Modified phenolic resin for fire resistive material and preparation method thereof

A technology of phenolic resin and refractory material, applied in fire-resistant coatings and other directions, can solve the problems of carbonized structure, difficult to graphitize carbon, poor oxidation resistance, environmental pollution, etc., to improve thermal shock stability, improve mechanical strength, and improve the degree of graphitization. high effect

Inactive Publication Date: 2008-08-20
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Commonly used binders for carbon composite refractory materials are asphalt and phenolic resin. Asphalt has a relatively high carbon residue rate, and there is a mesophase stage before the carbonization process, which is liquid carbonization, and the degree of graphitization of the carbonization structure is relatively high. It is in a glass state at room temperature, and the hot mixing process must be used in the mixing process with refractory granules and powders, which not only consumes energy, but also pollutes the environment due to the volatilization of a large amount of light aromatics in asphalt, especially among them. B[a]P has a strong carcinogenic effect on humans (He Junqiu, Wang Yanhua, Zhou Yanjun, etc. The current situation and improvement suggestions of carbon-containing refractory binders [J]. Fuel and Chemical Industry. 1998, 29 (1): 32~35.), which greatly affects the use of asphalt; the carbon residue rate of phenolic resin is relatively low, and it is solid carbonization, and the carbonization structure is hard graphitization carbon, but it can be adjusted to liquid, free phenol and formaldehyde content It is very low, which not only simplifies the mixing and molding process of refractor

Method used

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Effect test

Embodiment 1

[0012] A preparation method of high-efficiency modified phenolic resin for refractory materials, using the sol-gel method to prepare the cobalt metal oxide sol precursor, adding it to the phenolic resin diluted with absolute ethanol, the cobalt metal oxide sol precursor The amount of addition is 1wt% of the phenolic resin diluted with absolute ethanol; under the condition of 40-45°C, stir on the stirrer for 3-4 hours, then place it in the evaporator, adjust the pressure to 0.08-0.085MPa, and heat up to 40-45°C, react for 5-6 hours to obtain catalytically modified phenolic resin.

[0013] The metal oxide sol precursor preparation method of described cobalt is: Co(NO 3 ) 2 ·6H 2 O is added to 50% ethanol by volume to obtain 0.5mol / L Co(NO 3 ) 2 solution, and then using hydrazine as a catalyst to adjust its pH to 6-7; the volume percentage of water in the dispersion medium of the cobalt metal oxide sol precursor is lower than 50%.

[0014] The dilution amount of the phenolic...

Embodiment 2

[0017] A preparation method of high-efficiency modified phenolic resin for refractory materials, using the sol-gel method to prepare the metal oxide sol precursor of iron, adding it to the phenolic resin diluted with absolute ethanol, and the metal oxide sol precursor of iron The addition amount is 1wt% of the phenolic resin diluted with absolute ethanol; under the condition of 45~50 ℃, stir on the stirrer for 4~5 hours, then place it in the evaporator, adjust the pressure to 0.08~0.085MPa, heat up to 45-50°C, react for 5-6 hours to obtain catalytically modified phenolic resin.

[0018] The metal oxide sol precursor preparation method of described iron is: Fe(NO 3 ) 3 9H 2 O is added to 50% ethanol by volume to obtain 0.5mol / L Fe(NO 3 ) 3 solution, and then using hydrazine as a catalyst to adjust its pH to 6-7; the volume percentage of water in the dispersion medium of the iron metal oxide sol precursor is lower than 50%.

[0019] The dilution amount of the phenolic resin...

Embodiment 3

[0022] A preparation method of high-efficiency modified phenolic resin for refractory materials, using the sol-gel method to prepare the metal oxide sol precursor of nickel, adding it to the phenolic resin diluted with absolute ethanol, and the metal oxide sol precursor of nickel The amount of addition is 2wt% of the phenolic resin diluted with absolute ethanol; under the condition of 50-55°C, stir on the stirrer for 5-6 hours, then place it in the evaporator, adjust the pressure to 0.08-0.085MPa, and heat up to 50-55°C, react for 6-7 hours to obtain catalytically modified phenolic resin.

[0023] The metal oxide sol precursor preparation method of described nickel is: Ni(NO 3 ) 2 ·6H 2 O is added to 50% ethanol by volume to obtain 0.5mol / L Ni(NO 3 ) 2 solution, and then using hydrazine as a catalyst to adjust its pH to 6-7; the volume percentage of water in the dispersion medium of the iron metal oxide sol precursor is lower than 50%.

[0024] The dilution amount of the ...

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Abstract

The invention relates to a phenolic resin resin modified for refractories and a preparation method thereof. The technical scheme applied by the invention is that a sol-gel precursor of ferric, cobalt, or nickel metal oxide prepared by a sol-gel method are added into a dehydrated alcohol diluted phenolic resin, and the quantity of the sol-gel precursor of ferric, cobalt, or nickel metal oxide is 1-5 % by weight of the dehydrated alcohol diluted phenolic resin; the solution is stirred for 3-10 hours at the temperature of 40-85 DEG C, and then is put into a evaporator where the compound reacts for 5-10 hours at pressure of 0.08-0.09 MPa and temperature of 40-85 DEG C. Firstly, the phenolic resin modified for refractories prepared by the invention can transform the resin char from amorphous glassy carbon into crystalline graphitic carbon in-situ synthesizing a carbon nanotube in the refractories; secondly, availability of the carbon nanotube also can improve the carbon yield ratio of phenolic resin, thus improving the inoxidability, thermal shock resistance and mechanical strength for the refractories.

Description

technical field [0001] The invention belongs to the technical field of binders for composite refractory materials. In particular, it relates to a modified phenolic resin for refractory materials and a preparation method thereof. Background technique [0002] Commonly used binders for carbon composite refractory materials are asphalt and phenolic resin. Asphalt has a relatively high carbon residue rate, and there is a mesophase stage before the carbonization process, which is liquid carbonization, and the degree of graphitization of the carbonization structure is relatively high. It is in a glass state at room temperature, and the hot mixing process must be used in the mixing process with refractory granules and powders, which not only consumes energy, but also pollutes the environment due to the volatilization of a large amount of light aromatics in asphalt, especially among them. B[a]P has a strong carcinogenic effect on humans (He Junqiu, Wang Yanhua, Zhou Yanjun, etc. Th...

Claims

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Application Information

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IPC IPC(8): C08G8/28C08G8/04C09K21/02
Inventor 李亚伟王国飞赵雷李远兵金胜利李淑静谢婷
Owner WUHAN UNIV OF SCI & TECH
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