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甲基苯基环硅氧烷制备工艺的研究
The Preparation Technology of Methylphenylcyclosiloxane
【摘要】 以甲基苯基二氯硅烷为原料,在无有机溶剂条件下水解,水解产物在碱催化剂存在下高温裂解,制备产率及纯度都较高的甲基苯基环硅氧烷。经过系统的实验找到了最佳的反应条件,并由气相色谱-质谱联用法(GC-MS)对产物进行了组成分析。实验结果表明,最佳的水解反应条件为甲基苯基二氯硅烷在1mol/L的HCl水溶液中水解,PhMeSiCl2与水的质量比为1:3,反应温度65~70℃,水解产率达到88.5%。裂解反应最佳的催化剂为LiOH,占反应物的质量百分比为1.5%,反应温度250~300℃,环硅氧烷产率达78.0%。
【Abstract】 Methylphenyldichlorosilane was used as the original reactant to hydrolyzed in the non-organic-solvent environment and then the hydrolyzates cracked under high temperature with alkali catalysts to produce methylphenylcyclosiloxane of high yield and purity.The products were analyzed by gas chromatography/mass spectroscope(GC-MS).After a series of experiments,the best reaction conditions were found.The results showed that the hydrolysis yield of methylphenyldichlorosilane reached 88.5%at the best reaction conditions of mass ratio of methylphenyldichlorosilane to water 1:3,reaction temperature 65-70℃and 1.0 mol/L HCl aqueous solution.The best catalyst for the cracking reaction was LiOH.The yield of cyclosiloxane was 78.0%at the conncentration of LiOH 1.5%,reaction temperature 250-300℃.
【Key words】 methylphenyldichlorosilane; cyclosiloxane; hydrolyzation; cracking; gas chromatography-mass spectroscope;
- 【文献出处】 化学反应工程与工艺 ,Chemical Reaction Engineering and Technology , 编辑部邮箱 ,2011年01期
- 【分类号】TQ264.1
- 【被引频次】11
- 【下载频次】340