新型含甲基苯基硅芳醚芳炔树脂的制备与性能

牛奇 唐均坤 李传 骆佳伟 刘晓天 袁荞龙 黄发荣

牛奇, 唐均坤, 李传, 骆佳伟, 刘晓天, 袁荞龙, 黄发荣. 新型含甲基苯基硅芳醚芳炔树脂的制备与性能[J]. 航空材料学报, 2019, 39(3): 69-74. doi: 10.11868/j.issn.1005-5053.2019.000013
引用本文: 牛奇, 唐均坤, 李传, 骆佳伟, 刘晓天, 袁荞龙, 黄发荣. 新型含甲基苯基硅芳醚芳炔树脂的制备与性能[J]. 航空材料学报, 2019, 39(3): 69-74. doi: 10.11868/j.issn.1005-5053.2019.000013
Qi NIU, Junkun TANG, Chuan LI, Jiawei LUO, Xiaotian LIU, Qiaolong Yuan, Farong HUANG. Preparation and properties of new poly (methylphenyl silylene aryl ether arylacetylene) resin[J]. Journal of Aeronautical Materials, 2019, 39(3): 69-74. doi: 10.11868/j.issn.1005-5053.2019.000013
Citation: Qi NIU, Junkun TANG, Chuan LI, Jiawei LUO, Xiaotian LIU, Qiaolong Yuan, Farong HUANG. Preparation and properties of new poly (methylphenyl silylene aryl ether arylacetylene) resin[J]. Journal of Aeronautical Materials, 2019, 39(3): 69-74. doi: 10.11868/j.issn.1005-5053.2019.000013

新型含甲基苯基硅芳醚芳炔树脂的制备与性能

doi: 10.11868/j.issn.1005-5053.2019.000013
基金项目: 中央高校基本科研业务费专项资金资助(222201817001);装备预研教育部联合基金(6141A02033226)
详细信息
    通讯作者:

    黄发荣(1962—),男,博士,教授,研究方向为特种树脂及其复合材料,(E-mail)fhuanglab@ecust.edu.cn

  • 中图分类号: TQ 324.21

Preparation and properties of new poly (methylphenyl silylene aryl ether arylacetylene) resin

  • 摘要: 以1,4-二(4’-乙炔苯氧基)苯与甲基苯基二氯硅烷为原料,通过格氏反应合成具有二苯醚结构的含甲基苯基硅芳醚芳炔(PSEA-P2)树脂,进而制备其碳纤维增强复合材料。通过核磁共振(1H-NMR)、红外光谱(FT-IR)、差热分析(DSC)、热重分析(TGA)、动态热机械分析(DMA)等分析手段对树脂及其复合材料的结构与性能进行表征。结果表明:PSEA-P2树脂加工窗口为110~175 ℃,适合复合材料模压成型;树脂浇铸体具有优良的力学强度和耐热性能,在室温~450 ℃未出现玻璃化转变,弯曲强度可达54.3 MPa,氮气下热分解温度Td5达到531 ℃;T300碳纤维增强复合材料室温下弯曲强度可达518.0 MPa,400 ℃下弯曲强度保留率为53%。

     

  • 图  1  PSEA-P2树脂的合成路线

    Figure  1.  Synthesis scheme of PSEA-P2 resin

    图  2  PSEA-P2树脂的1H-NMR谱图

    Figure  2.  1H-NMR spectrum of PSEA-P2 resin

    图  3  PSEA-P2树脂的红外谱图

    Figure  3.  FT-IR spectrum of PSEA-P2 resin

    图  4  PSEA-P2树脂的黏度-温度曲线

    Figure  4.  Viscosity-temperature curve of PSEA-P2 resin

    图  5  PSEA-P2树脂的DSC谱图

    Figure  5.  DSC curve of PSEA-P2 resin

    图  6  PSEA-P2树脂的DMA谱图

    Figure  6.  DMA curve of PSEA-P2 resin

    图  7  PSEA-P2树脂的TGA谱图

    Figure  7.  TGA curve of PSEA-P2 resin

    表  1  PSEA-P2树脂的DSC分析结果

    Table  1.   DSC analysis result of PSEA-P2 resin

    Sample Ti/℃ Tp/℃ Tf/℃ ΔH/(J•g–1
    PSEA-P3 213 247 279 353
    下载: 导出CSV

    表  2  T300 CF/PSEA-P2复合材料力学性能

    Table  2.   Mechanical properties of T300 carbon cloth reinforced PSEA-P2 resin composite

