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Preparation method of highly dispersed supported metal catalyst

A metal 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 nanocluster growth and other problems

Active Publication Date: 2019-03-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the thiol molecules on the surface of this type of catalyst occupy the active sites on the metal surface, which has a great inhibitory effect on the catalytic performance of the metal, and the removal of these surface molecules by roasting may lead to the growth of nano-clusters, so How to prepare highly dispersed supported cluster catalysts is an urgent scientific problem and one of the key issues for the industrial application of metal nanocatalysts.

Method used

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  • Preparation method of highly dispersed supported metal catalyst
  • Preparation method of highly dispersed supported metal catalyst
  • Preparation method of highly dispersed supported metal catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Embodiment 1, Au (0.1wt%) / SiO 2 -NH 2 Catalyst preparation:

[0019] (1) Weigh 1.0g Si0 2 Carrier, ultrasonically dispersed into 50mL ethanol and 1mL of 3-aminopropyltriethoxysilane was added, then stirred under reflux for 8h, the precipitate was filtered and washed with deionized water, and dried at 80°C for 12h to obtain the surface function oxidized oxide support.

[0020] (2) Weigh 0.5g of the above-prepared oxide carrier, add it to 50mL of chloroauric acid solution with a concentration of 0.051mmol / L, and stir and adsorb at room temperature for 1h, then filter and wash the obtained mixture drying in an oven to obtain an oxide carrier with metal precursors loaded on its surface.

[0021] (3) Control the air humidity to be 10%, mix the oxide carrier obtained in step (2) with 0.1g sodium borohydride solid and then transfer it to a planetary ball mill, adjust the rotating speed to 200 rpm, grind for 5h, and then grind the obtained solid After washing with water an...

Embodiment 2

[0023] Embodiment 2, Au (0.5wt%) / SiO 2 -NH 2 Catalyst preparation:

[0024] (1) Weigh 1.0g Si0 2 Carrier, ultrasonically dispersed into 100mL ethanol and 2mL of 3-aminopropyltriethoxysilane was added, then stirred under reflux for 12h, the precipitate was filtered and washed with deionized water, and dried at 100°C for 8h to obtain the surface function oxidized oxide support.

[0025] (2) Weigh 0.5g of the above-prepared oxide carrier, add it to 100mL of chloroauric acid solution with a concentration of 0.127mmol / L, and stir and adsorb at room temperature for 3h, then filter and wash the obtained mixture drying in an oven to obtain an oxide carrier with metal precursors loaded on its surface.

[0026] (3) Control the air humidity to be 15%, mix the oxide carrier obtained in step (2) with 0.1g sodium borohydride solid and then transfer it to a planetary ball mill, adjust the rotating speed to 300 rpm, grind for 3h, and then grind the obtained solid After washing with water...

Embodiment 3

[0028] Embodiment 3, Au (1.5wt%) / TiO 2 -NH 2 Catalyst preparation:

[0029] (1) Weigh 1.0g Ti0 2(Anatase) carrier, ultrasonically dispersed into 150mL ethanol and added 3mL of 3-aminopropyltriethoxysilane, then stirred under reflux for 24h, filtered the precipitate and washed with deionized water, dried at 120°C for 6h , that is, the surface functionalized oxide support.

[0030] (2) Weigh 0.5g of the above-prepared oxide carrier, add it to 150mL of chloroauric acid solution with a concentration of 0.338mmol / L, and stir and adsorb at room temperature for 5h, then filter and wash the obtained mixture drying in an oven to obtain an oxide carrier with metal precursors loaded on its surface.

[0031] (3) Control the air humidity to 20%, mix the oxide carrier obtained in step (2) with 0.1g sodium borohydride solid and then transfer it to a planetary ball mill, adjust the rotating speed to 400 rpm, grind for 2h, and then grind the obtained solid After washing with water and eth...

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Abstract

The invention relates to a preparation method of a highly dispersed supported metal catalyst. The method comprises: adsorbing one of metal precursors such as chloroauric acid, tetrachloropalladic acidor chloroplatinic acid onto a surface of a carrier and drying; and grinding the product with a certain air humidity to achieve in-situ reduction the metal precursor by utilizing active hydrogen generated by slow hydrolysis of a reducing agent that is NaBH4 or KBH4, thus preparing the catalyst. The method is performed without a solvent at room temperature, and avoids particle growth caused by liquid phase nucleation and high temperature sintering, so as to obtain the highly dispersed or even monoatomic catalyst suitable for catalytic hydrogenation reaction.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a method for preparing highly dispersed and supported metal catalysts by using a solid phase reduction method. Background technique [0002] Metal catalysts (noble metals such as Au, Pt, Ru, Au, Pd, and non-noble metals Ni, Fe, Cr, Co, etc.) have attracted much attention because of their excellent catalytic activity and selectivity, and have been widely used in hydrogenation, desorption Chlorine, oxidation, aromatization, coupling and other reactions. However, the particle size of metal nanoparticles usually has a great influence on the efficiency and selectivity of catalysts. Especially for noble metal catalysts, small-sized particles can not only provide more surface atoms to promote the reaction, but also greatly improve the efficiency and selectivity of catalysts. The utilization rate of the metal has a very good promotion effect on its industrial large-scale a...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J37/16
CPCB01J27/24B01J37/16
Inventor 黄延强刘清港王新葵杨小峰张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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