Preparation method used for combining dimethyl carbonate efficient catalysts

A technology of dimethyl carbonate and a catalyst is applied in the field of preparation of a catalyst for synthesizing dimethyl carbonate by methanol liquid phase oxidative carbonylation, and can solve the problems of uneven catalyst particles, poor dispersion of active components, easy agglomeration of active components, and the like, Achieve the effect of reducing equipment corrosion, reducing production costs, high selectivity and yield

Inactive Publication Date: 2012-12-26
HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst particles prepared by the solid-phase method and the impregnation method are not uniform, and the dispersion of the active components is poor; the catalysts prepared by the sol-gel method are easy to agglomerate during the subsequent heat treatment process, which reduces the dispersion.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0019] Take 5.7g Cu(NO 3 ) 2 , dissolved in 100mL deionized water, added 38.8g activated carbon, activated carbon is prepared from fruit shell raw materials, the specific surface area is 1127m 2 / g, the iodine adsorption value is 806mg / g, and the mesh number is 200 mesh. Stir evenly, then add 2.3mol / L of KBH dropwise 4 For reduction, use magnetic stirring during the dropwise addition process, the rotation speed is 500r / min, and the reduction temperature is 30°C. After the reduction is complete, filter and wash until the filtrate is neutral, and dry at 50-70°C to prepare the catalyst for use.

[0020] Weigh 5g of the prepared catalyst and add it to a 500mL autoclave, then add 200mL of anhydrous methanol, pressurize it to 3.0Mpa with nitrogen, then switch the nitrogen to a mixed gas (O 2 : 8%, CO: 92%). The reaction was carried out at 100° C. for 2 hours. After cooling, gas chromatography was used for analysis, and the selectivity of dimethyl carbonate was 96.78%, and the s...

example 2

[0022] Take 8.2g Cu(NO 3 ) 2 , dissolved in 100mL deionized water, added 34.9g of activated carbon, activated carbon is prepared from fruit shell raw materials, the specific surface area is 1236m 2 / g, the iodine adsorption value is 997mg / g, and the mesh number is 180 mesh. Stir evenly, then add 3.1mol / L of KBH drop by drop 4 For reduction, magnetic stirring is used during the dropping process, the number of revolutions is n=500r / min, and the reduction temperature is 40°C. After the reduction is complete, filter and wash until the filtrate is neutral, and dry at 50-70°C to prepare the catalyst for use.

[0023] Weigh 5g of the prepared catalyst and add it to a 500mL autoclave, then add 200mL of anhydrous methanol, pressurize it to 3.0Mpa with nitrogen, then switch the nitrogen to a mixed gas (O 2 : 8%, CO: 92%). The reaction was carried out at 100° C. for 2 hours. Adopt gas chromatographic analysis after cooling, the selectivity of dimethyl carbonate is 99.67%, and the sp...

example 3

[0025] Take 6.5g Cu(NO 3 ) 2 , dissolved in 100mL of deionized water, added 18.4g of activated carbon, activated carbon is prepared from woody raw materials, the specific surface area is 1584m 2 / g, the iodine adsorption value is 971mg / g, and the mesh number is 210 mesh. Stir evenly, then add 4.2mol / L NaH dropwise 2 PO 2 For reduction, magnetic stirring is used during the dropwise addition process, the number of revolutions is n=500r / min, and the reduction temperature is 90°C. After the reduction is complete, filter and wash until the filtrate is neutral, and dry at 50-70°C to prepare the catalyst for use.

[0026] Weigh 5g of the prepared catalyst and add it to a 500mL autoclave, then add 200mL of anhydrous methanol, pressurize it to 3.0Mpa with nitrogen, then switch the nitrogen to a mixed gas (O 2 : 8%, CO: 92%). The reaction was carried out at 100° C. for 2 hours. Adopt gas chromatographic analysis after cooling, the selectivity of dimethyl carbonate is 92.46%, the s...

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Abstract

The invention discloses a preparation method for combining dimethyl carbonate efficient catalysts. The preparation method for combining the dimethyl carbonate efficient catalysts comprises the following steps of dipping activated carbons into aqueous solutions of copper compounds, dropwise adding reducing agent solutions to the aqueous solutions to carry out reduction, stirring in magnetic mode and keeping certain reduction temperature, after reduction, filtering and washing until washed filtrate is neutral, then drying. At last people can obtain the catalysts, wherein active components of the catalysts are copper Cu and carriers of the catalysts are active carbons. Compared with the prior art, when the catalysts which are prepared by the preparation method for combining the dimethyl carbonate efficient catalysts are used for dimethyl carbonate combined by methanol liquid-phase oxidative carbonylation, the catalysts are provided with the higher selectivity and yield of the dimethyl carbonate and have the advantages of greatly reducing corrosion of equipment, improving product quality, and lowering product cost.

Description

technical field [0001] The invention relates to a method for preparing a catalyst, in particular to a method for preparing a catalyst for liquid-phase oxidative carbonylation of methanol to synthesize dimethyl carbonate. Background technique [0002] Dimethyl carbonate is an important green organic chemical raw material, which is widely used in the fields of coatings, medicine, pesticides, organic chemical raw materials, food additives, antioxidants, gasoline additives, and electronic chemicals. At present, the production of dimethyl carbonate mainly adopts the process route of methanol liquid-phase oxidative carbonylation. This process is to feed oxygen or air and CO into liquid-phase methanol to generate dimethyl carbonate under the action of a catalyst. There are two main types of catalysts that are widely considered to have effective catalytic performance in the synthesis of dimethyl carbonate. One is based on metal oxides or molecular sieves, PdCl 2 -CuCl 2 , CuCl 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72C07C69/96C07C68/00
Inventor 银凤翔李国儒陈标华王亮
Owner HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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