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Preparation method of nitrogen-doped spherical graphene loaded flaky molybdenum disulfide catalyst

A molybdenum disulfide, nitrogen doping technology, used in electrodes, electrolysis processes, electrolysis components, etc.

Active Publication Date: 2021-05-11
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, during application, graphene's carbon sheets are easily bonded back together, losing many of its advantages

Method used

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  • Preparation method of nitrogen-doped spherical graphene loaded flaky molybdenum disulfide catalyst
  • Preparation method of nitrogen-doped spherical graphene loaded flaky molybdenum disulfide catalyst
  • Preparation method of nitrogen-doped spherical graphene loaded flaky molybdenum disulfide catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The preparation method of the nitrogen-doped spherical graphene-supported flake molybdenum disulfide catalyst described in the present invention realizes the regulation and control of flake molybdenum disulfide loaded in the spherical graphene by changing the nitrogen-doped structure in the spherical graphene, In order to control the catalytic activity of the nitrogen-doped spherical graphene-supported sheet-like molybdenum disulfide catalyst in the electrocatalytic hydrogen evolution reaction, the specific steps are as follows:

[0046] (1) Preparation of positively charged polystyrene microspheres

[0047] Mixture 1 was obtained by dissolving 10.0 g of styrene and 1.5 g of polyvinylpyrrolidone in 100.0 ml of deionized water in a 500 ml three-necked flask. The mixture was stirred mechanically at room temperature for 30 minutes under nitrogen protection. Then 0.26 g of 2,2'-azobisisobutylamidine dihydrochloride was dissolved in 20.0 ml of deionized water and added to m...

Embodiment 2

[0054] (1) This step is the same as step (1) in Example 1.

[0055] (2) This step is the same as step (2) in Example 1.

[0056] (3) This step is the same as step (3) in Example 1, and the solid sample is 2 The temperature of calcination in the atmosphere is adjusted to 3°C / min at 420°C -1 Calcined at a heating rate of 2 hours at 5°C / min -1 The heating rate was increased to 750 °C and then calcined for 1 hour to obtain nitrogen-doped spherical graphene mainly composed of pyridinic nitrogen, which was labeled as nitrogen-doped spherical graphene 2. The specific surface area, nitrogen-doped structure and nitrogen-doped content of nitrogen-doped spherical graphene 2 are listed in Table 1 and Table 2, respectively.

[0057] (4) This step is the same as step (4) in embodiment 1, obtains nitrogen-doped spherical graphene supported flake molybdenum disulfide catalyst 2. The polarization curve of nitrogen-doped spherical graphene-supported sheet-like molybdenum disulfide catalyst ...

Embodiment 3

[0059] (1) This step is the same as step (1) in Example 1.

[0060] (2) This step is the same as step (2) in Example 1.

[0061] (3) This step is the same as step (3) in Example 1, and the solid sample is 2 The temperature of calcination in the atmosphere is adjusted to 3°C / min at 420°C -1 Calcined at a heating rate of 2 hours at 5°C / min -1 The heating rate was increased to 1000°C and then calcined for 1 hour to obtain nitrogen-doped spherical graphene mainly composed of graphitic nitrogen, which was labeled as nitrogen-doped spherical graphene 3. The specific surface area, nitrogen-doped structure and nitrogen-doped content of nitrogen-doped spherical graphene 3 are listed in Table 1 and Table 2, respectively.

[0062] (4) This step is the same as step (4) in Example 1, and obtains nitrogen-doped spherical graphene supported flake molybdenum disulfide catalyst 3. The electrocatalytic hydrogen evolution polarization curve of nitrogen-doped spherical graphene-supported shee...

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Abstract

The invention discloses a preparation method of a nitrogen-doped spherical graphene loaded flaky molybdenum disulfide catalyst, which comprises the following specific steps: (1) adding an initiator into styrene and polyvinylpyrrolidone to prepare polyethylene microspheres with positive charges; (2) preparing a graphene oxide aqueous solution from graphite powder, sodium nitrate and 95% concentrated sulfuric acid; (3) adding the graphene oxide aqueous solution and a nitrogen-doped precursor into the polyethylene microspheres with positive charges, conducting reacting while stirring, filtering the reacted mixture, conducting drying to obtain a solid sample, and calcining the solid sample in a nitrogen atmosphere to prepare nitrogen-doped spherical graphene; and (4) adding the spherical graphene with the nitrogen-doped structure and ammonium tetrathiomolybdate into a reaction solvent for reaction, then conducting filtering and washing by using a washing solution, and conducting drying to obtain the nitrogen-doped spherical graphene loaded flaky molybdenum disulfide catalyst.

Description

technical field [0001] The invention relates to an electrocatalytic hydrogen evolution reaction catalyst, in particular to a method for preparing a nitrogen-doped spherical graphene-supported flake molybdenum disulfide catalyst Background technique [0002] Hydrogen is considered an ideal energy carrier for clean and sustainable energy technologies. Electrochemical hydrogen evolution technology is a promising hydrogen production technology. Currently, platinum (Pt) and Pt-group materials are considered to be the most effective catalysts, but their high cost and scarcity limit their wide application. Molybdenum disulfide, a transition metal dichloride product with a two-dimensional layered structure, has been extensively studied in recent years. It is found that bulk 2D layered MoS2 mainly consists of thermodynamically favorable basal plane sites, but the basal planes are catalytically inert. Compared with the catalytically inert basal surface, the edge of the MoS2 sheet h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/04C25B11/091
CPCC25B1/04Y02E60/36
Inventor 田小宁蒋仲庆
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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