Preparation method of M1/M2xP-type monoatomic 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, achieve controllable active sites and loading, and simple synthesis , the effect of long service life

Active Publication Date: 2019-04-02
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 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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  • Preparation method of M1/M2xP-type monoatomic catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) In an inert atmosphere, M 1 Metal organic complex [Ag( i Pr-MeAMD)] 2 Dissolve in anhydrous organic toluene solvent to obtain a solution with a concentration of 15 mg / L;

[0035] (2) Fe from the market 2 P-type metal phosphide is the carrier. Put 1.0g of it in the bottle. Under an inert atmosphere, first add anhydrous toluene solvent (40mL), and slowly drop 4mL of the solution prepared in step (1) into it under stirring. After the addition is complete, continue to reflux and stir under an inert atmosphere for 0.5 h at 110°C, filter and wash with anhydrous toluene to obtain an intermediate product;

[0036] (3) Disperse the intermediate product obtained in step (2) in anhydrous toluene (40 mL), and then add 2 mL of the reducing agent methyl aluminum, let it reflux and stir for 0.5 h at 80°C, filter, and use ether Wash the filter residue 3 times and dry it to obtain the single atom catalyst Ag / Fe 2 P;

[0037] The loading amount of the catalyst prepared in this embodiment i...

Embodiment 2

[0042] (1) In an inert atmosphere, M 1 Metal organic complex [Cu( i Pr-MeAMD)] 2 Dissolve in anhydrous organic tetrahydrofuran solvent to obtain a solution with a concentration of 10mg / L;

[0043] (2) Ni 2 P-type metal phosphide is the carrier. Put 1.0g of it in a bottle, add anhydrous tetrahydrofuran solvent (50mL) under an inert atmosphere, slowly add 15mL of the solution prepared in step (1) to it with stirring, dropwise After completion, stirring was continued at 50°C under an inert atmosphere for 16 hours, filtered and washed with anhydrous tetrahydrofuran to obtain an intermediate product;

[0044] (3) Disperse the obtained intermediate product in anhydrous tetrahydrofuran (50mL), then add 2mL of the reducing agent hydrazine (N 2 H 4 ), let it stir for 10h at 25℃, filter, wash the filter residue with n-hexane solvent 3 times, and dry it to obtain the monoatomic catalyst Cu / Ni 2 P, the load is measured to be 10wt%.

[0045] Using the catalyst prepared in this embodiment to degra...

Embodiment 3

[0049] (1) In an inert atmosphere, M with a specific electron-deficient structure 1 Metal organic complex [Ni( t Bu-DAD) 2 ] Dissolve in anhydrous ether solvent to obtain a solution with a concentration of 15mg / L;

[0050] (2) Fe obtained from the market 2 P-type metal phosphide is the carrier, put 1.0g of it into the bottle, add anhydrous toluene solvent (45mL) under an inert atmosphere, slowly add 6mL of the solution prepared in step (1) to it while stirring, dropwise After completion, continue to stir at 25°C under an inert atmosphere for 24 hours, filter and wash with anhydrous ether to obtain an intermediate product;

[0051] (3) Disperse the obtained intermediate product in anhydrous ether (45 mL), add 3 mL of the reducing agent methyl borane, let it stir at 60°C for 6 hours, filter, and wash the filter residue with n-hexane solvent 3 times , Drying to obtain a single atom catalyst Ni / Fe 2 P single-atom catalyst with a loading amount of 0.08wt%;

[0052] Use the catalyst prepa...

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Abstract

The invention discloses a preparation method of a M1/M2xP-type monoatomic catalyst. The preparation method includes: (1) in an inert gas atmosphere, dissolving an organic complex M1L2 or M12L2, havingan electron deficiency structure, of a M1 metal in an organic solvent A to prepare a metal/organic complex solution; (2) adding a M2xP-type metal phosphide to an organic solvent B, and in an inert gas atmosphere, dropwise adding the metal organic complex solution, then performing a reaction in the inert gas atmosphere; (3) after the reaction in the step (2) is completed, adding a reducing agent to the system to perform a reduction reaction, and filtering a mixed liquid after the reduction reaction, and washing and drying filter residues to obtain the M1/M2xP-type monoatomic catalyst. The monoatomic catalyst is prepared through a novel coordination technology, so that various metal mono-atoms can be supported on various phosphorus-containing substrates, thus producing monoatomic catalystsin different types. The monoatomic catalysts are controllable in dispersity, active sites and support quantity.

Description

Technical field [0001] The invention belongs to the field of catalyst preparation, and specifically relates to a M 1 / M 2 x Preparation method of P-type single atom catalyst. technical background [0002] The research and development of more efficient catalysts has always been the focus of materials and chemistry. The most widely used in industry is the supported metal catalysts with high catalytic activity. Among them, the high catalytic activity is based on the size of the supported metal atom particles. For this reason, researchers continue to try smaller size particles. In recent years, research has found that sub-nano clusters have higher catalytic activity than nano-clusters. The ideal state of the substrate supported metal structure catalyst 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. [0003] Single-atom catalysts have both the active centers of homogeneous ca...

Claims

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Application Information

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Patent Type & Authority Applications(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
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