Preparation method of Cu nanoparticle-loaded ordered mesoporous carbon catalyst

A nanoparticle and catalyst technology, which is applied in the field of preparation of ordered mesoporous carbon-supported Cu nanoparticle catalysts, can solve the problems of grain growth, catalytic activity reduction, and catalytic activity decline, and achieve high activity, high reactivity, good stability effect

Inactive Publication Date: 2015-09-09
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although activated carbon (AC)-supported chlorine-free copper-based catalysts showed good oxidative carbonylation reaction activity, the catalytic activity of this type of catalyst still declined with the progress of the reaction.
The research of Zheng Huayan et al. thinks that Cu 0 Elemental Cu in the / AC catalyst adsorbs O in the reaction atmosphere 2 converted to Cu 2 O, as the reaction proceeds, Cu 2 O grains grow up, and obvious agglomeration occurs, resulting in a decrease in catalytic activity

Method used

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  • Preparation method of Cu nanoparticle-loaded ordered mesoporous carbon catalyst
  • Preparation method of Cu nanoparticle-loaded ordered mesoporous carbon catalyst
  • Preparation method of Cu nanoparticle-loaded ordered mesoporous carbon catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 3.2g of tri-block copolymer F127 into 32g of ethanol, stir magnetically at room temperature until completely dissolved. Dissolve 8g of 25% resole phenolic resin (phenol / formaldehyde) in ethanol and 4mL with 0.08g Cu(NO 3 ) 2 ·3H 2 O (copper nitrate trihydrate) ethanol solution was slowly added to the above solution and stirred for 2h. After stirring, the solution was allowed to stand at room temperature for 4 hours, the supernatant liquid was discarded, and the viscous sol in the lower layer was placed in a blast drying oven, and the temperature was set at 85°C for 24 hours. After drying, the sample was placed in a nitrogen-protected tube furnace, and the temperature was raised to 350°C at a heating rate of 1°C / min, kept at a constant temperature for 3 hours, and then raised to 900°C at a heating rate of 3°C / min, and kept at a constant temperature for 2 hours , and finally, the sample dropped to room temperature under the protection of nitrogen to obtain Cu-OMC c...

Embodiment 2

[0029] At 40°C, 0.06g Cu(CH3 COO) 2 ·H 2 O and 3.2g triblock copolymer F127 were added to 16g ethanol, stirred for 30min until completely dissolved. Slowly add 8g of 25% ethanol solution of resole phenolic resin (resorcinol / formaldehyde) into the above solution and stir for 2h, spread the solution evenly on a watch glass, evaporate the solvent for 4h at 30°C, and place the sample Place it in a blast drying oven, heat polymerization at 100°C for 24h. Then, the sample was placed in a nitrogen-protected tube furnace, and the temperature was raised to 350 °C at a heating rate of 1 °C / min, kept at a constant temperature for 3 h, then raised to 800 °C at a heating rate of 5 °C / min, and kept at a constant temperature for 2 h, and finally , the sample dropped to room temperature under the protection of nitrogen to obtain Cu-OMC catalyst.

[0030] The transmission electron microscope test results of the catalyst are as follows: figure 2 . It can be seen that the Cu-OMC catalyst h...

Embodiment 3

[0033] Add 3.2g of tri-block copolymer F127 into 32g of ethanol, stir magnetically at room temperature until completely dissolved. 8 g of 25% ethanol solution of resole phenolic resin (phenol / formaldehyde) and 4 mL of ethanol solution dissolved with 0.08 g of copper oxalate were slowly added to the above solution in turn and stirred for 2 h. After stirring, the solution was allowed to stand at room temperature for 4 hours, the supernatant liquid was discarded, and the viscous sol in the lower layer was placed in a blast drying oven, and thermally polymerized at 85° C. for 24 hours. Then, the sample was placed in a nitrogen-protected tube furnace, raised to 300°C at a heating rate of 1°C / min, kept at a constant temperature for 3 hours, and then raised to 600-900°C at a constant temperature of 2-3°C / min. Keep it for 2-3h, and finally, the sample is lowered to room temperature under the protection of nitrogen to obtain Cu-OMC catalyst.

[0034] The transmission electron microsco...

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Abstract

The invention discloses a preparation method of a Cu nanoparticle-loaded ordered mesoporous carbon catalyst. A carbon source precursor, a template and a copper salt are co-assembled in a solvent so that the Cu nanoparticle-loaded ordered mesoporous carbon catalyst is prepared. The Cu nanoparticle-loaded ordered mesoporous carbon catalyst is a nanoscale catalyst. Copper particles with the sizes of 5-25nm are inlaid in channels and surfaces of the ordered mesoporous carbon so that migration and agglomeration in the reaction process are not produced easily. The Cu nanoparticle-loaded ordered mesoporous carbon catalyst has high stability in normal pressure continuous fixed bed gas phase methanol oxidation carbonylation synthesis of dimethyl carbonate, has good reaction activity and has a good industrial application prospect.

Description

technical field [0001] The invention belongs to the field of heterogeneous catalysis of chemical industry, and in particular relates to a preparation method of an ordered mesoporous carbon-supported Cu nano particle catalyst. Background technique [0002] Dimethyl carbonate is the simplest organic carbonate, non-toxic and easy to biodegrade. It is the basic raw material for the non-phosgene green synthesis of other carbonates and polyester materials. It is also an important non-toxic solvent and gasoline octane additive. It is widely used in the market Broad prospects. Using methanol as a raw material, the synthesis of DMC through oxidative carbonylation route has high equilibrium conversion rate, low cost and green synthesis, and is one of the important routes for clean and efficient utilization of coal. [0003] At present, catalysts using copper or palladium chloride as active components in the gas phase reaction have the problem of deactivation caused by the loss of chl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B82Y30/00B82Y40/00C07C69/96C07C68/00
Inventor 王瑞玉刘玲马静
Owner CHINA UNIV OF MINING & TECH
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