管内三甲基氯硅烷和氨气连续化制备六甲基二硅氮烷工艺研究

Research on the Continuous Preparation of Hexamethyldisilazane by Trimethylchlorosilane and Ammonia in the Tubular Reactor

设计了管内三甲基氯硅烷和氨气连续化制备六甲基二硅氮烷的反应工艺,实验结果表明,此工艺可以连续制备六甲基二硅氮烷,实验中还探究了进料流量、进料液浓度配比、气液原料比对反应程度的影响。混合液流量3.6 mL/min、液体进料TMS-MM体积比1∶3、进料氨气与液体摩尔比1.5∶1为反应的最佳条件。在此条件下,氨气利用率基本达到100%,TMS转化率达到99%以上,副产物氯化铵不会堵塞管路。

The reaction process of continuous preparation of hexamethyldisilazane by trimethylchlorosilane and ammonia was designed. The experimental results showed that this process can continuously prepare hexamethyldisilazane. Then we studied the influences of the flow rate, the concentration ratio of the liquid, and the ratio of the gas-liquid raw materials on the reaction. The optimum condition was that the flow rate of mixed solution was 3.6 mL/min, the volume ratio of the liquid feed TMS-MM was 1 ∶ 3, and the molar ratio of the feed ammonia to liquid is 1.5 ∶ 1. Under this condition, the utilization rate of ammonia was basically 100%, the conversion rate of TMS was over 99%, and the by-product ammonium chloride did not block the pipeline.