固体超强酸SO4^2-/ZrO2催化合成七甲基三硅氧烷的研究

以含氢硅油和六甲基二硅氧烷（MM）为原料,在SO4^2-/ZrO2固体超强酸催化下进行调聚反应,制得1,1,1,3,5,5,5-七甲基三硅氧烷（MDHM）。考察了原料配比、反应温度、反应时间及催化剂用量对MDHM收率的影响,并用红外光谱及气相色谱-质谱联用分析对产物进行了表征。结果表明,MDHM的最佳合成工艺为：反应温度70℃,反应时间7 h,MM与含氢硅油的质量比4∶1,SO4^2-/ZrO2固体超强酸用量为投料总质量的4%;在此条件下,MDHM的收率为31%-34%,固体超强酸的使用次数达到16次,产品质量较高。

Synthesis of 1,1,1,3,5,5,5-heptamethyltrisiloxane with Solid Super Acid SO4^2-/ZrO2 as Catalyst

1 ,1 ,1 ,3 ,5 ,5 ,5-heptamethyltrisiloxane was prepared with hexamethydisiloxane and methyl-hydrogen silicone fluid as the starting materials and SO4^2- /ZrO2 solid super acid as the catalyst. The influences of reactant mass ratio,reaction temperature,reaction time and catalyst dosage on the yield of 1,1,1,3,5,5,5-heptamethyltrisiloxane were investigated,the optimal conditions for synthesis were as follows：the reaction tem-perature was 70℃,the mass ratio of MM and methyl-hydrogen silicone fluid was 4∶1 ,the reaction time was 7 hours,and the mass fraction of SO4^2- /ZrO2 solid super acid was 4%. Under the optimal conditions,the yield of 1,1,1,3,5,5,5-heptamethyltrisiloxane was 31% -34%,and solid super acid can be used for 16 times, with good quality.