Contact Mass in the Direct Synthesis of Alkoxysilanes. Raman Spectroscopy Study

ИНЭОС OPEN Pub Date : 2023-05-30 DOI:10.32931/io2218a
S. S. Bukalov, M. N. Temnikov, I. N. Krizhanovskiy, R. R. Aysin
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Abstract

Raman spectroscopy was used to study the composition of contact masses (CMs) CuCl + Si obtained by different methods, which are utilized in the direct synthesis of alkoxysilanes. The CMs prepared by the classical method were shown to include copper oxides in a mixture with silicon and on the surface of metallic copper and Cu5Si intermetallide. Along with copper oxides, an active phase containing terminal Cu–Cl groups was also observed. In the case of mechanochemical synthesis, the formation of copper oxides was not observed. In view of the metallic conductivity of Cu3Si and Cu5Si, their direct identification using Raman spectra is not possible. All the mentioned copper-containing phases are involved in the reaction with alcohols and esters as catalysts. A difference between the two methods for obtaining CMs comes down to the presence or absence of a "catalytic cocktail", which significantly affects the parameters of the direct synthesis course.
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直接合成烷氧基硅烷的接触质量。拉曼光谱研究
利用拉曼光谱研究了不同方法得到的CuCl + Si接触质量(CMs)的组成,这些接触质量可用于直接合成烷氧基硅烷。用经典方法制备的CMs在与硅的混合物中以及在金属铜和Cu5Si金属间化物的表面上都含有铜氧化物。除了铜氧化物外,还观察到含有末端Cu-Cl基团的活性相。在机械化学合成的情况下,没有观察到铜氧化物的形成。考虑到Cu3Si和Cu5Si的金属导电性,用拉曼光谱直接识别它们是不可能的。上述所有含铜相都参与了以醇和酯为催化剂的反应。两种获得CMs的方法之间的差异归结为“催化混合物”的存在与否,这对直接合成过程的参数有很大影响。
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