硅化镁-氯化铵法制备硅烷的工艺研究

以氯化铵、硅化镁为原料,液氨为溶剂制备硅烷。考察了原料配比、反应温度、反应时间以及氯化铵-液氨溶液中氯化铵质量分数对反应的影响。实验结果表明,实验最佳条件是氯化铵与硅化镁物质的量比7.4∶1、反应温度-30℃、反应时间2 h、氯化铵-液氨溶液中氯化铵质量分数22%。在此实验条件下,硅烷的收率大于或等于95.18%。经热重分析,反应沉淀物为六氨氯化镁。

Process study on preparation of silane from magnesium silicide and ammonium chloride

Silane is prepared from magnesium silicide and ammonium chloride with liquid ammonia as solvent. The effects of raw materials ratio,reaction temperature,reaction time and ammonium chloride mass fraction in the ammonium chloride-liquid ammonia solution are investigated. The experimental results show that the optimum reaction conditions are as follows ： the mole ratio of ammonium chloride to magnesium silicide is 7.4：1 ,the reaction temperature is - 30℃, the reaction time is 2 h, and the ammonium chloride mass fraction is 22%. Under the optimum reaction condition,the yield of silane is greater than 95.18%. By the thermal-gravimetric a- nalysis,the reaction sediment is determined as hexa-ammonia magnesium chloride.