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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, JIANG Zhengtao, ZHUANG Qixin. 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, JIANG Zhengtao, ZHUANG Qixin. 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(22171086,52073091, 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,研究方向为耐高温高性能材料。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

Synthesis and Performance of High Temperature Resistant Thermosetting Benzoxazole Resins

  • 摘要: 通过水介质反应法合成4种热固性苯并噁唑树脂(DAR-C、DAR-N、LAR-C和LAR-N),并对其进行了表征,研究了其溶解性;采用差示扫描量热法(DSC)研究了树脂的固化行为,用热失重分析(TGA)和宽频介电谱仪研究了树脂的耐热性和介电性能。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得较为完好,LAR-N固化后得到的热固性树脂PLAR-N在空气中的Td5达到了612 ℃,1 kHz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  水介质反应法合成苯并噁唑树脂示意图

    Figure  1.  Synthetic route of benzoxazole resin by aqueous medium reaction method

    图  2  热固性苯并噁唑树脂单体结构示意图

    Figure  2.  Schematic diagram of thermosetting benzoxazole resin monomer

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

    Figure  3.  EI-MS spectra of DAR-C(a)、DAR-N(b)、LAR-C(c) and LAR-N(d)

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

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

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

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

    图  6  TiTpTfβ的拟合直线图

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

    图  7  苯并噁唑树脂的DSC曲线

    Figure  7.  DSC Curves of benzoxazole resins

    图  8  热固性苯并噁唑树脂的TGA曲线

    Figure  8.  TGA Curves of thermosetting benzoxazole resins

    图  9  热固性苯并噁唑树脂的介电常数-频率(a)和介电损耗-频率(b)曲线

    Figure  9.  Dielectric constant-frequency and dielectric loss-frequency curves of thermosetting benzoxazole resins

    表  1  苯并噁唑树脂固化工艺

    Table  1.   Curing process of benzoxazole resin

    ResinCuring process
    DAR-C
    DAR-N
    LAR-C
    LAR-N
    R.T—Room temperature
    下载: 导出CSV

    表  2  苯并噁唑树脂的溶解性

    Table  2.   Solubility of benzoxazole resins

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

    表  3  苯并噁唑树脂单体的Ti0Tp0Tf0

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

    ResinTi0/℃Tp0/℃Tf0/℃
    DAR-C158184203
    DAR-N268273284
    LAR-C139170190
    LAR-N304310325
    下载: 导出CSV

    表  4  热固性苯并噁唑树脂的Td5

    Table  4.   Td5 of thermosetting benzoxazole resins

    ResinTd5/℃Td10/℃
    PDAR-C555600
    PDAR-N600659
    PLAR-C583632
    PLAR-N612669
    下载: 导出CSV

    表  5  常见聚合物和PLAR-N的介电常数和介电损耗

    Table  5.   Dielectric constant and dielectric loss of common polymers and PLAR-N

    Resin ε tan δ
    PE[3] 2.30 0.005
    PVC[3] 2.55 0.012
    PTEF[3] 2.60 0.024
    PBO[3] 2.70 0.010
    PLAR-N* 2.24 0.008
    * This work
    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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