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Preparation method of ZnO assistant-containing copper catalyst for synthesis of methylchlorosilane

A technology of methyl chlorosilane and copper catalyst, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., which can solve the problems of unfavorable ball milling and uniform dispersion of additive ZnO, Problems such as uneven particle density and difficult operation and control of ball milling can achieve the effects of good catalytic effect, high equipment utilization rate and low production cost

Active Publication Date: 2014-06-04
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

[0011] The purpose of the present invention is to overcome the inhomogeneity of ball milling particle density in the process of adding additive ZnO in the preparation process of copper catalyst in the prior art, which is not conducive to the uniform dispersion of ball milling and additive ZnO, or the process is complicated, difficult to operate and control, and the catalyst cost Higher defect, thereby providing a kind of preparation method for the copper catalyst containing auxiliary agent ZnO that is used for synthesizing methyl chlorosilane

Method used

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  • Preparation method of ZnO assistant-containing copper catalyst for synthesis of methylchlorosilane
  • Preparation method of ZnO assistant-containing copper catalyst for synthesis of methylchlorosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Add the sodium carbonate solution with a concentration of 1.5mol / L into the zinc chloride solution with a concentration of 8mol / L under stirring to obtain a white jelly, add 300g of atomized copper powder to the white jelly, and fully Stir to obtain a uniform mixture of white jelly and copper powder. After standing and aging for 4 hours to separate layers, wash and filter the sediment in the lower layer to obtain a uniform mixture of copper powder and basic zinc carbonate. The mixture was placed in a vacuum drying oven, dried in vacuum at 30°C for 6 hours, pulverized, put into a tube furnace, and air was introduced when the temperature was raised to 400°C. The molar ratio of the amount of air to the copper powder added was 15. After oxidizing for 5 hours, stop heating and aeration. The obtained mixture of partially oxidized copper powder and ZnO was subjected to wet ball milling, the mass ratio of ball milling beads to material was 20, the mass ratio of ball milling bea...

Embodiment 2

[0051] Add the sodium carbonate solution with a concentration of 3.5mol / L into the zinc nitrate solution with a concentration of 20mol / L under stirring to obtain a white jelly, add 300g of electrolytic copper powder to the white jelly, and fully stir, A homogeneous mixture of white jelly and copper powder was obtained, and after standing and aging for 8 hours to separate layers, the lower sediment was washed and filtered to obtain a homogeneous mixture of copper powder and basic zinc carbonate. The mixture was placed in a vacuum drying oven, dried under vacuum at 100°C for 5 hours, pulverized, put into a tube furnace, and air was introduced when the temperature was raised to 400°C. The molar ratio of the amount of air to the copper powder added was 15. After oxidizing for 5 hours, stop heating and aeration. The obtained mixture of partially oxidized copper powder and ZnO was subjected to dry ball milling, the mass ratio of ball milling beads to material was 2, and the ball mil...

Embodiment 3

[0053] Add the sodium carbonate solution with a concentration of 1.5mol / L into the zinc sulfate solution with a concentration of 10mol / L under stirring to obtain a white jelly. After standing and aging for 12 hours, add 300g of electrolytic copper powder, and fully Stir, wash and filter to obtain a uniform mixture of copper powder and basic zinc carbonate. The mixture was placed in a vacuum drying oven, dried under vacuum at 100°C for 1 hour, pulverized, put into a tube furnace, and air was introduced when the temperature was raised to 600°C. The molar ratio of the amount of air to the copper powder added was 8. After oxidizing for 2.5 hours, stop heating and ventilation. The obtained mixture of partially oxidized copper powder and ZnO was subjected to wet ball milling, the mass ratio of ball milling beads to material was 2, the mass ratio of ball milling beads to liquid dispersant was 1, and the ball milling time was 4 hours. After ball milling, the catalyst samples were obt...

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Abstract

The invention discloses a preparation method of a ZnO assistant-containing copper catalyst for synthesis of methylchlorosilane. The preparation method comprises the following steps of in wet-method preparation of zinc oxide, adding copper powder into the preparation system, carrying out stirring mixing, carrying out filtration and drying to obtain a uniform mixture of basic zinc carbonate and the copper powder, carrying out calcination at a temperature of 400-600 DEG C for 1-5h to obtain a uniform mixture of zinc oxide and Cu-Cu2O-CuO powder, carrying out ball milling, carrying out filtration and carrying out drying to obtain the ZnO assistant-containing copper catalyst. The preparation method realizes preparation of the ZnO assistant-containing copper catalyst by combination of copper powder partial oxidation and wet-method preparation of zinc oxide, and has simple processes, a high equipment utilization rate and a low production cost. Uniform mixing of raw materials are realized easily by a wet method, and after sintering, sintered particles comprising uniformly mixed Cu-Cu2O-CuO powder and zinc oxide are obtained. The preparation method is conducive to further ball milling and uniform dispersion of a ZnO assistant. The ZnO assistant-containing copper catalyst has high catalyst activity and high selectivity.

Description

technical field [0001] The invention relates to the field of catalysts used for synthesizing methylchlorosilanes, in particular, the invention relates to a method for preparing a copper catalyst containing auxiliary agent ZnO used for synthesizing methylchlorosilanes. Background technique [0002] Organosilicon materials are a class of polymer compounds with Si-O bonds as the main body and organic groups introduced as side chains on Si atoms. Because it has both organic and inorganic structures, organosilicon materials have many excellent properties and special functions, and are widely used in cutting-edge defense technologies and various sectors of the national economy. The production of organosilicon materials is inseparable from organosilicon monomers. Among them, the amount of methylchlorosilane accounts for more than 90% of the total amount of organosilicon monomers, and the amount of dimethyldichlorosilane (dimethyl for short) in methylchlorosilane is the largest ( a...

Claims

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Application Information

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IPC IPC(8): B01J23/80C07F7/16
Inventor 高俊杰李云杰张学迪刘殿忠张振玉张懿
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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