Method for preparing double mesoporous high (100) crystal plane tungsten carbide material

A tungsten carbide material and double mesoporous technology, applied in the direction of carbide, tungsten/molybdenum carbide, etc., can solve the problems of increasing equipment cost, energy consumption, and low surface utilization, so as to enhance electrocatalytic performance and avoid hard agglomeration , The effect of pore structure maintenance

Active Publication Date: 2014-05-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In more detail, controlling the porosity and pore size distribution of the catalyst is the main factor affecting the basic properties of the catalyst, including the specific surface area and gas-liquid phase diffusion. The inability to enter the pores leads to a very low actual surface utilization rate. WC materials with two types of pore distribution are considered to be a more practical catalytic material. If a simpler method can be used without increasing equipment costs and excessive energy consumption, Obtaining biporous or even porous WC with two types of mesoporous pore distribution is a research direction with practical application value and potential expansion prospects.

Method used

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  • Method for preparing double mesoporous high (100) crystal plane tungsten carbide material
  • Method for preparing double mesoporous high (100) crystal plane tungsten carbide material
  • Method for preparing double mesoporous high (100) crystal plane tungsten carbide material

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Embodiment 1

[0036] Configure solutions A and B. Solution A is ammonium metatungstate and copper sulfate plus deionized water (W:Cu mass ratio 1:0.5). The concentration of solution A is 20wt%, and solution B is 10wt% ammonium carbonate solution. While shaking solution A, add solution B dropwise at a rate of 50 μL / min. After the dropwise addition, the particles were filtered to obtain precursor particles (composite crystals); after vacuum drying at 100°C, the obtained precursor particles were 2Atmosphere (CO:H 2 The volume ratio is 1:2), and the carbonization treatment is carried out, and the temperature is raised to 800°C according to the 5°C / min program and kept for 6 hours to obtain a double-porous WC-metal material. Then, the double-porous WC-metal material was treated with 20% hydrochloric acid to obtain the expanded double-porous WC material. The shape of the particles can be seen in figure 1 , to further enlarge the topography as shown in figure 2 . The pore size distribution i...

Embodiment 2

[0038] Configure solutions A and B. Solution A is ammonium metatungstate and copper sulfate plus deionized water (W:Cu mass ratio 1:0.1). The concentration of solution A is 5wt%, and solution B is 50wt% ammonium carbonate solution. While shaking solution A, add solution B dropwise at a rate of 200 μL / min. After the dropwise addition, the particles were filtered to obtain precursor particles (composite crystals); after vacuum drying at 60°C, the resulting precursor particles were 2 Atmosphere (CO:H 2 The volume ratio is 1:1.5), and the carbonization treatment is carried out, and the temperature is raised to 800°C according to the 2°C / min program and kept for 6 hours to obtain a double-porous WC-metal material. Then, the double-porous WC-metal material was treated with 20% hydrochloric acid to obtain the expanded double-porous WC material. The pore size of the sample is double-pore distribution, the small pore size is around 2.8nm, and the second mesopore is around 3-10nm. It...

Embodiment 3

[0040] Configure solutions A and B, A solution is ammonium metatungstate and copper sulfate plus deionized water (W:Cu mass ratio 1:0.2), A solution concentration is 20wt%, B solution is 5wt% ammonium carbonate solution, in While ultrasonically oscillating solution A, add solution B dropwise at a rate of 100 μL / min. After the dropwise addition, the particles were filtered to obtain precursor particles (composite crystals); after vacuum drying at 80°C, the obtained precursor particles were 2 Atmosphere (CO:H 2 The volume ratio is 1:2), and the carbonization treatment is carried out, and the temperature is raised to 750°C according to the 3°C / min program and kept for 8 hours to obtain a double-porous WC-metal material. Then, the double-porous WC-metal material was treated with 20% hydrochloric acid to obtain the expanded double-porous WC material. The pore size of the sample is double-pore distribution, the small pore size is around 5nm, and the second mesopore is around 5-30n...

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Abstract

The invention discloses a method for preparing a double mesoporous high (100) crystal plane tungsten carbide material. The method comprises the following steps of: (1) preparing a mixed aqueous solution of ammonium meta-tungstate and copper sulfate, adding a 5 to 50 mass percent ammonium carbonate aqueous solution dropwise at the speed of 50 to 200mu L / min during ultrasonic oscillation to deposit solid particles, and filtering after a dropwise adding process to obtain precursor particles; (2) drying the precursor particles in vacuum at the temperature of between 60 and 100 DEG C, putting the precursor particles into a tube furnace and carbonizing to obtain a mesoporous tungsten carbide composite material; and (3) performing acid treatment on the mesoporous tungsten carbide composite material, and thus obtaining the double mesoporous tungsten carbide material. Double mesoporous tungsten carbide (WC) which is prepared by the method is formed by piling up nano WC particles, and the growth of a WC (100) crystal plane is promoted, so that the sorption / desorption capacity of the WC to hydrogen (H2) and the electro-catalysis property of the WC are improved.

Description

(1) Technical field [0001] The invention relates to a preparation method of a porous tungsten carbide material, in particular to a preparation method of a high (100) crystal plane tungsten carbide material composed of two mesoporous pore structures. (2) Background technology [0002] Tungsten carbide (WC) has a very wide range of applications in the field of cemented carbide, because its surface electron layer is similar to platinum (Pt), it has Pt-like catalytic activity in certain reactions, and has excellent performance as a Since the 1960s, WC has been reported to have good catalytic activity for the dehydrogenation of cyclohexane and the dehydrogenation of ethylbenzene to styrene. WC not only has the characteristics of replacing precious metal catalysts such as platinum, but also has strong acid resistance and good thermal and chemical stability, which makes it have the potential to become a high-performance catalyst from its own attributes. [0003] It is well known t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/34C01B32/949
Inventor 马淳安陈赵扬褚有群祝爱娟
Owner ZHEJIANG UNIV OF TECH
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