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Mesoporous silicon carbide material and mfg. method thereof

A silicon carbide mesoporous and mesoporous silicon carbide technology is applied in chemical instruments and methods, carbon compounds, inorganic chemistry, etc., to achieve the effects of low cost, easy availability of raw materials and simple equipment

Inactive Publication Date: 2003-03-12
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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There is no report on the mesoporous silicon carbide material and its preparation method

Method used

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Embodiment 1

[0021] Dissolve 5 g of phenolic resin in 20 ml of absolute ethanol, add 0.5 g of nickel nitrate, and stir electromagnetically to make it completely dissolved. Then add 20ml of ethyl orthosilicate and 3ml of 3.5% oxalic acid aqueous solution, and control the stirring at 20°C for 56 hours. After the carbon-silicon binary sol is formed, add 2ml of 30% hexamethylenetetramine aqueous solution, stir for 1 hour, let stand at 20°C for 48 hours to gel, and bake the gel at 100°C for 20 hours. Obtain the silicon carbide precursor. Put the precursor into the alumina boat, put it into the tube furnace, in an argon atmosphere, heat up to 800°C at a heating rate of 3°C / min, and then heat up to 1250°C at a heating rate of 2°C / min. After reacting for 20 hours, it was cooled to room temperature. The sample is treated in the air at 600°C for 4 hours, washed with a mixture of cyanofluoric acid and hydrochloric acid to remove unreacted silica, washed with water, filtered, and dried to obtain a specifi...

Embodiment 2

[0023] Dissolve 12 g of phenolic resin in 40 ml of absolute ethanol, add 0.5 g of nickel nitrate, and electromagnetically stir to dissolve it completely. Then add 50ml of ethyl orthosilicate and 1ml of concentrated hydrochloric acid, and control the stirring at 30°C for 30 hours. After the carbon-silicon binary sol is formed, 3 ml of 40% hexamethylenetetramine aqueous solution is added, and after stirring for 1 hour, it is allowed to stand for 36 hours to gel. The gel was baked at 80°C for 30 hours to prepare a silicon carbide precursor. The precursor was put into an alumina boat, put into a tube furnace, and heated to 820°C at a heating rate of 4°C / min under an argon atmosphere, and kept for 30 minutes. Then the temperature was raised to 1200°C at a heating rate of 2°C / min, and after 24 hours of reaction, the temperature was lowered to room temperature. Treat the sample in the air at 600°C for 4 hours, wash with a mixture of cyanofluoric acid and hydrochloric acid to remove unrea...

Embodiment 3

[0025] Dissolve 15 g of phenolic resin in 50 ml of absolute ethanol, add 2 g of cobalt acetate, and stir to make it completely dissolved. Then add 50ml of propyl orthosilicate and 2ml of acetic acid, and stir at 40°C for 24 hours to form a carbon-silicon binary sol. Then 6ml of 30% hexamethylenetetramine aqueous solution was added, stirred for 1 hour, allowed to stand for 24 hours to make it gel, and then baked at 150°C for 5 hours to prepare a silicon carbide precursor. Put the precursor into the alumina boat, put it into the tube furnace, in an argon atmosphere, heat up to 850°C at a heating rate of 4°C / min, hold for 10 minutes, and then heat up to 1350 at a temperature rise rate of 1°C / min After reacting for 10 hours, the temperature is lowered to room temperature. The sample is treated in the air at 800°C for 1 hour, washed with a mixture of cyanofluoric acid and hydrochloric acid to remove unreacted silica, washed with water, filtered, and dried to obtain a specific surface a...

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Abstract

A powdered mesoporous silicon carbide material with beta crystal form, 3-50 nm of pore size distribution and 60-120 sq.m / g of specific surface area is prepared through dissolving phenolic resin in absolute alcohol or acetone, adding transition metal salt, stirring while adding ethyl (methyl or propyl) silicate and inorganic acid, hydrolysis, adding cross-linking agent, gelatinizing, thermal reactino in argon atmosphere, cooling, high-temp treating, acid washing, water washing, filtering and drying. It has low cost.

Description

[0001] Field: [0002] The invention belongs to a non-oxide mesoporous material and a preparation method thereof, and specifically relates to a silicon carbide mesoporous material and a preparation method thereof. Background technique: [0003] Silicon carbide has good mechanical strength, thermal stability, chemical inertness, thermal and electrical conductivity, and good resistance to radiation and electromagnetic loss. Therefore, silicon carbide as a high-performance special structural material has received widespread attention. At present, the preparation method of silicon carbide is mainly the Acheson method, that is, coke powder and quartz sand (SiO 2 ) The molar ratio is 3:1, mixed with appropriate amount of additives, and then heated to above 2000°C in an electric arc furnace, and silicon carbide is prepared through a series of complex chemical reactions. The silicon carbide prepared by this method is mainly an alpha crystal phase, with poor purity and small specific surfac...

Claims

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Application Information

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IPC IPC(8): C01B32/977C04B35/565
Inventor 郭向云靳国强梁萍王冬华
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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