Carbon resistance ultra-fine nano-tungsten carbide material and its preparation method and application

An ultra-fine nano, tungsten source technology, applied in chemical instruments and methods, carbides, nanotechnology, etc., can solve the problems of particle agglomeration and large particles, achieve uniform particle size distribution, improve catalyst performance, reduce step loss and The effect of energy consumption

Inactive Publication Date: 2016-08-17
ZHEJIANG UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the particles of the obtained WC material are still relatively large, and the reason is still the particle agglomeration of ultrafine nanoparticles during the high temperature process.

Method used

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  • Carbon resistance ultra-fine nano-tungsten carbide material and its preparation method and application
  • Carbon resistance ultra-fine nano-tungsten carbide material and its preparation method and application
  • Carbon resistance ultra-fine nano-tungsten carbide material and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0035] Add 0.08g of ammonium metatungstate to 50ml of distilled water and mix it with a solution made of 25ml of ethanol, 0.2ml of concentrated ammonia solution and 0.05g of sodium dodecylbenzenesulfonate. After stirring, add 0.5g of resorcinol and stir After 30 minutes, 0.5ml of formaldehyde was added, stirred at room temperature for 24 hours, then transferred to a hydrothermal reaction kettle and kept in a blast drying oven at 120°C for 15 hours, and the obtained compound was dried in a blast drying oven at 80°C. In the high-temperature tube furnace, the carbonization gas is 200ml / min of CO gas, raised from room temperature to 400°C at a rate of 5°C / min, kept at 400°C for 1 hour, and then heated to 900°C at the same heating rate for 6 hours. After cooling to room temperature, the obtained powder is the carbon resistance ultrafine nano WC material. It looks like figure 1 . WC components dispersed well, but partly showed agglomeration phenomenon. The particle size of highly...

Embodiment 2

[0037]Add 0.02g of ammonium metatungstate to 10ml of distilled water and mix it with a solution made of 5ml of ethanol, 0.05ml of concentrated ammonia solution and 0.005g of sodium dodecylbenzenesulfonate. After stirring, add 0.1g of resorcinol and stir After 30 minutes, 0.1ml of formaldehyde was added, stirred at room temperature for 8 hours, then transferred to a hydrothermal reaction kettle and kept in a blast oven at 80°C for 12 hours, and the obtained polymer was dried in a blast oven at 80°C. In the high-temperature tube furnace, the carbonization gas is 50ml / min of CO gas, raised from room temperature to 400°C at a rate of 1°C / min, kept at 400°C for 1 hour, and then heated to 900°C at the same heating rate for 2 hours. After cooling to room temperature, the obtained powder is the carbon resistance ultra-fine nano-WC material, but the output is less. The particle size of WC is about 2nm.

Embodiment 3

[0039] Add 0.02g of ammonium metatungstate to 20ml of distilled water and stir, then add to the solution made of 8ml of ethanol, 0.1ml of concentrated ammonia solution and 0.01g of sodium dodecylbenzenesulfonate, stir and add 0.25g of resorcinol and stir After 30 minutes, 0.35ml of formaldehyde was added, stirred at room temperature for 24 hours, then transferred to a hydrothermal reaction kettle and kept in a blast drying oven at 100°C for 12 hours, and the obtained polymer was dried in a blast drying oven at 80°C. In a high-temperature tube furnace, the temperature rises from room temperature to 400°C at a rate of 2.5°C / min, and the carbonization gas is 150ml / min of CO gas. After keeping at 400°C for 1 hour, it is heated to 900°C at the same heating rate for 4 hours. After cooling to room temperature, the obtained powder is the carbon resistance ultrafine nano WC material. It looks like figure 2 . The carbon component particle size reaches 250nm. The particle size of WC ...

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Abstract

A carbon resistance ultrafine nano WC material and its preparation method and application. The preparation method of the carbon resistance ultrafine nano WC material includes: (1) adding a deionized aqueous solution of a tungsten source to a mixture of ethanol, concentrated ammonia water and surface active In a solution made of a tungsten agent, the tungsten source is ammonium metatungstate, sodium tungstate or tungsten chloride, and the surfactant is sodium dodecylbenzenesulfonate, cetyltrimethylammonium bromide Or P123, add resorcinol after stirring evenly, add formaldehyde after stirring evenly, and then stir at room temperature for 8-28 hours to obtain a mixed solution; (2) perform a hydrothermal reaction on the mixed solution, and dry to obtain a mixed polymer; (3) mix The polymer is carbonized at a high temperature in a CO atmosphere to obtain a carbon-resistance ultrafine nano-WC material. The WC material can keep the WC particles stable in the high temperature process without secondary agglomeration. It can be used as an electrocatalyst in the electrocatalytic nitro reduction reaction, and can also be used as a carrier to prepare a platinum-loaded catalyst. The prepared platinum-loaded catalyst can be Applied in methanol fuel cell anode catalysis.

Description

(1) Technical field [0001] The invention relates to an ultrafine nanometer tungsten carbide material as well as its preparation method and application. (2) Background technology [0002] Catalysts play a very important role in the chemical industry, and researchers at home and abroad have done a lot of research on the development of new catalysts. In terms of increasing the activity of catalysts, the current research directions are mainly focused on increasing the specific surface area of ​​the active component or reducing the particle size of the active component. [0003] Tungsten carbide (Tungsten carbide, WC) is a non-precious metal material with excellent performance and has platinum-like catalytic activity. It has shown certain catalytic performance in the fields of chemical catalysis and electrocatalysis, such as fuel cells, catalytic hydrogenation Wait. It is worth noting that WC also has unique properties to be a good electrocatalyst, such as: better acid resistan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/34B01J27/22H01M4/92B82Y40/00C01B32/949
CPCC09C1/48C01B32/949H01M4/925Y02E60/50
Inventor 马淳安褚有群毛信表陈赵扬施梅勤
Owner ZHEJIANG UNIV OF TECH
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