三苯基甲硅烷的精制工艺研究

Study on Triphenyl Silicane Purification Process

采用无水乙醇为溶剂,利用重结晶对三苯基甲硅烷粗品进行精制,确定了重结晶的最佳工艺条件:无水乙醇与三苯基甲硅烷粗品质量比为3∶1,在-10℃下快速冷却结晶,结晶时间为9 h,为使纯度达95%以上进行2次重结晶。此条件下,制得的三苯基甲硅烷晶体纯度为95.56%,回收率为91.52%。

Crude tfiphenyl siliean was purified in a solvent, and the optimum conditions of recrystallization recrystallization process with anhydrous alcohol as the were identified, i.e. that the mass ratio of anhydrous alcohol to crude tfiphenyl silican is 3 ： 1, that the crystallization time is 9 h when subjecting the solution to rapid crystallization at - 10℃, and that two times of such recrystallization are necessary to obtain the triphenyl silican product with the purity of 95% or better. The purity of the triphenyl silican crystal prepared at above conditions was 95.56%, and the percent recovery of this triphenyl silican crystal was 91.52%.