    Temperature/℃ Flexural strength/MPa Flexural modulus/GPa ILSS/MPa
    RT 518.0 ± 54.8 51.4 ± 4.9 30.8 ± 2.7
    400 275.1 ± 24.9 44.9 ± 0.7 15.7 ± 1.6
    下载: 导出CSV
  • [1] AUSTIN W B, BILOW N.Diethynyl aromatic hydrocarbons which homopolymerize and char efficiently after cure: US4284834[P]. 1981-08-18.
    [2] KWAK G,MASUDU T. Synthesis and thermal properties of region-and stereoregular poly(silylene-1, 4-phenylenevinylene)s[J]. Macromol Rapid Commun,2001,22(15):1233-1236. doi: 10.1002/1521-3927(20011001)22:15<1233::AID-MARC1233>3.0.CO;2-1
    [3] HOMRIGHAUSEN C,KELLER T. High-temperature elastomers fromsilarylene-siloxane-diacetylene linear polymers[J]. Journal of Polymer Science:Part A: Polymer Chemistry,2002,40(1):88-94. doi: 10.1002/(ISSN)1099-0518
    [4] WANG F,XU J,ZHANG J,et al. Synthesis and thermal cure of diphenyl ethers terminated with acetylene and phenylacetylene[J]. Polymer International,2006,55(9):1063-1068. doi: 10.1002/(ISSN)1097-0126
    [5] MANOJ K,DAWN D,CHRISTOPHER A K,et al. Hybrid inorganic-organic poly(carborane-siloxane-arylacetylene)structural isomers with in-chain aromatics: synthesis and properties[J]. Journal of Polymer Science, Part A: Polymer Chemistry,2013,51(12):2638-2650. doi: 10.1002/pola.26653
    [6] ITOH M,MITSUZUKA M,KENJI W,et al. A novel synthesis and extremely high thermal stability of poly[(phenylsily1ene)-ethynylene-l, 3-phenyleneethynylne][J]. Macromolecules,1994,27:7917-7919. doi: 10.1021/ma00104a056
    [7] BUVAT P,JOUSSE F,DELNAU L,et al. Synthesis and properties of new processable type polyarylacetylenes[J]. International Sampe Symposium and Exhibition,2000,46:134-145.
    [8] GAO F,ZHANG L L,HUANG F R,et al. Synthesis and characterization of poly(tetramethyldisiloxane-ethynylenephenyleneethynylene)resins[J]. Journal of Polymer Research,2011,18(2):163-169. doi: 10.1007/s10965-010-9403-7
    [9] 杨建辉,周燕,汪强,等. 硅氮烷改性含硅芳炔树脂及其复合材料的性能[J]. 宇航材料工艺,2014,44(6):37-41. doi: 10.3969/j.issn.1007-2330.2014.06.009

    YANG J H,ZHOU Y,WANG Q,et al. Properties of a silicon-containing arylacetylene resin modified with silazane and its composite[J]. Aerospace Materials & Technology,2014,44(6):37-41.) doi: 10.3969/j.issn.1007-2330.2014.06.009
    [10] 闫德强,杨庆涛,周燕,等. 改性含硅芳炔树脂及复合材料的制备和性能表征[J]. 宇航材料工艺,2016,46(3):43-46. doi: 10.3969/j.issn.1007-2330.2016.03.009

