采用三氯化铝（AlCl3）作为助反应物,通过苯基三氯硅烷（PhSiCl3）的水解和缩聚,在80℃合成了球形聚苯基硅倍半氧烷（PPSQ）。研究表明,AlCl3水溶液是球形聚苯基硅倍半氧烷（PPSQ）形成的重要因素,当n（PhSiCl3）/n（AlCl3）=6（物质的量比）,在适当浓度的四甲基氢氧化铵甲醇溶液催化下进行反应,得到的PPSQ产率高,热稳定性好。通过红外光谱（FT-IR）、拉曼光谱（Raman）、热失重分析（TGA）、X射线衍射（XRD）及29Si核磁和扫描电镜（SEM）等方法对PPSQ进行了结构分析,表明合成的PPSQ没有羟基,分子链规整度较高,热稳定性好,高温残炭率高,硅质量分数为21.86%。
Spherical polyphenylsilsesquioxane（PPSQ） was synthesized at 80 ℃ through the hydrolysis and condensation of phenyl trichlorosilane（PhSiCl3）,with aluminum chloride（AlCl3） as assistant reactant.Solution of tetramethylammonium hydroxide（N（CH3）4OH） in methanol was used as catalyst.Aqueous solution of AlCl3 is a key factor for the formation of spherical PPSQ.When PhSiCl3/ AlCl3=6（molar ratio） and the appropriate amount of N（CH3）4OH,PPSQ could be synthesized in high yield and had good thermal stability.The structure of PPSQ was finally characterized by FTIR,Raman,TGA,XRD,29Si NMR and SEM and so on.Results show that PPSQ chain is of high regularity,on the chain there is no hydroxyl group,and the silicon content in PPSQ is 21.86%.PPSQ synthesized is of high char residue at 850 ℃.
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