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Phosphorus-doped carbon-loaded molybdenum-tungsten carbide catalyst, preparation and application thereof

A catalyst, phosphorus doping technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of limiting the electrochemical hydrogen evolution activity and stability of carbides, the difficulty of uniform dispersion of active sites, Particle size is not easy to control, etc., to achieve the effect of enriching lattice defect sites, enriching adjustable denaturation, and regular morphology

Pending Publication Date: 2020-06-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, conventional carbides need to be calcined under high temperature conditions, the preparation method is harsh, the particle size is not easy to control, and the active sites are not easy to disperse uniformly, which seriously limits the improvement of the electrochemical hydrogen evolution activity and stability of carbides.

Method used

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  • Phosphorus-doped carbon-loaded molybdenum-tungsten carbide catalyst, preparation and application thereof
  • Phosphorus-doped carbon-loaded molybdenum-tungsten carbide catalyst, preparation and application thereof
  • Phosphorus-doped carbon-loaded molybdenum-tungsten carbide catalyst, preparation and application thereof

Examples

Experimental program
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Effect test

Embodiment 01-12

[0029] Preparation method of phosphorus-doped carbon-supported molybdenum-tungsten carbide catalyst using MoWCu-MOF as precursor

[0030] 1) Mix a certain amount of heteropoly acid, 0.2g copper acetate, 0.08g L-glutamic acid, and 0.12g trimesic acid, and stir to obtain MoWCu-MOF.

[0031] 2) Heat the MOF precursor obtained in 1) in a tube furnace at 2°C min -1 The heating rate was raised to 800°C, calcined for 6 hours under nitrogen atmosphere, and the temperature was naturally lowered.

[0032] 3) Disperse the catalyst obtained in 2) in 0.5M H 2 SO 4 , stirred at 50°C for 2 h to obtain the catalyst. The dosage of heteropoly acid is shown in Table 1.

[0033] 4) Electrochemical test: Take 4 mg of the catalyst prepared in step 3) and add it to 485 μl of alcohol, 500 μl of water and 15 μl of 0.05wt% Nafion mixed solution, ultrasonically disperse evenly, take 10 μl and drop it on the glassy carbon rotating disc electrode, Dry at room temperature. The catalyst loading was 0....

Embodiment 13-24

[0038] Preparation method of phosphorus-doped carbon-supported molybdenum-tungsten carbide catalyst using MoWCu-MOF as precursor

[0039] 1) Mix 0.4g phosphomolybdic acid, 0.2g phosphotungstic acid, 0.2g copper acetate, 0.08g L-glutamic acid, and 0.12g trimesic acid, and stir to obtain MoWCu-MOF.

[0040] 2) Heat the MOF precursor obtained in 1) in a tube furnace at 2°C min -1 The heating rate is raised to a certain temperature, calcined for a period of time under a nitrogen atmosphere, and the temperature is naturally lowered.

[0041] 3) Disperse the catalyst obtained in 2) in 0.5M H 2 SO 4 , stirred at 50°C for 2 h to obtain the catalyst.

[0042] 4) The electrochemical test method is the same as that of Example 01-12. Such as Figure 4 It was shown that the onset potential of catalyst 18 was -0.08 V and the overpotential was 0.18 V, which was close to that of commercial 20% Pt / C.

[0043] Adopt X-ray diffraction analysis instrument to characterize above-mentioned 14 ...

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Abstract

The invention relates to a preparation method of a phosphorus-doped carbon-loaded molybdenum-tungsten carbide electrochemical hydrogen evolution catalyst, and belongs to the technical field of electrocatalytic materials. According to the invention, MoWCu multi-element metal-based MOF is used as a precursor, and then high-temperature heat treatment is carried out to obtain the catalyst; through nano confinement carbonization of an organic ligand and in-situ conversion of metal center ions, a component-controllable multi-element metal carbide / phosphorus-doped carbon nano composite structure is synthesized, so that an efficient electrochemical hydrogen evolution catalyst is created; the preparation method is simple in process, agglomeration of molybdenum-tungsten carbide nanoparticles is limited to a great extent, repeatability is good, and mass production is easy; and the catalyst shows good performance in an electro-catalytic hydrogen evolution reaction (HER) under an alkaline condition, and has a certain application prospect.

Description

technical field [0001] The invention belongs to the field of catalyst preparation and electrochemical technology, and relates to a method for preparing an electrocatalyst for electrochemical hydrogen evolution reaction, in particular to a method for preparing a phosphorus-doped carbon-supported molybdenum-tungsten carbide hydrogen evolution catalyst. Background technique [0002] With the increasing demand for hydrogen energy in aerospace, navigation and other national defense technology fields, the development of hydrogen energy has extremely important industrial value and social significance. At present, the main sources of hydrogen are electrolysis of water to produce hydrogen, coal, petroleum, natural gas and other fossil fuels to produce hydrogen, biomass thermochemical and microbial hydrogen production, and solar photocatalytic hydrogen production. Among them, electrolysis of water for hydrogen production is considered to be one of the most effective hydrogen evolution...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/22B01J35/00B01J37/08C25B1/04C25B11/06
CPCB01J27/22B01J37/086C25B1/04C25B11/073B01J35/33Y02E60/36
Inventor 王爱琴钮珊珊张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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