六甲基二硅烷胺钠的合成工艺改进  

Improvement in synthesis of sodium hexamethyldisilazide

作　　者：周广山 刘金彪[1] 卢博为[2,3] 谢志强 卢俊瑞 ZHOU Guangshan;LIU Jinbiao;LU Bowei;XIE Zhiqiang;LU Junrui(School of Chemistry and Chemical Engineering,Tianjin University of Technology,Tianjin 300384,China;School of Chemical Engineering and Technology,Tianjin University,Tianjin 300072,China;Tianjin Ruiling Chemical Engineering Co.,Ltd.,Tianjin 300384,China;College of Chemistry,Nankai University,Tianjin 300071,China)

机构地区：[1]天津理工大学化学化工学院,天津300384 [2]天津大学化工学院,天津300072 [3]天津瑞岭化工有限公司,天津300384 [4]南开大学化学学院,天津300071

出　　处：《天津理工大学学报》2024年第5期127-131,共5页Journal of Tianjin University of Technology

基　　金：国家自然科学基金(21476174)。

摘　　要：在已报道的方法上,使用六甲基二硅烷胺和氢化钠在无溶剂条件下合成了六甲基二硅烷胺钠,改进了反应的温度、时间、物料配比,最佳收率能够达到99.2%。目标化合物的结构经核磁氢谱(H nuclear magnetic resonance spectrum,1H NMR)、红外光谱(infra-red spectrum,IR)和高分辨质谱(high resolution mass spectrometer,HRMS)确证。后续阶段新加入洗涤步骤,减少后处理时间,提高了产品摩尔浓度。改进后的工艺操作简便,成本较低,最终产品为清澈透明的淡黄色溶液,且产品摩尔浓度与性状符合市场产品质量的标准。Based on the method reported in the literature,sodium hexamethyldisilazide was synthesized from hexamethyldisilane amine and sodium hydride under solvent-free conditions,the reaction temperature,time and material ratio were improved by using hexamethyldisilane amine and sodium hydride as the reaction model.The best yield can reach to 99.2%.The structures of the target compounds were confirmed by 1H NMR,IR and HRMS.In the subsequent stage,a new washing step is added to reduce the post-treatment time and increase the product molarity.The improved process is simple in operation and low in cost.The final product is a clear and transparent light yellow solution,and the product molarity and properties meet the market product quality standards.

关 键 词：六甲基二硅烷胺钠 无溶剂 洗涤 酸碱滴定 

分 类 号：O626.23[理学—有机化学]