甲基二苯乙炔基硅烷及其网络聚合物的合成与表征

Synthesis and Characterization of Methyl-di(phenylethynyl)silane and Its Network Polymer

以苯乙烯为原料合成的苯乙炔和甲基二氯硅烷在有机镁试剂中反应, 合成了甲基二苯乙炔基硅烷(MDPES)单体. 通过高效液相色谱分离技术获得了纯度高于 99.9%的 MDPES, 并用 FTIR, C NMR, H NMR, MS 和元素分析进行 13 1了表征. 在较高温度下, MDPES 可以交联形成网络聚合物, 为此通过 DSC 和 FTIR 跟踪了交联反应, 证明 MDPES 的交联反应包括 Si—H 键与 C≡C 键间的加成反应和分子中的 C≡C 键间发生的 Diels-Alder 反应. 交联后的 MDPES 网络聚合物具有优异的耐热性, 在空气中的 Td5高达 568 ℃, 介电损耗 tan δ 为 2.47×10-3(1×106 Hz).

Methyl-di(phenylethynyl)silane (MDPES) was synthesized with phenylacetylene and methyl-dichlorosilane in the presence of organic magnesium reagent and purified with HPLC. The purity of separated MDPES is higher than 99.9% and was characterized by means of FTIR, C-13 NMR, H-1 NMR, MS and elemental analysis. Since MDPES can be cross-linked at high temperature to form network polymer, the cross-linking reaction process was monitored with DSC and FTIR respectively. The experimental results exhibit that both condensation reaction between Si-H and Cequivalent toC bonds and Diels-Alder reaction of two C-C bonds have taken place. MDPES network polymer shows excellent heat resistance. The value of T-d5 (temperature of 5% mass loss) is as high as 568 degreesC in air and the value of dielectric dissipation factor is 2.47 x 10(-3) (1 x 10(6) Hz).