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A kind of preparation method of porous carbon supported tungsten carbide composite material

A composite material and tungsten carbide technology, applied in the field of material science, can solve the problems of low hydrogen evolution catalytic activity and poor stability, and achieve the effects of short process flow, prevention of agglomeration and growth, and good dispersion

Active Publication Date: 2021-07-09
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to improve the problems of low hydrogen evolution catalytic activity and poor stability of existing tungsten carbide catalysts, and design a composite carbon-based precursor for the synthesis of various metal oxides (tungsten oxide + other metal oxides) by solution combustion, and then Subsequent high-temperature carbonization reaction and washing in acidic solution to remove oxides to obtain porous carbon-supported tungsten carbide composite materials, thus developing a fast, simple, efficient and low-cost method for preparing new tungsten carbide catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 4.587g ammonium tungstate, 1.779g magnesium nitrate, 2.273g zinc nitrate, 1.968g calcium nitrate, 1.125g glycine and 1.72g glucose into a 500ml beaker, and add deionized water and stir to obtain a clear aqueous solution. The solution is heated on a resistance furnace, and a solution combustion synthesis reaction occurs, and a fluffy precursor can be obtained after the reaction. The precursor was placed in a tube furnace and fed with N 2 (The gas flow rate is 120mL / min) for high-temperature carbonization reaction, raising the temperature to 900°C at a rate of 6°C / min, and keeping it for 3 hours. After the reaction, a composite material of MgO / CaO / WC / C is obtained, and ZnO and carbon react and pyrolyze Pores are created on carbon substrates for the high-temperature evaporation of Zn simple substance. Immerse in the prepared 1.5M excess hydrochloric acid solution beaker, soak and let it stand for 30 hours, filter the supernatant, remove the lower layer of powder and...

Embodiment 2

[0030] Weigh 3.058g of ammonium metatungstate, 1.186g of magnesium nitrate, 1.515g of zinc nitrate, 1.312g of calcium nitrate, 0.65g of urea and 1.35g of glucose into a 300ml beaker, add deionized water and place it on a resistance furnace while heating slowly Stir to obtain a clear aqueous solution after stirring evenly, then put it into a muffle furnace and heat it at a constant temperature of 200°C for 1 hour to generate a solution combustion synthesis reaction. The powder is placed in a tube furnace under an Ar atmosphere (the gas flow rate is 150mL / min), and the heating rate is raised to 800°C at a rate of 7°C / min for carbonization for 4 hours to obtain a composite powder of MgO / CaO / WC / C, ZnO It reacts with carbon and pyrolyzes Zn elemental substance to evaporate at high temperature to create pores on the carbon substrate. After re-grinding, immerse in the prepared 1.0M excess hydrochloric acid solution beaker, soak and let it stand for 48 hours, filter the supernatant, t...

Embodiment 3

[0032]Weigh 3.058g of ammonium metatungstate, 2.373g of magnesium nitrate, 1.92g of citric acid and 3.923g of sucrose into a 300ml beaker, add deionized water to obtain a clear aqueous solution, put the solution on a resistance furnace for heating, and In the solution combustion synthesis reaction, the solution is heated from the beginning until the gel is covered with a rubber stopper, and a fluffy precursor can be obtained after the reaction. Put the precursor into a tube furnace and feed it with Ar (the flow rate of the gas is 100mL / min) to carry out high-temperature carbonization reaction, raise the temperature to 1100°C for 2 hours at a rate of 10°C / min, and then cool with the furnace to obtain MgO Composite material of / WC / C. Immerse in the prepared 0.5M excess hydrochloric acid solution beaker, soak and let it stand for 40 hours, filter the supernatant, remove the lower layer of powder, wash with deionized water in a high-speed centrifuge for 4 times, and dry in a dryin...

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PUM

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Abstract

The invention discloses a method for preparing a porous carbon-loaded tungsten carbide composite material, which belongs to the field of material science and technology. The material is highly dispersed and uniformly loaded tungsten carbide nanoparticles on a carbon skeleton with a large network of pore structures. The specific preparation method is: using metal nitrate, tungsten source, fuel and soluble organic carbon source as raw materials, the precursor of tungsten oxide and other metal oxides uniformly embedded in the carbon matrix is ​​obtained through the solution combustion synthesis reaction, and the synergistic coupling pore-forming effect is used. , after subsequent high-temperature carbonization and pickling to remove oxides, the specific surface area is as high as 1000m 2 / g or more porous carbon-supported tungsten carbide materials. The raw materials of the present invention are easy to obtain, the process is simple, and the requirements for equipment are low. The prepared porous carbon-supported tungsten carbide powder material has fine particles, narrow particle size distribution, good dispersibility, high specific surface area and pore volume, and uniform loading of tungsten carbide particles. It is not easy to fall off, and as a platinum-substituting catalyst, it can significantly reduce the cost of electrocatalysts, and at the same time improve its hydrogen evolution catalytic performance, and has good industrial application prospects.

Description

technical field [0001] The invention belongs to the technical field of material science, and in particular relates to designing a method for preparing a porous carbon-loaded tungsten carbide composite material with a high specific surface area. Background technique [0002] Energy shortage and environmental pollution are two major problems facing the development of human society since the 21st century. Therefore, it is imperative to find clean and renewable energy and develop efficient energy storage and conversion technologies. Hydrogen energy is regarded as the most ideal energy carrier due to its high calorific value, high energy density (143KJ / g) and abundant reserves. In recent years, electrolysis of water to produce H 2 (HER) is considered to be an ideal method to prepare clean hydrogen energy, which is of great significance to alleviate the energy crisis and reduce the emission of greenhouse gases. The core problem of this method is to develop efficient, stable and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/22B01J35/10B01J21/18B01J37/08B01J37/06B82Y30/00B82Y40/00C25B1/04C25B11/091
CPCB01J27/22B01J21/18B01J37/08B01J37/06C25B1/04C25B11/091B01J35/33B01J35/618B01J35/638Y02E60/36
Inventor 吴昊阳秦明礼王倩玉周士棋贾宝瑞曲选辉
Owner UNIV OF SCI & TECH BEIJING
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