    YAN D Q,YANG Q T,ZHOU Y,et al. Preparation and characterization of modificated silicon-containing arylacetylene resin[J]. Aerospace Materials & Technology,2016,46(3):43-46.) doi: 10.3969/j.issn.1007-2330.2016.03.009
    [11] 邓鹏,石松,周燕,等. 含硅芳炔树脂的化学流变特性[J]. 宇航材料工艺,2011,41(4):24-26. doi: 10.3969/j.issn.1007-2330.2011.04.006

    DENG P,SHI S,ZHOU Y,et al. Rheological character of a silicon-containing arylacetylene resin[J]. Aerospace Materials & Technology,2011,41(4):24-26.) doi: 10.3969/j.issn.1007-2330.2011.04.006
    [12] JIANG Y,LI J F,HUANG F R,et al. Polymer-derived SiC/B4C/C nanocomposites: structural evolution and crystallization behavior[J]. Journal of the American Ceramic Society,2014,97(1):310-315. doi: 10.1111/jace.12670
    [13] ZHOU Y,BU X J,HUANG F R,et al. Nanocomposites of a silicon-containing arylacetylene resin with octakis(dimethylsiloxy)octasilsesquoixane[J]. Journal of Wuhan University of Technology,2015,30(6):1310-1316. doi: 10.1007/s11595-015-1313-4
    [14] 严浩,齐会民,黄发荣,等. 新颖含硅芳基多炔树脂的合成与性能[J]. 石油化工,2004,33(9):880-886. doi: 10.3321/j.issn:1000-8144.2004.09.018

    YAN H,QI H M,HUANG F R,et al. Synthesis and characterization of poly(arylene acetylene)containing dimethylsilylene[J]. Petrochemical Technology,2004,33(9):880-886.) doi: 10.3321/j.issn:1000-8144.2004.09.018
    [15] WANG C F,HUANG F R,JIANG Y,et al. A novel oxidation resistant SiC/B4C/C nanocomposite derived from a carborane-containing conjugated polycarbosilane[J]. Journal of the American Ceramic Society,2012,95(1):71-74. doi: 10.1111/j.1551-2916.2011.04972.x
    [16] 汤乐旻,周燕,田鑫,等. 改性含硅芳炔树脂及其复合材料性能研究[J]. 玻璃钢/复合材料,2012(6):41-46. doi: 10.3969/j.issn.1003-0999.2012.06.009

    TANG L M,ZHOU Y,TIAN X,et al. Inveestion on properties of a modifies silicon-containing arylacetylene resin and its composites[J]. Fiber Reinforced Plastics/Composites,2012(6):41-46.) doi: 10.3969/j.issn.1003-0999.2012.06.009
    [17] BU X J,ZHOU Y,HUANG F R,et al. The strengthening and toughening effects of a novel octa(propargyl propyl sulfide)POSS(OPPSP)on silicon-containing arylacety-lene(PSA)resin[J]. Materials Letters,2016,174:21-23. doi: 10.1016/j.matlet.2016.03.067
    [18] HAN M N,GUO K K,WANG F,et al. Synthesis, characterization, and properties of thermosets based on the cocuring of an acetylene-terminated liquid-crystal and silicon-containing arylacetylene oligomer[J]. Journal of Applied Polymer Science,2017,134(33):1-11.
    [19] CHEN H G,XIN H,HUANG F R,et al. Synthesis and properties of poly(dimethylsilylene-ethynylene-phenoxyphenoxyphenylene-ethynylene)[J]. High Performance Polymers,2017,29:595-601. doi: 10.1177/0954008316655862
  • 加载中
图(7) / 表(2)
计量
  • 文章访问数:  2618
  • HTML全文浏览量:  1496
  • PDF下载量:  45
  • 被引次数: 0
出版历程
  • 收稿日期:  2019-01-30
  • 修回日期:  2019-02-19
  • 网络出版日期:  2019-04-11
  • 刊出日期:  2019-06-01

目录

    /

    返回文章
    返回