低聚甲基氢硅氮烷的合成工艺改进

Technological Improvement on Synthesis of Methyl Hydrogen Polysilazane Oligomers

以甲基氢二氯硅烷为原料,正己烷为溶剂,通过氨解法合成低聚甲基氢硅氮烷.利用红外光谱(FT-IR)表征该低聚物的结构.通过正交试验选择最佳反应条件,考察反应温度、反应时间和反应溶剂用量对产物收率的影响.实验结果表明:反应时间、反应温度和溶剂用量均对低聚物的收率产生影响,其影响强弱顺序为溶剂用量>反应温度>反应时间.最佳反应条件为溶剂用量与甲基氢二氯硅烷的体积比6.7∶1,反应温度0℃,反应时间4 h,其产率可达88.20%.

Methyl hydrogen polysilazane oligomers were synthesized by aminolysis of methyl hydrogen dichlorosilane in the n-hexane solvent. The polysilazane were charecterized by Fourier Transform Infrared （Fr-IR） spectroscopy. The optimal reaction time, reaction temperature and amount of solvent were obtained by orthogonal experiment. The results show these factors influenced the yield of oligomers, and the order of the factors is amount of solvent 〉 reaction time 〉 reaction temperature. The optimal reactive conditions are volume ratio of solvent to methyl hydrogen dichlorosilane 6. 7： 1, reaction time 4 h and reaction temperature 0 ℃. The high yield of oligomers could reach 88.2 %.