Reparation method of ternary copper CuO-Cu2O-Cu catalyst for synthesizing methyl chlorosilane

Abstract

The invention relates to the field of the preparation of catalysts, and in particular relates to a preparation method of a ternary copper CuO-Cu2O-Cu catalyst for synthesizing methyl chlorosilane. The preparation method comprises the following steps of: putting copper powder into a heating furnace, replacing air in the heating furnace by use of nitrogen, carrying out primary oxidation in the medium temperature stage of 250-400DEG C, carrying out ball milling, rupturing a surface oxidation film stopping copper particles to be further oxidized, carrying out secondary oxidation in the medium temperature stage of 250-400DEG C, carrying out ball milling, and adjusting the component content and particle size of the catalyst through the twice oxidation and the ball milling, so as to obtain the product CuO-Cu2O-Cu catalyst, wherein the molar ratio of the air passing quantity to copper powder in the process of oxidization is 10:(1-10), the ventilation reaction time is 0.5-5 hours, the mass ratio of the ball-milled bead to the material in the process of ball milling is 20:(1-10), and the ball milling time is 0.5-8 hours. The component content and particle size of the catalyst of the preparation method can be optimally adjusted, so that the catalyst is higher in dimethyl dichloro-silane yield and silicon power raw material conversion ratio.

Description

technical field [0001] The invention relates to the field of catalyst preparation, in particular, the invention relates to a ternary copper CuO-Cu for synthesizing methylchlorosilane 2 The preparation method of O-Cu catalyst. Background technique [0002] As a new type of high-tech material, silicone material has been widely used in the fields of electronic appliances, petroleum, chemical industry, aerospace, construction, textile, medicine, daily chemical and other fields since its industrial production in the early 1940s. It is an indispensable new material for development and improvement of people's living standards. Methylchlorosilane monomer is the backbone of the entire silicone industry, and the vast majority of silicone materials contain polysiloxanes made from dimethyldichlorosilane, which is also methylchlorosilane The part with the largest demand in the chemical industry, so the synthesis of dimethyldichlorosilane is the top priority. E.G. Rochow invented the d...

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Problems solved by technology

[0006] Patent CN1072870 proposes to use copper salt solution and metals more active than copper as raw materials, and in a reaction kettle with a gas bubbling device, adopt a one-step method of reduction precipitation and suspension oxidation to directly prepare cuprous oxide, cupric oxide, and copper. Ternary copper catalyst; patent CN1008423 proposes to prepare ternary copper catalyst CuO-Cu with copper sulfate through dehydration drying, hydrogen reduction and partial oxidation and other processes 2 O-Cu; ​​patent CN1724156 also adopts copper sulfate as raw material, after drying, use ammonia synthesis gas to reduce and partially oxidize to prepare ternary copper catalyst, but the catalyst is prepared by the above method, the regulation of catalyst particle size and components is difficult, and the preparation process It is more complex and requires more special devices and equipment

Patent CN101811057 proposes the method of simply mixing copper powder, cuprous oxide, cupric oxide and ball milling to prepare ternary copper catalyst. Although the method is simple, due to the mixing of the three raw materials, in order to maintain the uniformity of the catalyst components, the The requirements of the ball milling process are relatively high, resulting in great difficulty in controlling the particle size of the catalyst, and the ball milling process is not easy to operate

[0007] Patents US4503165 and US4504597 adopt the method of ball milling partially oxidized copper powder to prepare ternary copper catalyst CuO-Cu 2 O-Cu, although it is easy to obtain a catalyst with uniform composition, the patent only describes the preparation of the catalyst by ball milling partially oxidized copper, but there is no information on how to obtain partially oxidized copper and how to control its conditions. It is given, and the patent uses primary oxidation ball milling. In the preparation process, the raw material copper powder is required to obtain the catalyst after primary oxidation ball milling. Therefore, the requirements for the partial oxidation and ball milling of copper powder are relatively strict and difficult to operate.

[0008] The oxidation process of copper powder is closely related to the particle size and oxidation temperature of copper powder (Oxidation of Metals, 2005, 63(516): 261-275). In the medium temperature stage (250-400°C), dense The oxide film on the surface of copper particles hinders further oxidation (Acta Metallica Sinica, 2008, 44(7): 821-825), but as the temperature rises further, the oxidation temperature enters the high temperature zone, and the oxide film on the surface of copper particles cracks or falls off, making Oxidation proceeds further and rapidly, the oxidation is easy to harden and uneven, and the oxidation process is difficult to operate and control

[0009] Therefore, the existing methods for preparing catalysts all have the disadvantages of preparing catalysts, the regulation of catalyst particle size and components is relatively difficult, the preparation process is relatively complicated, and more special devices and equipment are needed or the preparation process is not easy to control, and the catalytic efficiency is low, Therefore, it is of great significance to improve the catalytic effect of the catalyst and make the preparation process simple and easy.

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