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
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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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