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Efficient stable supported copper-based catalyst and preparation method thereof

A copper-based catalyst and stable loading technology, which is applied in the field of efficient and stable loaded copper-based hydrogenation catalyst and its preparation, can solve the problems of unstable structure, poor dispersion of copper active components, poor molecular dynamics diffusion performance, etc., and achieve Effects of improved stability, unique structural advantages, and high accessibility

Active Publication Date: 2019-04-05
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is aimed at Cu / SiO in the prior art 2 In order to solve the problems of poor dispersion of copper active components in the catalyst, unstable structure and poor molecular dynamics diffusion performance, a high-efficiency and stable supported copper-based catalyst and its preparation method are provided

Method used

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  • Efficient stable supported copper-based catalyst and preparation method thereof
  • Efficient stable supported copper-based catalyst and preparation method thereof
  • Efficient stable supported copper-based catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A highly dispersed and stable copper-based catalyst is prepared by the following method:

[0038] 1) Mix 40ml of N,N-dimethylformamide and 100ml of ethanol to form a solution, add 20g of 2,3-pyridinedicarboxylic acid into it and stir until completely dissolved, then add 1.8mol / L Cu( NO 3 )·3H 2 O solution until completely dissolved, continue to stir and disperse at 1500rpm for 1 hour, transfer the mixed solution to a reaction kettle at 120°C for 12 hours; after the reaction is complete, naturally cool to room temperature, filter with suction, wash with distilled water and absolute ethanol three times each, to obtain It is a crystalline solid, and the sample is dried in a vacuum oven at 120°C for 24 hours to obtain a bulk copper-organic coordination material, which is ground into a powder with a particle size of 400 mesh.

[0039] 2) Disperse 15g of copper-organic coordination material solid powder obtained in 1) in 623ml of deionized water to form a suspension, then a...

Embodiment 2

[0042] A highly dispersed and stable copper-based catalyst is prepared by the following method:

[0043] 1) Mix 50ml of N,N-dimethylformamide and 300ml of isopropanol to form a solution, add 20g of 3,5-pyridinedicarboxylic acid into it and stir until completely dissolved, then slowly stir and add 1.08mol / L concentration of Cu(CH 3 COO) 2 ·H 2 O solution until completely dissolved, continue to stir and disperse at 600rpm for 4 hours, transfer the mixed solution to a reaction kettle at 130°C for 24 hours; after the reaction is complete, naturally cool to room temperature, filter with suction, wash with distilled water and absolute ethanol three times each, to obtain Crystalline solid, the sample was dried in a vacuum oven at 105°C for 48 hours to obtain a bulk copper-organic coordination material, which was ground into a 350-mesh powder.

[0044] 2) Disperse 10 g of copper-organic coordination material solid powder obtained in 1) in 305 ml of deionized water to form a suspens...

Embodiment 3

[0046] A highly dispersed and stable copper-based catalyst is prepared by the following method:

[0047] 1) Mix 60ml of N,N-dimethylformamide and 100ml of butanol into a solution, add 20g of 2,2'-bipyridyl-5,5'-dicarboxylic acid into it and stir until completely dissolved, then stir slowly Add 0.41mol / L concentration of CuCl 2 2H 2 O solution until completely dissolved, continue to stir and disperse at 1200rpm for 3 hours, transfer the mixed solution to a reaction kettle at 105°C for 48 hours; after the reaction is complete, naturally cool to room temperature, filter with suction, wash with distilled water and absolute ethanol three times each, to obtain Crystalline solid, the sample was dried in a vacuum oven at 145°C for 12 hours to obtain a bulk copper-organic coordination material, which was ground into a 325-mesh powder.

[0048] 2) Disperse 20 g of copper-organic coordination material solid powder obtained in 1) in 777 ml of deionized water to form a suspension, then a...

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Abstract

The invention discloses an efficient stable supported copper-based catalyst and a preparation method thereof. Soluble copper solution is added into six-membered heterocyclic radical dicarboxylic acid,N, N-dimethyl formamide and alcohol mixed solution, reaction is performed to form a copper-organic ligand material, the material is crushed and grinded into dry powder, and the dry powder is added into water to form slurry. The slurry reacts with a silicon precursor compound, a triblock copolymer P123, monobasic acid and alcohol to obtain the efficient stable supported copper-based catalyst provided with a central radial mesoporous channel, the surface of the catalyst is folded, copper content is 15-45% of the total weight of the catalyst, cuprous content is 40-80mol% of the total mole numberof active copper, the specific surface area of the catalyst is larger than 500m<2> / g, the pore volume of the catalyst is larger than 1.0ml / g, and average mesoporous size is 3.0-8.0nm. The catalyst isused for glycol synthesis reaction by dimethyl oxalate hydrogenation, dimethyl oxalate conversion rate is higher than 99%, and glycol selectivity is higher than 96%.

Description

technical field [0001] The invention relates to a high-efficiency and stable supported copper-based hydrogenation catalyst and a preparation method thereof, in particular to a Cu / SiO catalyst used for hydrogenation of dimethyl oxalate to synthesize ethylene glycol 2 Catalyst and method for its preparation. Background technique [0002] The hydrogenation reaction of dimethyl oxalate (DMO) is the most critical step in the process of CO coupling synthesis of ethylene glycol. At the same time, in addition to the production of ethylene glycol, the hydrogenation reaction of dimethyl oxalate can also be used to produce methyl glycolate (MG) and ethanol, which are important components of the coal chemical industry chain. In 1985, UCC Corporation of the United States applied for two patents on the hydrogenation of dimethyl oxalate. The US4677234 technology mainly uses copper carbonate and ammonium carbonate as raw materials to prepare Cu-Si catalysts; US4628128 introduces a Cu-Si ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J35/10C07C29/149C07C31/20
CPCC07C29/149B01J23/72B01J35/618B01J35/617B01J35/638B01J35/647C07C31/202Y02P20/52
Inventor 王志光王建青王炳春李进
Owner CHINA CATALYST HLDG CO LTD
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