二-(4-羟基丁基)四甲基二硅氧烷的合成研究

The Study on the Synthesis of Bis - (4 - hydroxylbutyl)tetramethyldisiloxane

采用一步法以二甲基二氯硅烷、四氢呋喃和金属镁粉为原料,在碘乙烷和单质碘催化下合成二-(4-羟基丁基)四甲基二硅氧烷。产物温合物减压过滤,以除去镁盐。滤液无需蒸馏提纯,而直接水解,干燥,减压蒸馏,收集71℃/1333Pa馏份。还探讨和优化合成条件:四氢呋喃与二甲基二氯硅烷之摩尔比应大于3.5;Grignard反应停止后应继续加热回流1小时;蒸馏时系统压力为1333Pa。

In this paper, using ethyl iodide (C2H5I) and iodine (12) as catalysts, bis - (4 - hydroxylbutyl) tetramethyldisiloxane was directly synthesized from dimethyldichlorosilane, tetrahydrofuran and powder of metal magnesium. The mixture of products was filtrated by a vacuum pump to remove the magnesium salt. Distillation of the filtration solution was not necessary in this method, but the solution could be directly hydrolyzed, then dried, distilled in vacuum and collected fraction at 71℃/1333Pa.The optimized conditions of the synthesis was discussed and concluded: 1) the molar ratios of tetrahydrofuran to dimethyldichlorosilane should be larger than 3.5; 2) the container for reaction should be continuosuly heated and refluxed for one more hour after Grignard reaction was halt: 3) the appropriate pressure of last vacuum distillation should be 1333Pa.