Preparation method of molybdenum disulfide with nanopore structure

A nanoporous structure, molybdenum disulfide technology, applied in molybdenum sulfide, electrodes, electrolysis process, etc., can solve the problems of poor conductivity, few catalyst active sites, low catalytic efficiency, etc., and achieve strong conductivity, good catalytic performance and Stability, effect of high active site density

Active Publication Date: 2021-07-30
GUIZHOU MINZU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for preparing molybdenum disulfide with a nanoporous structure, so as to solve the problem of low catalytic efficiency due to the lack of active sites and poor conductivity of the catalyst in the current electrolytic hydrogen production process using molybdenum disulfide as a catalyst. And the problem of poor stability

Method used

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  • Preparation method of molybdenum disulfide with nanopore structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A preparation method of block molybdenum disulfide catalyst with nanopore structure, specifically as follows:

[0020] 1) Weigh commercial high-purity molybdenum disulfide powder and nano-silica powder (particle size 10-100 nanometers), and mix the two according to the mass ratio of 1:2.

[0021] 2) Weigh the mixed powder, put it into a ball mill jar together with balls and milling aids, and after vacuuming, pass in argon protection, and carry out wet milling in a high-energy ball mill for 12 to 48 hours.

[0022] 3) After ball milling, use a sieve to separate the slurry and balls, then transfer the slurry to a vacuum drying oven, and dry it in vacuum at 40-60°C for 2-8 hours.

[0023] 4) Use an agate mortar to grind the dried powder for 1-5 minutes.

[0024] 5) Weigh 1.0-3.0 g of the mixed powder, press it into a cylinder under the condition of 1 MPa in a powder tablet press, and wrap it with an inert metal sheet or polytetrafluoroethylene.

[0025] 6) Grinding the s...

Embodiment 2

[0037] A preparation method of block molybdenum disulfide catalyst with nanopore structure, specifically as follows:

[0038] 1) Weigh commercial high-purity molybdenum disulfide powder and nano-silica powder (particle size 10-100 nanometers), and mix the two according to the mass ratio of 1:4.

[0039] 2) Weigh the mixed powder, put it into a ball mill jar together with balls and milling aids, and after vacuuming, pass in argon protection, and carry out wet milling in a high-energy ball mill for 12 to 48 hours.

[0040] 3) After ball milling, use a sieve to separate the slurry and balls, then transfer the slurry to a vacuum drying oven, and dry it in vacuum at 40-60°C for 2-8 hours.

[0041] 4) Use an agate mortar to grind the dried powder for 1-5 minutes.

[0042] 5) Weigh 1.0-3.0 g of the mixed powder, press it into a cylinder under the condition of 1 MPa in a powder tablet press, and wrap it with an inert metal sheet or polytetrafluoroethylene.

[0043] 6) Grinding the s...

Embodiment 3

[0055] The molybdenum disulfide sheet with nanoporous structure prepared in Examples 1 and 2 was adhered to the top of a glassy carbon rod as a working electrode, the silver / silver chloride electrode was used as a reference electrode, and the stone-milled rod was used as a counter electrode for electrochemical testing.

[0056] Such as figure 1 As shown, the experimental results show that the prepared molybdenum disulfide has a lower hydrogen evolution overpotential (the exchange current density is 10mA / cm 2 The overpotential was 162mV), and the small Tafel slope (41mV), showing that it has good catalytic performance, and the material still maintains the overpotential and Tafel slope similar to the initial value after 2000 cycles of linear voltammetry scanning , indicating that it has good stability.

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Abstract

The invention discloses a preparation method of molybdenum disulfide with a nano-pore structure. The method comprises the following steps: grinding molybdenum disulfide and nano silicon dioxide mixed powder, pressing into a cylinder, wrapping with an inert metal sheet or polytetrafluoroethylene, grinding sodium chloride into powder, drying to prepare a sodium chloride cylinder containing the mixed powder cylinder, corroding the sodium chloride cylinder slice in a hydrofluoric acid solution, and performing cleaning and drying to obtain the molybdenum disulfide catalyst with the nano-pore structure. The molybdenum disulfide prepared by the method disclosed by the invention has the advantages of high active site density, strong conductivity, good catalytic performance and good stability.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a preparation method of molybdenum disulfide with a nanoporous structure. Background technique [0002] Electrocatalytic water splitting for hydrogen production is a closed-loop production process. The starting material and by-products are both water and the process is clean and pollution-free. It is a promising strategy for hydrogen production. One of the bottlenecks currently restricting its development is the expensive Pt-based noble metal catalysts. In order to promote the popularization of electrocatalytic water splitting for hydrogen production, it is urgent to develop low-cost non-precious metal catalysts. Among many alternative non-precious metal catalytic materials, nano-layered molybdenum disulfide has attracted widespread attention due to its predictable catalytic effect and low price. However, the layered structure 2H phase MoS which is easy...

Claims

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Application Information

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IPC IPC(8): C01G39/06C25B11/075C25B1/04
CPCC01G39/06C25B1/04C01P2006/16Y02E60/36
Inventor 崔灿谢雅典胡海良张建辉牛姣姣
Owner GUIZHOU MINZU UNIV
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