直接法合成甲基氯硅烷及其气相色谱分析

采用简单混合法和超声分散法2种催化剂触体制备方法,将自制铜粉与适量的氧化锌助催化剂混合,由直接法合成甲基氯硅烷,并建立了毛细管气相色谱法定量分析甲基氯硅烷的方法。结果表明:超声分散法比简单混合法制备的催化剂触体活性高,其合成的二甲基二氯硅烷选择性和反应中硅粉转化率均较高;以苯为内标物,采用OV-210为固定液的毛细管色谱柱和火焰离子化检测器,对合成产物进行气相色谱法定量分析,分析方法的准确度及精确度均较高。

Synthesis of methylchlorosilane by direct process and its gas chromatographic analysis

Two preparation methods of contact mass were used to mix ZnO promoters with copper powder formed by oxidation and reduction reaction from CuSO4 in order to synthesize methylchlorosilane by direct process. The contact mass prepared with ultrasonic dispersion method was proved to hold higher activity than that of prepared with simple mixing method. Both the selectivity of dimethyldichlorosilane and the silicon powder conversion in the reaction process were much higher. In addition, methylchlorosilanes were analyzed quantitatively with gas chromatogram. Methyltrichlorosilane, dimethyldichlorosilane and trimethylchlorosilane were analyzed quantitatively by OV-210 capillary column with flame ionization detector as well as benzene was adopted as the internal standard. And the analysis method was proved to be precise and accurate.