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a m 1 /m 2 x Preparation method of p-type single-atom catalyst

A catalyst, M12L2 technology, applied in catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve problems such as difficult to control metal dispersion, and achieve low utilization rate of metal atoms and controllable loading capacity , long service life effect

Active Publication Date: 2021-08-24
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] For the above-mentioned deficiencies that exist in the prior art, the purpose of the present invention is to provide a kind of M 1 / M 2 x The preparation method of P-type single-atom catalysts solves the problem that the existing methods are difficult to control the metal dispersion

Method used

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  • a m <sup>1</sup> /m <sup>2</sup> <sub>x</sub> Preparation method of p-type single-atom catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Under an inert atmosphere, M with an electron-deficient structure 1 Metal-organic complexes [Ag( i Pr-MeAMD)] 2 Dissolve in anhydrous organic toluene solvent to obtain a solution with a concentration of 15mg / L;

[0036] (2) With commercially available Fe 2 The P-type metal phosphide is a carrier, 1.0g of it is put into a bottle, under an inert atmosphere, first add anhydrous toluene solvent (40mL), and slowly add 4mL of the solution prepared in step (1) dropwise under stirring, After the dropwise addition, continue stirring under reflux at 110°C for 0.5h under an inert atmosphere, filter and wash with anhydrous toluene to obtain an intermediate product;

[0037] (3) Disperse the intermediate product obtained in step (2) in anhydrous toluene (40mL), then add 2mL of reducing agent methylaluminum, let it reflux and stir at 80°C for 0.5h, filter, and diethyl ether Wash the filter residue 3 times and dry to obtain the single-atom catalyst Ag / Fe 2 P;

[0038] The lo...

Embodiment 2

[0043] (1) Under an inert atmosphere, M with an electron-deficient structure 1 Metal-organic complexes [Cu( i Pr-MeAMD)] 2 Dissolve in anhydrous organic tetrahydrofuran solvent to obtain a solution with a concentration of 10mg / L;

[0044] (2) Commercially available Ni 2 P-type metal phosphide as a carrier, put 1.0g of it into a bottle, add anhydrous tetrahydrofuran solvent (50mL) under an inert atmosphere, slowly add 15mL of the solution prepared in step (1) dropwise under stirring, and add After completion, continue stirring at 50°C for 16 h under an inert atmosphere, filter and wash with anhydrous tetrahydrofuran to obtain an intermediate product;

[0045] (3) The obtained intermediate product is dispersed in anhydrous tetrahydrofuran (50mL), and then 2mL of reducing agent hydrazine (N 2 h 4 ), let it stir at 25°C for 10h, filter, wash the filter residue 3 times with n-hexane solvent, and dry it to obtain the single-atom catalyst Cu / Ni 2 P, measured its load as 10wt%. ...

Embodiment 3

[0050] (1) Under an inert atmosphere, M with a specific electron-deficient structure 1 Metal-organic complexes [Ni( t Bu-DAD) 2 ] was dissolved in anhydrous ether solvent to obtain a solution of 15mg / L concentration;

[0051] (2) With commercially available Fe 2 P-type metal phosphide as a carrier, put 1.0g of it into a bottle, add anhydrous toluene solvent (45mL) under an inert atmosphere, slowly add 6mL of the solution prepared in step (1) dropwise under stirring, dropwise After completion, continue to stir at 25°C for 24h under an inert atmosphere, filter and wash with anhydrous ether to obtain an intermediate product;

[0052] (3) Disperse the obtained intermediate product in anhydrous ether (45mL), add 3mL of reducing agent methylborane, let it stir at 60°C for 6h, filter, and wash the filter residue 3 times with n-hexane solvent , and dried to obtain the single-atom catalyst Ni / Fe 2 P single atom catalyst, the loading is 0.08wt%;

[0053] Use the catalyst prepared ...

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Abstract

The invention discloses a M 1 / M 2 x The preparation method of P-type single-atom catalyst comprises the following steps: (1) under inert atmosphere, will possess the M of electron-deficient structure 1 metal organic complex M 1 L 2 or M 1 2 L 2 Dissolve in the organic solvent A, obtain metal-organic complex solution; (2) M 2 x The P-type metal phosphide is added to the organic solvent B, and the metal-organic complex solution is added dropwise thereto under an inert atmosphere. After the dropwise addition, the reaction is carried out under an inert atmosphere; (3) after the reaction in step (2) is completed, Add a reducing agent to the system to carry out the reduction reaction, filter the mixed solution after the reduction reaction, and dry the filter residue after washing to obtain the M 1 / M 2 x P-type single-atom catalysts. The present invention adopts a brand-new coordination method to prepare single-atom catalysts, which can realize the loading of various metal single atoms on various phosphorus-containing substrates, and prepare different types of single-atom catalysts. Points and loads are controllable.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, in particular to a M 1 / M 2 x A method for preparing a P-type single-atom catalyst. [0002] technical background [0003] The development of more efficient catalysts has always been the focus of materials and chemistry. The most widely used in industry is the supported metal catalyst with high catalytic activity. The root of high catalytic activity lies in the size of the supported metal atom particles. For this reason, researchers continue to try smaller-sized particles. In recent years, studies have found that sub-nanometer clusters have higher catalytic activity than nano-clusters. The ideal state of a catalyst with a substrate-supported metal structure is that the metal atoms are independently distributed on the substrate one by one to achieve the highest degree of dispersion. This is a single-atom catalyst. [0004] Single-atom catalysts have both the active center of homogeneous cata...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/185B01J35/00B01J37/00B01J37/16
CPCB01J27/1853B01J35/0046B01J35/0066B01J37/0009B01J37/16
Inventor 丁玉强杜立永余绍山
Owner JIANGNAN UNIV