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Sheet-shaped or polyhedron-shaped supported silver catalyst and preparation method thereof

A technology of supported silver and polyhedron, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. Uniformity, irregular shape, etc.

Inactive Publication Date: 2014-05-07
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The supported catalyst particles prepared by the impregnation method used in industry have irregular shape and non-uniform size, and it is difficult to improve the activity and selectivity.
[0004] Silver is the most widely used ethylene epoxidation catalyst in industry, and its morphology has a significant effect on the improvement of catalytic selectivity and activity (Phillip Christopher et al., ChemCatChem, 2010, 2, 78~83.), but currently there is a lack of A method for morphology-controlled synthesis on alumina substrates

Method used

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  • Sheet-shaped or polyhedron-shaped supported silver catalyst and preparation method thereof
  • Sheet-shaped or polyhedron-shaped supported silver catalyst and preparation method thereof
  • Sheet-shaped or polyhedron-shaped supported silver catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh 4.2967g of silver oxide into a 20ml glass sample bottle, place the sample bottle in an ice-water bath, and add 12.0ml of deionized water under stirring conditions. After stirring for 30min, 2.57g oxalic acid hydrate (H 2 C 2 o 4 2H 2 O) Slowly add to the above solution in batches and react for 1h. The resulting liquid was then transferred to a centrifuge tube, and the supernatant was removed by centrifugation. Add about 6.0 ml of deionized water to the obtained precipitate, stir and wash thoroughly, then centrifuge to remove the supernatant, and repeat the washing twice. Add 12ml of deionized water to the above sample, place it in an ice-water bath, stir for 10min, slowly add 5.0ml of ethylenediamine dropwise to the resulting mixture, cover the bottle, and continue stirring for 1h, then turn the resulting solution at 5000 rpm Centrifuge for 10 minutes under the condition of 10 minutes, absorb the supernatant, impregnate 9.0g of α-alumina particles A (specific...

Embodiment 2

[0040] Weigh 4.2969g of silver oxide into a 20ml glass sample bottle, place the sample bottle in an ice-water bath, and add 13.3ml of deionized water under stirring conditions. After stirring for 30 min, 2.42 g of oxalic acid hydrate was slowly added to the above solution in batches, and reacted for 1 h. Then transfer the obtained liquid into a centrifuge tube, rinse the sample bottle with a small amount of deionized water, recover the sample into the centrifuge tube as much as possible, centrifuge at 5000 rpm for 5 min, and remove the supernatant. Add about 4 ml of deionized water to the obtained precipitate, stir and wash thoroughly, then centrifuge to remove the supernatant, and repeat the washing twice. Add 13.4 ml of deionized water to the above sample, place it in an ice-water bath, stir for 10 minutes, slowly add 5.0 ml of ethylenediamine dropwise to the resulting mixture, and continue stirring for 1 hour, then centrifuge the resulting solution at 5000 rpm 10min, absor...

Embodiment 3

[0044] Weigh 0.4412g trisodium citrate (C 6 h 5 o 7 Na 3 2H 2 O), add 20ml of deionized water, fully stir and dissolve, and obtain a 75mM trisodium citrate aqueous solution.

[0045] Weigh 0.088g of the loaded silver catalyst sample CatB prepared above, place it in a 500ml beaker covered with aluminum foil in the dark, add 75ml of deionized water, and add the above-mentioned trisodium citrate solution 17.2ml, 17.2ml successively under stirring conditions. ml 30wt% hydrogen peroxide, stirred for 10 minutes, then added 42.9ml of newly prepared 0.1M sodium borohydride solution, and continued to react for 2 hours. The obtained solid-liquid mixture is rich in nano-silver flakes and can be used directly. If the liquid solution is removed by leaching, the remaining solid sample is dried at room temperature for 24 hours to obtain a sample that is rich in flake nano-silver on the surface (SEM image see Image 6 ).

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Abstract

The invention relates to a sheet-shaped or polyhedron-shaped supported silver catalyst and a preparation method thereof. The invention belongs to the technical field of a supported silver catalyst. According to the invention, sheet-shaped or polyhedron-shaped supported silver is loaded on a carrier. The catalyst is prepared by using a two-step method. First, supported near-spherical silver particles are prepared; and with a chemical corrosion-regeneration method, the metal silver particles loaded on the carrier are converted in-situ into sheet-shaped or polyhedron-shaped metal silver particles. With the method provided by the invention, the obtained supported sheet-shaped or polyhedron-shaped metal silver particles can be applied in fields such as olefin partial oxidation reaction catalyzing, surface-enhanced Raman, surface-enhanced fluorescence, electrocatalysis, and the like. The preparation method is simple and feasible, and is suitable for large-scale preparations.

Description

technical field [0001] The invention relates to a supported silver catalyst, in particular to a flake or polyhedral supported silver catalyst and a preparation method of "impregnation-conversion", belonging to the technical field of supported silver catalysts. Background technique [0002] The catalyst itself is mostly nanoparticles. Studies have shown that the catalytic performance of materials is closely related to the size and shape of particles (Ahmadi Temer S., Wang Z.L., etc., Science, 1996, 272, 1924~1925; Dureuil V., etc., J. Crystal Growth, 2001, 233, 737~748 .). In particular, nanoparticles with different morphologies expose different crystal faces, resulting in huge differences in activity and selectivity. Therefore, when synthesizing catalyst nanoparticles, it is very important to control their shape while controlling their size and size distribution (Puntes V.F. et al., Science, 2001, 291:2115~2117.). [0003] Although the research on the controllable prepara...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J35/02B01J23/50C07D301/10C07D303/04B01J35/00
Inventor 蒋军孙晓明孙芳孙晚霞张慧段雪
Owner BEIJING UNIV OF CHEM TECH