先以乙炔基溴化镁、甲基氢二氯硅烷通过格式试剂法合成有机硅结构,再以三氯化硼为硼源,制备出一种硼改性的硅炔杂链树脂基体(HPBS)。通过GPC、FT-IR和NMR表征了其结构,利用DSC、FT-IR和流变研究了其固化行为,采用TGA、XRD研究了其固化物的耐热性和氧化稳定性。结果表明,HPBS聚合物热固化后,在氮气和空气中失重5%的温度(Td5)分别为621、556℃,1 000℃的质量保留率分别为85.9%和72.6%,结构中的硅硼无机元素在高温下可转化为B2O3、Si O2、B4C、Si C等耐热抗氧化物质。HBPS树脂表现出优异的耐热性和氧化稳定性。
A kind of boron-modified silicone alkyne hybrid polymer( HPBS) was prepared. The polymer was synthesized with ethynylmagnesium bromide,methyldichlorosilane and boron chloride by using Grignard reagent method. The structure of HPBS was characterized by GPC,FT-IR,1H-NMR and13C-NMR. Differential scanning calorimetry( DSC) and FT-IR were used to study the curing behaviors. The thermal and oxidation stability of the cured polymer was investigated by thermal gravimetry analysis( TGA)and XRD. The results show that HPBS can be thermally crosslinked. The temperature of 5% weight loss( Td5) of HPBS were621℃ and 556 ℃ in nitrogen and air,respectively; and the residues at 1 000 ℃ were 85. 9% and 72. 6%,respectively. The inorganic elements of silicon and boron can be converted into oxidation resistant materials such as B2O3,Si O2,B4 C and Si C at high temperatures. The HPBS resin shows excellent heat resistance and oxidation stability.