单官能团3-氯丙基笼形倍半硅氧烷(POSS)与官能化的聚苯乙烯(PS)进行缩合反应,得到POSS/PS复合材料,其热性能得到明显改善.单官能团3-氯丙基POSS由顶端封角法制备;PS经过3步处理以引入醇钠基团:Friedel-Crafts酰基化反应将羰基引入到PS的苯基上,羰基被硼氢化钠还原为羟基,金属钠与羟基反应生成醇钠基团;单官能团3-氯丙基POSS分子上的C-Cl与PS上的醇钠基团缩合从而制备POSS接枝的POSS/PS复合材料.利用~1H NMR和FTIR技术表征中间产物和POSS/PS复合材料,结果表明POSS笼上的C-Cl与官能化后PS链上的醇钠官能团之间的缩合反应效率很高.XRD测试表明POSS具有良好的分散性.TGA、DSC分析结果表明,由于POSS的引入,POSS/PS复合材料比纯PS的初始分解温度提高69℃,玻璃化转变温度提高16℃.
POSS/PS composite was synthesized through the condensation reaction of 3-chloropropylheptaisooctyl-POSS and functional PS.Sodium alkoxide group was attached to PS chain by three steps and the monofunctional-POSS molecule containing one single 3-chloropropyl group was synthesized by the corner-capping method.Thestructures of all intermediates and the POSS/PS composite were well characterized by ~1H NMR.FTIR and XRD.The results show that the condensation reaction of 3-chloropropylheptaisooctyl-POSS and functional PS is efficient,and POSS is well dispersed in the composite.The thermal properties were investigated by a differential scanningcalorimetry(DSC)and thermal gravimetric analysis(TGA).The data indicate that the glass transition temperature(T_g)and the initial decomposition temperature(T_(dec))of POSS/PS composite are 16℃ and 69℃ higher than those of the pure PS,respectively,which is mainly due to the incorporation of POSS unit.
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