Method for preparing copper-based catalyst for synthesizing organosilicone monomer

A technology of copper-based catalyst and organosilicon, which is applied in organic chemistry, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of process stability to be improved, unstable catalytic performance, and catalyst hardening, etc., to achieve ternary The effect of convenient component content, easy control of process parameters and mild production conditions

Active Publication Date: 2014-01-15
JINCHUAN GROUP LIMITED
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The particle size distribution range of the ternary copper catalyst prepared by the above method is relatively wide, which will lead to the instability of its catalytic performance
In addition, in the preparation of ternary components by partial oxidation, since the reduction and oxidation of copper are both strong exothermic reactions, the phenomenon of runaway temperature is prone to occur during the reaction process, resulting in hardening of the catalyst, and the process stability needs to be improved.

Method used

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  • Method for preparing copper-based catalyst for synthesizing organosilicone monomer

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Step 1, dissolving 0.49kg copper sulfate pentahydrate in deionized water, heating to make a copper sulfate solution with a temperature of 80°C and a concentration of 0.31kg / L;

[0033] Step 2, dissolving 0.25kg of sodium carbonate in 2L of deionized water and heating to make an alkaline solution with a temperature of 100°C;

[0034] Step 3: Add the copper sulfate solution described in Step 1 to the alkaline solution described in Step 2 under stirring conditions, and react at a temperature of 80° C. to form gray-black precipitates; collect the precipitates by filtration and dry them.

[0035] Step 4. Dry the precipitate collected in step 3 and place it in a fluidized bed reactor. Use a mixture of hydrogen and nitrogen as a reducing medium, and use a temperature-programmed reduction method for reduction: first preheat to 150°C; then adopt a temperature program, the heating rate is 30°C / h, and the final reduction temperature is 250°C. When the final temperature is reached,...

Embodiment 2

[0040] This embodiment is the same as Example 1, except that the basic compound is bicarbonate, hydroxide or ammonia, or at least two of carbonate, bicarbonate, hydroxide and ammonia. kind.

Embodiment 3

[0042] Step 1, dissolving 0.7kg anhydrous copper nitrate in deionized water, heating to make a copper nitrate solution with a temperature of 50°C and a concentration of 0.7kg / L;

[0043] Step 2. Dissolve 0.31kg of sodium hydroxide in 1L of deionized water and heat to make an alkaline solution with a temperature of 80°C;

[0044] Step 3: Add the copper salt solution described in Step 1 to the alkaline solution described in Step 2 under agitation, react at a temperature of 50° C. to 100° C. to form precipitates; collect the precipitates by filtration and dry.

[0045] Step 4. Dry the precipitate collected in step 3 and place it in a fluidized bed reactor. Use a mixture of hydrogen and nitrogen as a reducing medium, and use a temperature-programmed reduction method for reduction: first preheat to 150°C; then use temperature programming, the heating rate is 30°C / h, the final reduction temperature is 200°C, and when it reaches 200°C, keep it for 3 hours; the initial hydrogen concen...

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Abstract

The invention discloses a method for preparing a copper-based catalyst for synthesizing an organosilicone monomer. The method comprises the following steps: firstly, dissolving a soluble copper salt into water so as to prepare a copper salt solution; secondly, dissolving an alkali compound into water so as to prepare an alkali solution; thirdly, adding the copper salt solution into the alkali solution under the stirring condition, reacting under the condition that the temperature is 50-100 DEG C so as to generate sediment, filtering and collecting the sediment, and drying; fourthly, putting the collected sediment into a fluidized bed reactor, using a mixture gas of hydrogen and nitrogen as a reduction medium for carrying out temperature programmed reduction treatment; fifthly, using a mixture gas of oxygen and nitrogen as an oxidation medium for carrying out temperature programmed oxidization treatment; sixthly, cooling to the room temperature in nitrogen atmosphere so as to obtain the copper-based catalyst. According to the method, the low-cost copper salt is used as a raw material, the preparation process is simple in produce, good in stability and tender in production condition, no complex production equipment is needed, the prepared catalyst is high in catalysis activity, the Si powder conversion rate reaches more than 34%, and the dimethyl selectivity reaches more than 81%.

Description

technical field [0001] The invention belongs to the technical field of preparation of copper-based catalysts, and in particular relates to a method for preparing copper-based catalysts for synthesizing organosilicon monomers. Background technique [0002] China is the most potential market for organosilicon products, and its demand is increasing at an annual growth rate of about 20%, but the current domestic production is difficult to meet the requirements, so organosilicon has been listed as a key industry encouraged by the state. The most important factor restricting the development of the silicone industry is the synthesis technology of silicone monomers. There are many production methods for organosilicon monomers. Take methylchlorosilane as an example. At present, the industrial production of methylchlorosilane at home and abroad is based on CH 3 The "direct method" synthesis process of Cl and Si under the action of a catalyst has the advantages of simple production pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72C07F7/16
Inventor 刘玉强鞠鹤吕清华张玉萍朱纪念庞海丽陈国举贾波孙渊君杨莹杨鸿
Owner JINCHUAN GROUP LIMITED
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