Bimetal nanometer catalyst as well as preparation and application method thereof

A nano-catalyst and bimetallic nano-technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, carbon monoxide or formate reaction preparation, etc., can solve the problems of high catalyst cost and high loading capacity , to achieve the effect of simple and easy operation, small size and good catalytic activity in the preparation process

Active Publication Date: 2013-04-17
贵州鑫醇科技发展有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The main purpose of the present invention is: to provide a kind of precious metal loading capacity low, high performance for the catalyst precious metal Pd loading capacity is higher in CO gas-phase oxidation coupling process of producing dimethyl oxalate in coal-to-ethylene glycol technology, catalyst cost is high, etc. Bimetallic nanocatalyst with high and good stability for CO gas-phase oxidation coupling to dimethyl oxalate and preparation method thereof

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  • Bimetal nanometer catalyst as well as preparation and application method thereof
  • Bimetal nanometer catalyst as well as preparation and application method thereof
  • Bimetal nanometer catalyst as well as preparation and application method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Weigh 1g of α-alumina and add it to 15ml aqueous solution containing 0.0163g potassium chloropalladate, 0.0170g copper chloride, 0.2220g polyvinylpyrrolidone (PVP), 0.2100g citric acid, stir at room temperature for 0.5 hours, then add A 5ml aqueous solution of 0.0700g ascorbic acid was stirred and reduced at room temperature for 16 hours, and the product was separated by filtration to obtain a filtrate and a solid, and then the solid was washed 6 times with water, absolute ethanol, and acetone, and dried in vacuum at 60°C for 8 hours. The dried solid was activated at 400°C for 3 hours in an atmosphere of pure hydrogen (flow rate 40ml / min), and then cooled to room temperature in an atmosphere of pure hydrogen to prepare the catalyst. Catalyst XPS spectrum see image 3 and Figure 4 , from the electronic binding energy of Pd3d and Cu2P, it can be seen that the valence states of Pd and Cu elements in the catalyst are both zero valence. Catalyst electron microscope photo ...

Embodiment 2

[0055] Take by weighing 1g α-alumina and join in the filtrate among the embodiment 1, stir at room temperature 0.5 hour, then add the 5ml aqueous solution that contains 0.0700g ascorbic acid, stir and reduce at room temperature for 24 hours, product filtration separation obtains filtrate and solid, then The solid was washed 6 times with water, absolute ethanol and acetone, and dried under vacuum at 60°C for 8 hours. The dried solid was activated at 400°C for 3 hours in an atmosphere of pure hydrogen (flow rate 40ml / min), and then cooled to room temperature in an atmosphere of pure hydrogen to prepare the catalyst. Catalyst transmission electron microscope photo see Figure 8 , the electron micrograph shows that the Pd-Cu nanoparticles on the catalyst are highly dispersed on the surface of the carrier, the size of the nanoparticles is distributed in the range of 1-5nm, and the average size is 2.7nm. The actual loading of Pd in ​​the catalyst was 0.121% and the actual loading o...

Embodiment 3

[0057] Weigh 1g of α-alumina and add it to 15ml aqueous solution containing 0.0163g potassium chloropalladate, 0.0200g copper acetate, 0.2220g polyvinylpyrrolidone (PVP), 0.2100g citric acid, stir at room temperature for 0.5 hours, then add 0.0700 5ml of aqueous solution of ascorbic acid was stirred and reduced at room temperature for 16 hours, and the product was filtered and separated to obtain a filtrate and a solid, and then the solid was washed 6 times with water, absolute ethanol, and acetone, and dried at 60° C. in vacuum for 8 hours. The dried solid was activated at 400°C for 3 hours in an atmosphere of pure hydrogen (flow rate 40ml / min), and then cooled to room temperature in an atmosphere of pure hydrogen to prepare the catalyst. Catalyst transmission electron microscope photo see Figure 9 , the electron micrograph shows that the Pd-Cu nanoparticles on the catalyst are highly dispersed on the surface of the carrier, the size of the nanoparticles is distributed in th...

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Abstract

The invention discloses a bimetal nanometer catalyst used for preparing dimethyl oxalate through CO gas-phase oxidative coupling as well as preparation and an application method of the bimetal nanometer catalyst, and belongs to the technical field of preparation of the dimethyl oxalate. The bimetal nanometer catalyst is characterized in that a catalyst carrier is Alpha-aluminium oxide, an active component is Pd-Cu nanometer grains, the average size of the grain is 2-3nm, the Pd content of the active component is 0.01-2% and Cu content is 0.01-0.04% according to the mass of the catalyst carrier. The catalyst is prepared through a room temperature normal position load method, the preparation method is simple, the energy dissipation is low, the catalyst is suitable for industrial production, the active component Pd-Cu nanometer grains in the catalyst has high dispersity, large specific surface area, small size and uniformity in distribution; the catalyst provided by the invention adopts the Pd-Cu bimetal nanometer grains as the active component, and a bimetal component synergistic effect and a nanometer effect are utilized to reduce the content of the noble metal PD to 0.1% under the premise of keeping the high activity and stability of the catalyst, therefore and the cost of the catalyst is greatly reduced, and the partial substitution of the noble metal is realized.

Description

Technical field: [0001] The invention belongs to the technical field of dimethyl oxalate preparation, and relates to a bimetallic nano-catalyst used for preparing dimethyl oxalate through gas-phase oxidation coupling of CO in coal-based ethylene glycol and a preparation and application method thereof. technical background: [0002] Dimethyl oxalate is an important organic chemical raw material, which can be used to prepare oxalic acid, oxalyl chloride, oxalic acid ammonium, and can also be used in fine chemical industry to produce various dyes, medicines, important solvents, extractants and various intermediates. In addition, the hydrogenation of dimethyl oxalate can produce ethylene glycol, an extremely important chemical basic raw material. Ethylene glycol is widely used and is widely used in the production of polyester and antifreeze. In 2011, the global demand for ethylene glycol exceeded 25 million tons, of which 40% was in China. However, my country's production capa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89C07C69/36C07C67/36
Inventor 彭思艳郭国聪徐忠宁陈青松王志巧王明盛姚元根
Owner 贵州鑫醇科技发展有限公司
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