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High-dispersibility palladium catalyst and preparation method and application thereof

A palladium catalyst, highly dispersed technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of uneven particle size of Pd active components, poor stability, complicated methods, etc. , to achieve excellent catalytic activity and stability, good dispersion and simple preparation method

Active Publication Date: 2019-04-19
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to solve the technical problems of complex catalyst preparation process, uneven particle size of Pd active component, low activity and poor stability in the catalyst preparation process of formic acid decomposition to produce hydrogen in the prior art, and to provide a highly dispersed palladium Catalyst and its preparation method and application

Method used

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preparation example Construction

[0028] The preparation method of the highly dispersed palladium catalyst of the present invention, the steps are as follows:

[0029] 1) Using di-functional dienamide and di-functional diamine as raw materials, according to the molar ratio of the two at 1:1, react in methanol or water to form a hyperbranched polymer, and obtain a solution containing a hyperbranched polymer ;

[0030] Among them, the bis-enamide of bifunctionality is preferably one of N,N-methylenebisacrylamide, hexamethylene bisacrylamide, and ethylene bisstearamide; the diamine of bifunctionality is 1 -One of (2-pyridyl)piperazine, N-aminoethylpiperazine, 1,2-ethylenediamine, N-methylethylenediamine; there is no special restriction on the ratio of methanol or water to the polymer ; The reaction time is 12-24h, such as 12h, 14h, 16h, 18h, 20h, 22h, 24h.

[0031] 2) According to the required molar ratio of the hyperbranched polymer to palladium, the Pd(II) precursor is added dropwise to the solution containin...

Embodiment 1

[0041] At room temperature, add 0.2mmol of hexamethylenebisacrylamide and 0.2mmol of 1-(2-pyridyl)piperazine into water and react for 24h to obtain an aqueous solution containing a hyperbranched polymer. Add 0.012g of H 2 PdCl 4 Add dropwise into the aqueous solution containing the hyperbranched polymer, and react for 24 hours to obtain a composite solution containing the hyperbranched polymer-Pd nanoparticle complex; add 0.095g of Vulcan XC-72 activated carbon to 100mL of water, and ultrasonically disperse the activated carbon evenly. The activated carbon suspension is obtained; the composite solution containing the hyperbranched polymer-Pd nanoparticle complex is added to the activated carbon suspension, stirred and reacted for 12 hours, the complex is fully adsorbed on the surface of the activated carbon carrier, and is filtered by suction, washed with water, and dried , to obtain a solid; the obtained solid was decomposed and reduced for 0.5 h in an argon-hydrogen mixed ga...

Embodiment 2

[0044] At room temperature, add 1mmol N,N-methylenebisacrylamide and 1mmol N-methylethylenediamine to react in water for 10h to obtain an aqueous solution containing a hyperbranched polymer. Add 0.147g Na 2 PdCl 4 Add dropwise into the aqueous solution containing the hyperbranched polymer, and react for 20 hours to obtain a composite solution containing the hyperbranched polymer-Pd nanoparticle composite; add 0.95g of Vulcan XC-72 activated carbon to 800mL of water, and ultrasonically disperse the activated carbon evenly. The activated carbon suspension is obtained; the composite solution containing the hyperbranched polymer-Pd nanoparticle complex is added to the activated carbon suspension, stirred and reacted for 8 hours, the complex is fully adsorbed on the surface of the activated carbon carrier, and is filtered by suction, washed with water, and dried , to obtain a solid; the obtained solid was decomposed and reduced for 1 h in an argon-hydrogen mixed gas atmosphere with...

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Abstract

The invention relates to a high-dispersibility palladium catalyst and a preparation method and application thereof, and belongs to the technical field of catalysts and preparation thereof. The technical problems are solved that in the prior art, the preparation method of catalysts for decomposing formic acid to produce hydrogen is complicated and Pd active components are uneven in particle size, low in activity and poor in stability. The palladium catalyst is porous carbon surface-loaded with a hyperbranched polymer-Pd nanoparticle composite, a hyperbranched polymer is a polymer of difunctional dienamide and difunctional diamine, the particle size of the palladium catalyst is 0.8-2.0 nm, and the dispersion degree of Pd nanoparticles is greater than 80%. The invention further provides the preparation method of the palladium catalyst. The palladium catalyst has good dispersibility and stability and shows excellent catalytic performance for decomposing formic acid to produce hydrogen at room temperature, and the rate of catalyzing the decomposition of formic acid is high. The preparation method of the palladium catalyst is simple.

Description

technical field [0001] The invention belongs to the technical field of catalysts and their preparation, and in particular relates to a highly dispersed palladium catalyst and its preparation method and application. Background technique [0002] Hydrogen energy has been widely recognized as a clean energy source with high energy density. The preparation and utilization of hydrogen energy has become a hot spot of concern. Formic acid is an industrial by-product with a wide range of sources. It is cheap, safe and low-toxic. It is a liquid at room temperature and is easy to store and transport. The hydrogen content of formic acid is relatively high, which is 4.4 wt%. At present, the research on the production of hydrogen from the decomposition of formic acid is still in the initial stage. In the reaction of formic acid decomposition to produce hydrogen, the catalyst is extremely critical. It not only determines the speed and selectivity of the decomposition reaction, but its c...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J37/16B01J37/18C01B3/22
CPCB01J31/069B01J37/16B01J37/18C01B3/22
Inventor 邢巍于彦存王显孟庆磊刘长鹏葛俊杰
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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