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Direct synthesis of tetraalkoxysilanes in a high-pressure mechanochemical reactor
Reaction Chemistry & Engineering ( IF 3.9 ) Pub Date : 2021-12-20 , DOI: 10.1039/d1re00522g
Ilya N. Krizhanovskiy 1 , Maxim N. Temnikov 1 , Anton A. Anisimov 1 , Andrey K. Ratnikov 1, 2 , Ivan S. Levin 3 , Alexander V. Naumkin 1 , Sergey M. Chistovalov 1 , Aziz M. Muzafarov 1, 4
Affiliation  

We report the results of studies on the direct synthesis of tetraalkoxysilanes from alcohols and metallic silicon in a high-pressure mechanochemical reactor. The effect of the following factors on the process was considered: temperature (100–250 °C), amount of catalyst (0–20 wt%), type of catalyst, and type of the alcohol used in the synthesis. A silicon conversion of 90% with a selectivity of 94% with respect to a tetraalkoxysilane can be attained under optimal conditions. The studies showed that the temperature of the direct synthesis of alkoxysilanes was the lowest of the values reported to date (100 °C). Under these conditions, a silicon conversion of 77% and a selectivity of 98% with respect to a tetraalkoxysilane can be attained. It was shown that CuCl (20 wt%) exhibited the highest activity among copper-based catalysts, including CuF2, CuCl, CuBr, CuI, CuO, and Cu2O. In addition to MeOH, such alcohols as EtOH, n-BuOH, and EtO(CH2)2OH were used. The contact masses (CMs) sampled after 15 and 25 minutes and after reactions at 150, 200, and 250 °C were studied using SEM-EDX, PXRD, and XPS.

中文翻译:

在高压机械化学反应器中直接合成四烷氧基硅烷

我们报告了在高压机械化学反应器中从醇和金属硅直接合成四烷氧基硅烷的研究结果。考虑了以下因素对工艺的影响:温度(100-250°C)、催化剂的量(0-20 wt%)、催化剂的类型和合成中使用的醇的类型。在最佳条件下可以实现 90% 的硅转化率和 94% 的相对于四烷氧基硅烷的选择性。研究表明,烷氧基硅烷的直接合成温度是迄今为止报道的最低值(100°C)。在这些条件下,可以获得77%的硅转化率和98%的对四烷氧基硅烷的选择性。结果表明,CuCl (20 wt%) 在包括 CuF 在内的铜基催化剂中表现出最高的活性2、CuCl、CuBr、CuI、CuO、Cu 2 O。除了MeOH之外,还使用了EtOH、 n- BuOH、EtO(CH 2 ) 2 OH等醇。使用 SEM-EDX、PXRD 和 XPS 研究了 15 和 25 分钟后以及在 150、200 和 250 °C 下反应后的接触质量 (CM)。
更新日期:2022-01-07
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