材料领域有很好的应用前景。

     

  • 图  1  水介质法合成苯并噁唑示意图

    Figure  1.  Synthetic route of benzoxazole resin by aqueous media

    图  2  热固性苯并噁唑单体结构示意图

    Figure  2.  Schematic diagram of thermosetting benzoxazole resin

    图  3  DAR-C(a)、DAR-N(b)、DAR-lN(c)和LAR-N(d)的EI-MS图谱

    Figure  3.  DAR-C(a)、DAR-N(b)、DAR-lN (c) and LAR-N(d)electron bombardment-time-of-flight MS

    图  4  DAR-C(a)、DAR-N(b)、LAR-C(c)和LAR-N(d)单体红外光谱图

    Figure  4.  FT-IR of DAR-C(a), DAR-N(b), LAR-C(c) and LAR-N(d) monomers

    图  5  DAR-C(a)、DAR-N(b)、LAR-C(c)和LAR-N(d)不同升温速率下的DSC曲线图

    Figure  5.  DSC curves of DAR-C(a), DAR-N(b), LAR-C(c) and LAR-N(d) at different heating rates Figure

    图  7  聚苯并噁唑树脂的DSC曲线图

    Figure  7.  DSC curve of polybenzoxazole resin

    图  6  TiTpTf对β的拟合直线图

    Figure  6.  Fitting straight line graph of Ti, Tp and Tf to β

    图  8  聚苯并噁唑树脂的TGA曲线图

    Figure  8.  TGA curve of polybenzoxazole resin

    图  9  聚苯并噁唑树脂的介电常数和介电损耗-频率曲线图

    Figure  9.  Dielectric constant-frequency and Dielectric loss curve of polybenzoxazole resin

    表  1  苯并噁唑树脂固化工艺

    Table  1.   Curing process of benzoxazole resin

    ResinsCuring process
    DAR-C
    DAR-N
    LAR-C
    LAR-N
    下载: 导出CSV

    表  2  苯并噁唑树脂单体的溶解性

    Table  2.   Solubility of benzoxazole structure

    SolventAcetoneMethylbenzeneTHFEtOHDMSODMF
    DAR-C---------+
    DAR-N--------+-+
    LAR-C--++-++++
    LAR-N-+-+-+-+++
    PBO------------
    Note:-- Insoluble;- Slightly soluble;-+ Heat soluble;+ R.T soluble;++ Easily soluble at R.T
    下载: 导出CSV

    表  3  热固性苯并噁唑树脂单体的Ti0Tp0Tf0

    Table  3.   Ti0, Tp0, Tf0 of benzoxazole resin monomer

    ResinsNO.Ti0/℃Tp0/℃Tf0/℃
    DAR-Ca160190210
    DAR-Nc268273291
    LAR-Cd142174193
    LAR-Ne299314332
    下载: 导出CSV

    表  4  聚苯并噁唑树脂的Td5

    Table  4.   Td5 of polybenzoxazole resin

    ResinsTd5/℃Td10/℃
    PDAR-C555600
    PDAR-N600659
    PLAR-C583632
    PLAR-N612669
    下载: 导出CSV

    表  5  常见聚合物的介电常数和介电损耗

    Table  5.   The dielectric constant of common polymers

    ResinPEPVCPTEFPBOPLAR-N
    ε2.302.552.602.702.24
    tanδ0.0050.0120.0240.010.008
    下载: 导出CSV
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出版历程
  • 收稿日期:  2021-04-05
  • 网络出版日期:  2021-07-09

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