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  • CN 31-1691/TQ

含硅芳基炔丙基醚树脂及其复合材料的制备与性能

郑嘉栋 杨唐俊 袁荞龙 黄发荣

郑嘉栋, 杨唐俊, 袁荞龙, 黄发荣. 含硅芳基炔丙基醚树脂及其复合材料的制备与性能[J]. 华东理工大学学报(自然科学版). doi: 10.14135/j.cnki.1006-3080.20210813001
引用本文: 郑嘉栋, 杨唐俊, 袁荞龙, 黄发荣. 含硅芳基炔丙基醚树脂及其复合材料的制备与性能[J]. 华东理工大学学报(自然科学版). doi: 10.14135/j.cnki.1006-3080.20210813001
ZHENG Jiadong, YANG Tangjun, YUAN Qiaolong, HUANG Farong. Preparation and Properties of Silicon-Containing Propargyl Ether of Bisphenol Resins and Their Composites[J]. Journal of East China University of Science and Technology. doi: 10.14135/j.cnki.1006-3080.20210813001
Citation: ZHENG Jiadong, YANG Tangjun, YUAN Qiaolong, HUANG Farong. Preparation and Properties of Silicon-Containing Propargyl Ether of Bisphenol Resins and Their Composites[J]. Journal of East China University of Science and Technology. doi: 10.14135/j.cnki.1006-3080.20210813001

含硅芳基炔丙基醚树脂及其复合材料的制备与性能

doi: 10.14135/j.cnki.1006-3080.20210813001
基金项目: 中央高校基本科研业务费专项资金资助(JKD01211701)
详细信息
    作者简介:

    郑嘉栋(1992—),男,浙江绍兴人,硕士生,主要研究方向为高性能材料制备与应用。E-mail:18801953856@163.com

    通讯作者:

    袁荞龙, E-mail:qlyuan@ecust.edu.cn

  • 中图分类号: T323.9

Preparation and Properties of Silicon-Containing Propargyl Ether of Bisphenol Resins and Their Composites

  • 摘要: 将双酚二炔丙基醚和氯硅烷缩聚合成了含硅双酚A二炔丙醚树脂(PSPE-A)和含硅二苯醚二炔丙醚树脂(PSPE-O)两种含硅芳炔丙醚树脂(PSPE),并用二乙炔基苯封端PSPE制备了乙炔基苯基封端的DPSPE。合成的PSPE树脂固化温度高,用乙炔基苯基封端后可明显降低树脂的固化温度和降低固化反应表观活化能,并可将PSPE树脂固化物在氮气中的5%热失重温度(Td5)和800℃残留率(Yr800℃)提升至486℃和75%,玻璃化转变温度(Tg)高于400℃。QF/PSPE-A的弯曲强度和ILSS分别为461 MPa和35 MPa,T300CF/PSPE-A的弯曲强度和ILSS分别为655 MPa和39 MPa。

     

  • 图  1  PSPE树脂的化学结构式

    Figure  1.  Chemical structure of silicon-containing propargyl ether of bisphenols

    图  2  DPSPE树脂的化学结构式

    Figure  2.  Chemical structure of DPSPE resin

    图  3  PSAE-A (a)和PSPE-O (b)树脂1H-NMR谱图

    Figure  3.  1H-NMR spectra of PSPE-A (a) and PSPE-O (b) resins

    (a) (b)

    图  4  DPSPE-A (a)DPSPE-O (b)树脂的1H-NMR谱图

    Figure  4.  1H-NMR spectra of DPSPE-A (a) and DPSPE-O (b) resins

    图  5  含硅芳炔丙醚树脂的DSC曲线

    Figure  5.  DSC curves of silicon-containing arylpropargyl ether of bisphenol resins

    图  6  PSPE-A和PSPE-O树脂在110 ℃的黏时特性

    Figure  6.  Dependence of viscosity of PSPE-A and PSPE-O upon time at 110 ℃

    图  7  含硅芳炔丙醚树脂固化物氮气中的TGA曲线

    Figure  7.  TGA curves of cured silicon-containing propargyl ether of bisphenol resins in N2

    图  8  含硅双酚A炔丙醚树脂的DMA曲线

    Figure  8.  DMA curves of cured PSPE-A and DPSPE-A resins

    表  1  含硅芳炔丙醚树脂的GPC结果

    Table  1.   GPC results of silicon-containing propargyl ether of bisphenol resin

    Sample${ {M}_{{\rm{n}}} }$${ {M}_{{\rm{w}}} }$Polydispersity
    PSPE-A168028001.46
    PSPE-O158025201.49
    DPSPE-A107015801.47
    DPSPE-O101016001.58
    下载: 导出CSV

    表  2  含硅芳炔丙醚树脂的DSC数据

    Table  2.   DSC analysis results of silicon-containing arylpropargyl ether resins

    SampleTi/℃Tp1/℃Tp2/℃H/(J·g−1)
    PSPE-A244.2291.1316.4794
    PSPE-O232.7288.11409
    DPSPE-A203.5234.1310.61038
    DPSPE-O204.9238.3312.6935
    下载: 导出CSV

    表  3  含硅芳炔丙醚的DSC数据分析和表观活化能表

    Table  3.   DSC analysis results and apparent activation energy of silicon-containing propargyl ether of bisphenol resins

    Sampleφ/(℃·min−1)Tp/Kln(φ/ T2pln/φActivation energy/(kJ·mol−1)
    KissingerOzawa
    PSPE-A5557.9−11.0391.61288.9282.2
    10564.2−10.3682.30
    15567.4−9.9742.71
    20570.5−9.6972.99
    PSPE-O5549.05−11.0071.61169.6169.9
    10561.25−10.3582.30
    15565.67−9.9682.71
    20568.8−9.6912.99
    DPSPE-A5510.8−10.8621.6198.4102.5
    10523.6−10.2192.30
    15536.3−9.8612.71
    20537.6−9.5782.99
    DPSPE-O5507.6−10.8501.61108.1110.6
    10519.3−10.2022.30
    15528.3−9.8312.71
    20534.3−9.5662.99
    下载: 导出CSV

    表  4  含硅芳炔丙醚树脂固化物氮气中TGA数据

    Table  4.   TGA analysis results of cured silicon-containing propargyl ether of bisphenol resins in N2

    SampleTd5/℃Yr800℃/%
    PSPE-A421.558.7
    PSPE-E418.066.2
    DPSPE-A486.375.1
    DPSPE-O480.273.1
    下载: 导出CSV

    表  5  含硅芳炔丙醚树脂浇铸体的力学性能

    Table  5.   Mechanical properties of cured silicon-containing propargyl ether of bisphenol resins

    SampleFlexural strength/
    MPa
    Flexural modulus/
    GPa
    Impact strength/
    (kJ·m−2)
    PSPE-A35.8 ± 1.83.4 ± 0.24.14 ± 0.2
    DPSPE-A27.8 ± 1.93.2 ± 0.13.27 ± 0.2
    下载: 导出CSV

    表  6  纤维增强PSPE树脂基复合材料力学性能

    Table  6.   Mechanical properties of the cured fiber reinforced PSPE composites

    MatrixFiberFlexural strength/MPaFlexural modulus/GPaILSS/MPa
    PSPE-AQF461.3±4.422.4±0.935.6±1.0
    T300CF655.2±9.967.8±1.739.3±2.2
    PSPE-EQF357.2±4.923.8±0.627.4±1.8
    T300CF 470.2±11.055.2±2.330.0±1.0
    下载: 导出CSV
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出版历程
  • 收稿日期:  2021-08-13
  • 网络出版日期:  2021-10-12

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