氯硅烷歧化制备硅烷的工艺参数优化

摘要

本文研究了TCS两步歧化制备硅烷的工艺.通过实验选择一种高转化率国产树脂,降低了该工艺的成本投入.通过对两步歧化反应温度、反应压力和停留时间的优化,得出结论:TCS歧化反应温度在60～65℃时,转化率接近30％;DCS歧化反应温度在50～60℃时,转化率约20％,温度过高时(＞70℃)反应加快但易产生惰性不凝气体;系统压力不影响歧化的转化率,只要达到反应温度并及时移走反应产物,反应向正方向进行;固定床内氯硅烷停留时间在30～35min,反应转化率最高,停留时间少于23min,转化率将大大降低.%Two-step redistribution process to convert TCS into Silane is studied in this paper.Through this experiment,one domestically made resin with high conversion rate is selected to reduce the construction investment.After researching redistribution temperatures,pressures,and residential time,the following conclusions are drawn.TCS conversion rate reaches about 30％ at the temperature of 60-65℃C.DCS conversion rate reaches about 20％ at the temperature of 50 ～ 60℃C.When temperature is higher than 70℃C,DCS conversion rate is increased but inert and non-condensable gas is produced.System pressure does not have any significant impact on the conversion rate.Reaction is advanced to positive direction as long as the temperature is reached and the reactant is removed in time.Conversion rate reaches the highest when chlorosilane is resided in the fixed bed for 30～35 minutes.In the case of the residential time below 23 minutes,the conversation rate drops dramatically.