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高等学校化学研究 ›› 2019, Vol. 35 ›› Issue (6): 1076-1081.doi: 10.1007/s40242-019-9170-x

• Articles • 上一篇    下一篇

Synthesis, Thermal Degradation and Dielectric Properties of Poly[octyl(triphenylethynyl)]silane Resin

WANG Yanli, TAN Dexin   

  1. School of Chemistry and Chemical Engineering, Lingnan Normal University, Zhanjiang 524048, P. R. China
  • 收稿日期:2019-06-19 修回日期:2019-07-03 出版日期:2019-12-01 发布日期:2019-11-29
  • 通讯作者: TAN Dexin E-mail:tdxin@163.com
  • 基金资助:
    Supported by the Natural Science Foundation of Guangdong Province, China(No.2017A030307028), the Special Fund for Science and Technology Innovation Strategy of Guangdong Province, China(No.2018A01005), the Yangfan Plan of Guangdong Province, China(No.0003017011) and the Research Initiation Foundation of the Lingnan Normal University, China(Nos.ZL1604, ZL1822).

Synthesis, Thermal Degradation and Dielectric Properties of Poly[octyl(triphenylethynyl)]silane Resin

WANG Yanli, TAN Dexin   

  1. School of Chemistry and Chemical Engineering, Lingnan Normal University, Zhanjiang 524048, P. R. China
  • Received:2019-06-19 Revised:2019-07-03 Online:2019-12-01 Published:2019-11-29
  • Contact: TAN Dexin E-mail:tdxin@163.com
  • Supported by:
    Supported by the Natural Science Foundation of Guangdong Province, China(No.2017A030307028), the Special Fund for Science and Technology Innovation Strategy of Guangdong Province, China(No.2018A01005), the Yangfan Plan of Guangdong Province, China(No.0003017011) and the Research Initiation Foundation of the Lingnan Normal University, China(Nos.ZL1604, ZL1822).

摘要: Octyl(triphenylethynyl)silane monomer(OTPES) was synthesized with ethyl bromide, octyltrichlorosilane and phenylethylene by Grignard reaction. The molecular structure was confirmed by FTIR and NMR. The poly[octyl(triphenylethynyl)]silane resin(POTPES) was prepared by thermal polymerization and the corresponding thermal degradation behavior wasstudied by thermogravimetric analysis(TG) combining with model and model-free fitted methods. The dielectric property of resin was also studied by vector network analyzer. The results show that the melt point of OTPES was 50℃ and the processing window was over 236℃. The resin degradation temperature of Td5 occurred over 433℃ and the char yield was over 60% at 800℃. Based on Kissinger, Flynn-Wall-Ozawa, Coats-Redfern, Achar, Vyazovkin-Wight and Tang methods, the reaction activity(E) was 155.51, 152.97, 150.82, 146.02, 148.38 and 148.77 kJ/mol, respectively. Dielectric properties analysis displayed that the real part(ε') and the imaginary part(ε″) of the relative complex permittivity of POTPES was 2.5 and 0.05, respectively, and the dielectric loss tangent was between 0.03 and 0.25. The reflection loss of resin was more than -2.85 dB in all range of 1-5 mm thicknesses and 2-18 GHz frequency, which indicated that POTPES resin was a real wave-transparent resin matrix.

关键词: Octyl (triphenylethynyl) silane, Grignard reaction, Thermal polymerization, Thermal degradation behavior, Dielectric property

Abstract: Octyl(triphenylethynyl)silane monomer(OTPES) was synthesized with ethyl bromide, octyltrichlorosilane and phenylethylene by Grignard reaction. The molecular structure was confirmed by FTIR and NMR. The poly[octyl(triphenylethynyl)]silane resin(POTPES) was prepared by thermal polymerization and the corresponding thermal degradation behavior wasstudied by thermogravimetric analysis(TG) combining with model and model-free fitted methods. The dielectric property of resin was also studied by vector network analyzer. The results show that the melt point of OTPES was 50℃ and the processing window was over 236℃. The resin degradation temperature of Td5 occurred over 433℃ and the char yield was over 60% at 800℃. Based on Kissinger, Flynn-Wall-Ozawa, Coats-Redfern, Achar, Vyazovkin-Wight and Tang methods, the reaction activity(E) was 155.51, 152.97, 150.82, 146.02, 148.38 and 148.77 kJ/mol, respectively. Dielectric properties analysis displayed that the real part(ε') and the imaginary part(ε″) of the relative complex permittivity of POTPES was 2.5 and 0.05, respectively, and the dielectric loss tangent was between 0.03 and 0.25. The reflection loss of resin was more than -2.85 dB in all range of 1-5 mm thicknesses and 2-18 GHz frequency, which indicated that POTPES resin was a real wave-transparent resin matrix.

Key words: Octyl (triphenylethynyl) silane, Grignard reaction, Thermal polymerization, Thermal degradation behavior, Dielectric property