Continuous and Batch Organomagnesium Synthesis of Ethyl-Substituted Silanes from Ethylchloride, Tetraethoxysilane, and Organotrichlorosilane for Production of Polyethylsiloxane Liquids. 2. Continuous One-Step Synthesis of Ethylethoxy- and Ethylchlorosilanes
作者:Boris A. Klokov
DOI:10.1021/op000100p
日期:2001.5.1
them are (1) the replacement of some tetraethoxysilane 3 by ethyltrichlorosilane 10, (2) the optimum concentration of 3 and 10, (3) the excess of the granulated magnesium (the supply rate 50−110 g h-1), and, finally, (4) the columnar apparatus with the stirrer, resulting in high yields of di- and triethylsilanes, low duration of synthesis, and high selectivity of Grignard reagent. Continuous one-step
描述了用于乙基乙氧基和乙基氯硅烷的连续一步制造工艺的开发。改进了乙基取代硅烷的合成方法。成功合成的重要因素已经确定。其中有(1)用乙基三氯硅烷 10 代替部分四乙氧基硅烷 3,(2)3 和 10 的最佳浓度,(3)粒状镁的过量(供给量 50-110 g h-1),以及, 最后, (4) 带有搅拌器的柱状装置, 导致二和三乙基硅烷的高收率, 合成持续时间短, 格氏试剂的选择性高。连续一步合成已被纳入工业(高达 7-40 kg h-1 的镁),用于生产末端三乙基甲硅烷氧基含量低(5-20%)和高含量(高达 40%)的低聚乙基硅氧烷团体。描述了格氏合成的R/D过程规则。