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Preparation of highly dispersed molybdenum carbide/carbon composite electro-catalyst by adopting oxidation, reduction and fixation method

A technology of electrocatalyst and immobilization method, which is applied in the field of electrocatalysis, can solve problems such as harsh conditions and complicated preparation, and achieve the effects of simple process, convenient preparation and good stability

Active Publication Date: 2017-05-24
江苏先进无机材料研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But usually these methods are complicated to prepare and the conditions are harsh

Method used

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  • Preparation of highly dispersed molybdenum carbide/carbon composite electro-catalyst by adopting oxidation, reduction and fixation method
  • Preparation of highly dispersed molybdenum carbide/carbon composite electro-catalyst by adopting oxidation, reduction and fixation method
  • Preparation of highly dispersed molybdenum carbide/carbon composite electro-catalyst by adopting oxidation, reduction and fixation method

Examples

Experimental program
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Effect test

Embodiment 1

[0036] Choose citric acid as reducing carbon source, take by weighing citric acid 2.5g, and ammonium heptamolybdate ((NH 4 ) 6 Mo 7 o 24 .4H 2 O) 0.5g in a beaker, add 50mL of water to ultrasonically dissolve, then transfer to a hydrothermal kettle, heat at 180°C for 8h, after cooling, wash the black product with water, centrifuge, and dry. The dried product was subjected to H 2 / Ar atmosphere calcined to 800°C, the heating rate is 5°C / min, and kept for 5h, the molybdenum carbide / carbon composite catalyst can be obtained, denoted as MoC x -1.

[0037] The electrochemical test of the prepared highly dispersed molybdenum carbide / carbon composite catalyst for electrolysis of water to produce hydrogen is carried out in the following steps:

[0038] First, weigh 4mg of the above catalyst and disperse it in a mixed solution containing 1mL of absolute ethanol and 40uL Nafion solution (5%), ultrasonically obtain a uniformly dispersed suspension, then take 30uL of the above suspe...

Embodiment 2

[0040] Preparation process and steps in embodiment 2 are basically the same as above-mentioned embodiment 1, and difference is: the molybdenum source ammonium heptamolybdate ((NH 4 ) 6 Mo 7 o 24 .4H 2 O) quality is 2.5g, and the catalyst made is denoted as MoC x -2. The catalytic performance of the catalyst for hydrogen production by electrolysis of water is the same as in Example 1.

Embodiment 3

[0042] Preparation process and steps in embodiment 3 are basically the same as above-mentioned embodiment 1, and difference is: the molybdenum source ammonium heptamolybdate ((NH 4 ) 6 Mo 7 o 24 .4H 2 O) quality is 4g, and the catalyst made is denoted as MoC x -3. The catalytic performance of the catalyst for hydrogen production by electrolysis of water is the same as in Example 1.

[0043] figure 1 a is the XRD pattern of the sample after hydrothermal treatment and drying, figure 1 b is the XRD pattern after calcination under protective atmosphere. From figure 1 As can be seen in a, the sample after hydrothermal treatment is MoO 2 / C composites, indicating that after hydrothermal treatment, the molybdenum source was converted to MoO by redox reaction 2 The form is fixed and dispersed on the carbon material. From figure 1 It can be seen from b that after calcination in a protective atmosphere, both β-Mo 2 The phase of C and the phase of η-MoC are mixed phases of t...

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Abstract

The invention relates to a preparation method of a highly dispersed molybdenum carbide / carbon composite electro-catalyst by adopting an oxidation, reduction and fixation method. The preparation method comprises the following steps that 1, reducing organic matter and ammonium heptamolybdate are dissolved in water to prepare a mixed solution, wherein the mass ratio of the reducing organic matter to the ammonium heptamolybdate is 1: (0.1-2); 2, the mixed solution is subjected to hydrothermal treatment at the temperature of 120-200 DEG C for 4-24 hours, solid is separated out, and washing and drying are performed; 3, the dried solid is calcined in a protective atmosphere at the temperature of 600-1000 DEG C for 2-10 hours to obtain the highly dispersed molybdenum carbide / carbon composite electro-catalyst. The used raw materials are safe, non-toxic, simple to obtain and convenient to prepare and can be synthesized into molybdenum carbide nanomaterials in a large-scale mode.

Description

technical field [0001] The invention relates to a highly dispersed molybdenum carbide / carbon composite electrocatalyst prepared by a redox fixation method, which belongs to the technical field of electrocatalysis. Background technique [0002] Hydrogen production by electrolysis of water is an ideal hydrogen production method with high efficiency and environmental protection. The most ideal platinum-based catalyst currently used is due to its high price and limited resources, which limit its industrial application. Therefore, finding and discovering efficient and inexpensive non-precious metal electrocatalysts is the key to hydrogen production from water electrolysis. At present, some early transition metals, such as Fe, Co, Ni, Mo, W, etc., their metal alloys and carbides, nitrides, sulfides, phosphides, etc., are widely used to study hydrogen production by electrolysis of water. catalyst. Among them, β-Mo 2 C is one of the best non-precious metal electrocatalysts that ...

Claims

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Application Information

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IPC IPC(8): B01J27/22C25B1/04C25B11/06
CPCB01J27/22C25B1/04C25B11/051C25B11/057C25B11/077Y02E60/36
Inventor 周亚君张玲霞施剑林
Owner 江苏先进无机材料研究院
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