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Method for preparing high-load precious metal monatomic catalyst by in-situ photoreduction method

A high-load, precious metal technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the dispersion and catalytic performance. It can solve the problems of low dispersion and catalytic performance, low cost and simple preparation method.

Active Publication Date: 2021-01-05
SHANGLUO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the embodiments of the present invention is to provide a method for preparing a high-loaded noble metal single-atom catalyst by in-situ photoreduction, so as to solve the problem of low dispersibility and catalytic performance caused by the low single-atom loading prepared by the existing method

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  • Method for preparing high-load precious metal monatomic catalyst by in-situ photoreduction method
  • Method for preparing high-load precious metal monatomic catalyst by in-situ photoreduction method
  • Method for preparing high-load precious metal monatomic catalyst by in-situ photoreduction method

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Embodiment 1

[0034] The method for preparing the high-loaded gold single-atom catalyst by in-situ photoreduction method is carried out according to the following steps:

[0035] Step S1. After 0.5g graphene oxide is hydrothermally treated with 40ml of 1 mol / L sodium acetate at 180°C for 12 hours, it is washed with deionized water and absolute ethanol until the pH is (7,9], and the ultrasonic dispersion is 0.5 h;

[0036] Step S2, add 0.2 ml of acetylacetone to the solution obtained in step S1, and add dimethyl (acetylacetonate) gold (III) with a loading capacity of 5% (that is, the amount of gold in dimethyl (acetylacetonate) gold (III) The mass is 5% of the mass of graphene oxide) magnetic stirring after mixing;

[0037]Step S3, under an inert atmosphere, turn on a 500W metal halide lamp, carry out in situ photoreduction under the light of an inert atmosphere, and then freeze-dry to prepare a gold single atom catalyst. The reaction temperature of the in situ photoreduction is 35° C., and...

Embodiment 2

[0039] The method for preparing the highly loaded platinum single-atom catalyst by the in-situ photoreduction method is carried out according to the following steps:

[0040] Step S1. After 0.3g of azagraphene is hydrothermally treated with 40ml of 10mol / L potassium hydroxide at 130°C for 18h, it is washed with deionized water and absolute ethanol until the pH is (7,9] and ultrasonically dispersed 0.5h;

[0041] Step S2, adding 0.1 ml of acetone and palladium chloride with a loading capacity of 5% to the solution obtained in step S1 (that is, the mass of the palladium element in the palladium chloride is 5% of the mass of azagraphene) and magnetic stirring after mixing;

[0042] Step S3, under an inert atmosphere, turn on a 1000W high-pressure mercury lamp, perform in-situ photoreduction under inert atmosphere light, and then freeze-dry to prepare a platinum single-atom catalyst. The reaction temperature for in-situ photoreduction is 20° C., and the reaction time is 0.1 h. Th...

Embodiment 3

[0044] The method for preparing the palladium single-atom catalyst of high load by in-situ photoreduction method is carried out according to the following steps:

[0045] Step S1, after stirring 0.02g of azagraphene with 40ml of 5mol / L potassium hydroxide for 8h, wash it with deionized water and absolute ethanol until the pH is (7,9], and ultrasonically disperse for 1.0h ;

[0046] Step S2, adding 0.05ml of acetone and palladium chloride with a loading capacity of 3% to the solution obtained in step S1 (that is, the mass of the palladium element in the palladium chloride is 3% of the mass of azagraphene) and magnetic stirring after mixing;

[0047] Step S3, under an inert atmosphere, turn on a 600W metal halide lamp, perform in situ photoreduction under inert atmosphere light, and then freeze-dry to prepare a palladium single atom catalyst. The reaction temperature of the in situ photoreduction is 5° C., and the reaction time is 0.4 h. The prepared palladium single-atom catal...

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Abstract

The invention discloses a method for preparing a high-load precious metal monatomic catalyst by an in-situ photoreduction method, which comprises the following steps: treating aza-graphene, graphene oxide or three-dimensional network graphene oxide with a metal salt solution or a metal alkali solution to load sodium and potassium ions on the surface, washing with deionized water and absolute ethylalcohol to alkalescence, and carrying out ultrasonic dispersion; adding a noble metal salt solution and a carbonyl compound, mixing, and magnetically stirring; and finally, carrying out in-situ photoreduction under an illumination condition, and carrying out freeze drying to prepare noble metal single atoms. According to the invention, 40-60 ml of a sodium or potassium salt solution or alkali solution with the molar concentration of 1-15 mol / L is added into every 0.02-3.0 g of aza-graphene, graphene oxide or three-dimensional network graphene oxide carrier. The carbonyl compound is any one ofacetone, acetylacetone and acetophenone. The noble metal salt solution is chloride or acetylacetonate corresponding to noble metal elements. The high-load precious metal single atoms are obtained.

Description

technical field [0001] The invention belongs to the technical field of photocatalyst preparation, and relates to a method for preparing a high-load noble metal single-atom catalyst by an in-situ photoreduction method. Background technique [0002] In the field of catalysis, single-atom catalysts have shown superior performance over conventional catalysts. Different from traditional heterogeneous metal / semiconductor photocatalytic materials, single-atom photocatalysts can achieve the maximum utilization of metal atoms and greatly increase the active sites of photocatalysts; at the same time, the metal single atoms supported on the semiconductor surface have unique and different The saturated coordination environment exhibits excellent catalytic activity and enhances the intrinsic activity of each catalytic site. Since the single-atom catalyst was first reported in 2011, its unique characteristics of high activity and high atom utilization have set off a research storm in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42B01J23/46B01J23/52B01J23/58B01J27/24B01J31/22B01J35/00B01J37/16B01J37/34C01B3/04
CPCB01J37/344B01J37/16B01J23/52B01J27/24B01J23/462B01J23/468B01J23/42B01J23/58B01J31/2208C01B3/042B01J2531/18B01J2531/821B01J2531/827B01J2531/828B01J2531/824B01J35/391B01J35/39Y02E60/36
Inventor 曹宝月
Owner SHANGLUO UNIV