四甲基氢环四硅氧烷（D_4~H）的合成与表征

Synthesis and characterization of tetramethylcyclotetrasiloxane

研究了以一甲基氢二氯硅烷为原料通过水解缩合的方式合成四甲基氢环四硅氧烷（D4H）的方法。在一甲基氢二氯硅烷∶介质（乙醚∶蒸馏水）反应的体积比为1∶2（1∶1）,反应温度为30℃以内,反应时间3~4h的工艺条件下首先制备得到一甲基氢硅二醇,进一步以20%氢氧化钾为催化剂,在130~140℃下减压回流4h,得到最终产物。利用FT-IR1、H-NMR对产物结构进行了表征,结果表明,该物质即为目标产物—四甲基氢环四硅氧烷（D4H）。

The methylhydrodichlorosilane as raw material,tetramethylcyclotetrasiloxane was synthesized by hydrolysis-condensation reaction.First methylhydrosilanediol was synthesized under the following conditions：V（methylhydrodichlorosilane）∶V（water∶ether）=1∶（1∶1）,the reaction temperature was controlled within 30℃,and the reaction time was 3 to 4 hours.Then the synthesis conditions of tetramethylcyclotetrasiloxane were got： the amount of catalyst was 20%,reaction temperature was 134℃ and reaction time was four hours under the method of reduced pressure distillation.The structure of tetramethylcyclotetrasiloxane was further characterized by FTIR、1H-NMR.The results indicated that the product of tetramethylcyclotetrasiloxane（D4H） was the aimed outcome.