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Ternary copper catalyst CuO-Cu2O-Cu for synthesis of dimethyldichlorosilane and its preparation method

A technology of dimethyldichlorosilane and cuo-cu2o-cu, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of poor controllability of particle size and components, reducing agent Fe Problems such as difficult removal of powder and poor controllability of catalyst particle size, etc., achieve the effect of low price, high selectivity, and simple preparation process

Inactive Publication Date: 2012-11-14
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is a gap between the selectivity and catalytic activity of the domestic catalyst dimethyldichlorosilane compared with the catalyst of the US SCM company. The catalysts used in the synthesis of this monomer in the domestic organic silicon industry are mainly imported from abroad, resulting in high production costs; Monomer dimethyldichlorosilane has wide application, large demand, and high price, and a slight improvement in the performance of copper catalysts will generate huge economic benefits; therefore, the development of domestic copper catalysts with low prices, excellent quality, and stable performance is an organic Difficulties to be Solved Urgently in the Silicon Industry
[0006] At present, the research institute of Jilin Chemical Industry Co., Ltd. uses copper salt solution and metals more active than copper as raw materials. In a reactor with a gas bubbling device, a one-step method of reduction precipitation-suspension oxidation is used to directly prepare a Copper, copper oxide, and copper ternary copper catalysts have poor controllability of particle size and components, and the residual reducing agent Fe powder is difficult to remove
The ternary copper catalyst Cu-CuO-Cu prepared by copper sulfate dehydration drying, hydrogen reduction and partial oxidation researched by the Chengdu Organic Silicon Research Center of the Ministry of Chemical Industry 2 O, there is also the problem of poor controllability of catalyst particle size

Method used

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  • Ternary copper catalyst CuO-Cu2O-Cu for synthesis of dimethyldichlorosilane and its preparation method
  • Ternary copper catalyst CuO-Cu2O-Cu for synthesis of dimethyldichlorosilane and its preparation method
  • Ternary copper catalyst CuO-Cu2O-Cu for synthesis of dimethyldichlorosilane and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Take 10g of commercial CuO powder, put it into a fluidized bed reactor, and feed 200ml / min of N 2 , to make it fluidized; at 250°C, feed 7.5ml / min of CO gas, react for 120min, and crush and ball mill to obtain a ternary copper catalyst; the composition of the obtained copper catalyst after chemical analysis is: 4% Cu, 54% Cu 2 O and 42% CuO (weight percent, the same below).

[0034] The ternary copper catalyst material prepared above was subjected to an XRD test on an X'Pert PRO MPD multifunctional X-ray diffractometer produced by Panalytical Company of the Netherlands (Panalytical).

[0035] The particle size analysis of the ternary copper catalyst material prepared above was performed on a Dandong Baite BT-9300Z laser particle size distribution analyzer.

[0036] figure 1 It is the XRD pattern of the copper catalyst that embodiment 1 obtains, wherein 2θ=36.5 ° is Cu 2The characteristic peak of O, the shoulder peak that is made up of 2θ=35.5 ° and 2θ=38.8 ° is the ...

Embodiment 2

[0039] Take 10g of commercial CuO powder, put it into a stirred bed reactor, adjust the reaction temperature to 300°C, and feed 7.5ml / min of H 2 , reacted for 90min, and crushed and ball milled to obtain a ternary copper catalyst; the composition of the obtained copper catalyst was analyzed by chemical method: 3% Cu, 58% Cu 2 O, 38% CuO.

[0040] image 3 It is the XRD figure of the copper catalyst that embodiment 1 obtains, wherein 2θ=36.4 ° is Cu 2 The characteristic peak of O, the shoulder peak that is made up of 2θ=35.5 ° and 2θ=38.6 ° is the characteristic peak of CuO, and 2θ=43.2 ° is the characteristic peak of Cu, thus it can be seen that the catalyst prepared by this method is composed of Cu, Cu 2 A ternary copper catalyst composed of O and CuO.

[0041] Figure 4 For the particle size analysis of the copper catalyst obtained in Example 1, it can be seen from the figure that the particle size of the copper catalyst prepared by this method is basically less than 10 ...

Embodiment 3

[0043] Take 10g of commercial CuO powder, put it into a fluidized bed reactor, adjust the reaction temperature to 200°C, and feed 200ml / min of N 2 , make it fluidized; adjust the CO gas flow to 6.7ml / min, the reaction time is 180min, and crush the ball mill to obtain the ternary copper catalyst; the obtained copper catalyst is composed of 7% Cu, 50% Cu after chemical analysis 2 O and 43% CuO.

[0044] Figure 5 It is the XRD pattern of the copper catalyst that embodiment 3 obtains, wherein 2θ=36.6 ° is Cu 2 The characteristic peak of O, the shoulder peak that is made up of 2θ=35.5 ° and 2θ=38.8 ° is the characteristic peak of CuO, and 2θ=43.4 ° is the characteristic peak of Cu, thus it can be seen that the catalyst prepared by this method is composed of Cu, Cu 2 A ternary copper catalyst composed of O and CuO.

[0045] Figure 6 For the particle size analysis of the copper catalyst obtained in Example 3, it can be seen from the figure that the particle size of the copper c...

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Abstract

The invention relates to the field of catalysts used for synthesis of dimethyldichlorosilane, in particular to a ternary copper catalyst CuO-Cu2O-Cu for synthesis of dimethyldichlorosilane and its preparation method. The method comprises the following steps of: 1) taking copper oxide powder as a raw material, adding a reducing gas, controlling its flow to make the flow of the reducing gas introduced into per gram of CuO particles at 0.1ml / min-100ml / min, maintaining the temperature at 100DEG C-600DEG C, carrying out a reduction reaction for 0.5h-6h, thus obtaining partially reduced copper oxide; and 2) subjecting the partially reduced copper oxide obtained in step 1) to breaking and ball-milling, thus obtaining the ternary copper catalyst for synthesis of dimethyldichlorosilane. With copper oxide as the raw material, the method prepares the ternary copper catalyst CuO-Cu2O-Cu through a one-step reaction, and has the advantages of simple technological process, convenient operation, strong process controllability, and easy mass production. The prepared catalyst shows high dimethyldichlorosilane selectivity and silicon powder material conversion rate.

Description

technical field [0001] The present invention relates to the field of the catalyst that is used for synthesizing dimethyldichlorosilane, specifically, the present invention relates to a kind of ternary copper CuO-Cu that is used for synthesizing dimethyldichlorosilane 2 O-Cu catalyst and its preparation method. Background technique [0002] In 1940, E.G. Rochow invented the technology of direct synthesis of methyl chlorosilane, which has simple process, high yield, no solvent, low risk and easy realization of continuous large-scale production. It is still the most economical methyl chloride in industry so far. Silane production pathways. [0003] Copper is a classic catalyst for the direct synthesis of methylchlorosilanes. The copper catalyst used for the direct synthesis of methylchlorosilane initially used electrolytic copper powder. Since the surface of the electrolytic copper powder is relatively dense and the specific surface area is small, it is difficult to form acti...

Claims

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Application Information

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IPC IPC(8): B01J23/72B01J37/16C07F7/16
Inventor 苏发兵王莹利宋莲英车红卫贾昭翟世辉朱德洪
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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