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Silicon carbide block with macroporous and mesoporous composite structure, and preparation method thereof

A technology of composite structure and silicon carbide block, which is applied in the direction of home appliances, ceramic products, and other home appliances, can solve the problems of affecting catalytic efficiency, large diffusion resistance, and reduced specific surface area, so as to avoid the reduction of specific surface area and improve catalytic efficiency , good pore connectivity

Active Publication Date: 2014-04-23
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the above methods can effectively increase the specific surface area of ​​silicon carbide, the following problems still exist: (1) The products directly prepared by the above methods are all silicon carbide powders, which need to be pressed into silicon carbide blocks before actual use However, in the process of pressing and forming, the specific surface area will be reduced, the diffusion resistance will be increased, and the pores will be blocked; (2) the products obtained by the above methods only have a single mesopore, and the connectivity is relatively poor. In the process of high-speed fluid It will produce a large diffusion resistance and affect the catalytic efficiency

Method used

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  • Silicon carbide block with macroporous and mesoporous composite structure, and preparation method thereof
  • Silicon carbide block with macroporous and mesoporous composite structure, and preparation method thereof
  • Silicon carbide block with macroporous and mesoporous composite structure, and preparation method thereof

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preparation example Construction

[0026] The invention provides a method for preparing a silicon carbide block with a macropore and mesoporous composite structure, comprising the following steps:

[0027] (1) Under ice-bath conditions, fully dissolve polyethylene glycol (PEG) with a molecular weight of 10,000 in a nitric acid solution with a concentration of 10wt%, then add tetraethyl orthosilicate, and stir until the solution is clear to obtain the substance The molar ratio of the composition is a mixed solution of ethylene oxide (EO): ethyl orthosilicate: nitric acid = x: 1: 0.25, wherein ethylene oxide is a monomer of polyethylene glycol, by changing the epoxy The ratio of ethane in the mixed solution (0.45≤x≤0.55) can adjust the macropore diameter in the final silicon carbide block to meet different application requirements;

[0028] (2) Inject the mixed solution obtained in step (1) into a mold (polytetrafluoroethylene tube or 96-well plate) and seal it, and let it stand at 35-40°C for 24-72 hours to make...

Embodiment 1

[0035] (1) Under ice-bath conditions, fully dissolve polyethylene glycol with a molecular weight of 10,000 in a nitric acid solution with a concentration of 10wt%, then add tetraethyl orthosilicate, and stir until the solution is clear to obtain the molar composition of the substance The ratio is a mixed solution of ethylene oxide: ethyl orthosilicate: nitric acid = 0.45:1:0.25.

[0036] (2) Pour the mixed solution obtained in step (1) into a polytetrafluoroethylene tube and seal it, let it stand at 38°C for 48 hours, and obtain a silicon oxide block after demoulding and cleaning;

[0037] (3) Hydrothermally treat the silicon oxide block obtained in step (2) with 0.1mol / L ammonia water at 80°C for 24 hours, then wash and dry, and roast at 700°C for 2 hours to remove organic matter, and obtain a white silicon oxide template;

[0038] (4) Immerse the silicon oxide template obtained in step (3) into a toluene solution of polycarbosilane with a concentration of 10wt%, so that the ...

Embodiment 2

[0042](1) Under ice-bath conditions, fully dissolve polyethylene glycol with a molecular weight of 10,000 in a nitric acid solution with a concentration of 10wt%, then add tetraethyl orthosilicate, and stir until the solution is clear to obtain the molar composition of the substance The ratio is a mixed solution of ethylene oxide: ethyl orthosilicate: nitric acid = 0.50:1:0.25.

[0043] (2) Pour the mixed solution obtained in step (1) into a polytetrafluoroethylene tube and seal it, let it stand at 35°C for 72 hours, and obtain a silicon oxide block after demoulding and cleaning;

[0044] (3) Hydrothermally treat the silicon oxide block obtained in step (2) with 0.1mol / L ammonia water at 90°C for 18 hours, then wash and dry, and roast at 700°C for 2 hours to remove organic matter, and obtain a white silicon oxide template;

[0045] (4) Immerse the silicon oxide template obtained in step (3) into a toluene solution of polycarbosilane with a concentration of 10wt%, so that the p...

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Abstract

The invention provides a preparation method of a silicon carbide block with a macroporous and mesoporous composite structure. The preparation method comprises the following steps: preparing the mixed solution of ethylene oxide, tetraethoxysilane and nitric acid in the mol ratio of x: 1: 0.25, wherein x is greater than or equal to 0.45 and less than or equal to 0.55; pouring the mixed solution into a die and sealing, demolding after standing, carrying out hydro-thermal treatment by using ammonium hydroxide to obtain a silicon oxide template, soaking the silicon oxide template into the methylbenzene solution of polycarbosilane, heating until the methylbenzene completely volatilizes, carrying out pyrolysis treatment under the protection of an insert gas to obtain a silicon carbide and silicon oxide composite block, and then carrying out soaking treatment by using hydrofluoric acid to obtain the silicon carbide block. The method provided by the invention is capable of directly obtaining the silicon carbide block with the macroporous and mesoporous composite structure, and avoids the problems of specific surface area reduction, diffusion resistance increase and pore blockage due to subsequent processing; besides, the silicon carbide block is adjustable in macroporous pore diameter and good in pore connectivity; as a result, the mass transfer resistance is greatly reduced and the catalytic efficiency is improved; and moreover, the preparation method is simple in preparation and convenient to operate.

Description

technical field [0001] The invention belongs to the technical field of catalyst carrier materials, and in particular relates to a silicon carbide block with a macropore and mesoporous composite structure and a preparation method thereof. Background technique [0002] Silicon carbide materials have high high temperature chemical stability, high temperature mechanical strength, high temperature thermal stability, thermal conductivity and low thermal expansion rate, and are ideal catalyst supports for high temperature and highly erosive catalytic processes. However, the specific surface area of ​​traditional silicon carbide materials is low, and the specific surface area of ​​the highest such as β-silicon carbide is only 20-30m 2 / g, can not meet the requirements of industrial catalytic engineering. [0003] At present, there are two main methods of increasing the specific surface area of ​​silicon carbide: (1) using nanostructured carbon and (1) reacting silicon dioxide at hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/565C04B38/06C04B38/04
Inventor 李永生崔云龙施剑林
Owner EAST CHINA UNIV OF SCI & TECH
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