Benzoxazine resin based carbon aerogel and a preparing method thereof

A benzoxazine and carbon aerogel technology, which is applied in the field of porous carbon material preparation, can solve the problems of low product purity, high production cost and long preparation period, and achieves high specific surface area, reduced production cost and shortened preparation period. Effect

Inactive Publication Date: 2016-11-09
TAISHAN MEDICAL UNIV
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  • Abstract
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Problems solved by technology

[0004] The object of the present invention is to provide a benzoxazine resin-based carbon aerogel and its preparation method, aiming to solve the problems of long prep...

Method used

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  • Benzoxazine resin based carbon aerogel and a preparing method thereof
  • Benzoxazine resin based carbon aerogel and a preparing method thereof
  • Benzoxazine resin based carbon aerogel and a preparing method thereof

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preparation example Construction

[0054] Such as figure 1 As shown, the preparation method of the benzoxazine resin-based carbon aerogel of the embodiment of the present invention comprises the following steps:

[0055] S101: Weigh a certain amount of amine and paraformaldehyde into a four-necked flask, dissolve it with a certain amount of organic solvent, the mass of the organic solvent is 1 to 3 times the mass of the amine and paraformaldehyde, and put it at room temperature for 20 to 30 Stir at ℃ for 10-20 minutes to dissolve completely;

[0056] S102: Weigh a certain mass of phenolic monomer and dissolve it in an organic solvent whose mass is 1 to 2 times that of phenol, mix this solution with the above solution, and continue to stir at a stirring speed of 400 to 600r / min. Then gradually raise the temperature to 90°C, the heating rate is 1°C / min, and react at 90°C for 4-8 hours, so that the amine, paraformaldehyde and phenolic monomers undergo a ring-forming reaction to obtain a transparent, shallow red ...

Embodiment 1

[0067] Weigh 50g of 4,4'-methylene dianiline, add 30g of paraformaldehyde into a four-neck flask, dissolve with 250ml of xylene, and stir at room temperature 25°C for 20 minutes to completely dissolve;

[0068] Weigh 47.1g of phenol, dissolve it in 50ml of xylene, mix this solution with the above solution, continue to stir at a stirring speed of 400r / min, and gradually raise the temperature to 90°C at a heating rate of 1°C / min. React for 6 hours to prepare a benzoxazine solution with a concentration of 30%; place the above benzoxazine solution in an oil bath at 130°C and heat it for 6 hours to solidify to obtain a partially cured polybenzoxazine wet gel ;

[0069] The above polybenzoxazine wet gel was naturally dried at an ambient temperature of 25°C and normal pressure for 10 hours to obtain a partially cured polybenzoxazine airgel;

[0070] The conditions for placing the partially cured polybenzoxazine airgel in a carbonization furnace and performing heat treatment under th...

Embodiment 2

[0074] Weigh 75g of 4,4'-methylene dianiline, add 45g of paraformaldehyde into a four-neck flask, dissolve with 150ml of xylene, and stir at room temperature 25°C for 20 minutes to completely dissolve;

[0075] Weigh 70.7g of phenol and dissolve it in 50ml of xylene. After dissolving, add this solution to the above solution and stir at a stirring speed of 600r / min. The reaction was carried out for 8 hours to obtain a 50% benzoxazine solution;

[0076] The above benzoxazine solution was placed in an oil bath at 130°C and heated for 8 hours to solidify to obtain a partially cured polybenzoxazine wet gel;

[0077] The above polybenzoxazine wet gel was naturally dried at an ambient temperature of 25°C and normal pressure for 12 hours to obtain a partially cured polybenzoxazine airgel;

[0078] The conditions for placing the partially cured polybenzoxazine airgel in a carbonization furnace and performing heat treatment under the protection of an inert gas are as follows: from room...

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Abstract

Benzoxazine resin based carbon aerogel and a preparing method thereof are disclosed. The method includes weighing an amine and paraformaldehyde, adding into a four-neck distillation flask, adding an organic solvent, stirring at room temperature until full dissolution, weighing a phenol monomer, dissolving the monomer into the organic solvent, mixing the obtained solution with the solution mentioned above, stirring, gradually heating to allow the amine, the paraformaldehyde and the phenol monomer to be subjected to an annulation reaction to obtain a benzoxazine solution, heating the benzoxazine solution in an oil bath to cure the benzoxazine solution so as to prepare partially-cured polybenzoxazine wet gel, naturally drying the partially-cured polybenzoxazine wet gel to prepare partially-cured polybenzoxazine aerogel, and subjecting the cured polybenzoxazine aerogel to heat treatment and high-temperature carbonization in an inert atmosphere to prepare polybenzoxazine resin based carbon aerogel. The product has advantages of a short preparation period, a low production cost, low equipment requirements, high safety, and high product purity.

Description

technical field [0001] The invention belongs to the technical field of preparation of porous carbon materials, and in particular relates to a benzoxazine resin-based carbon aerogel and a preparation method thereof. Background technique [0002] Carbon airgel is a new type of amorphous porous carbon material with a three-dimensional network structure, which has high porosity (80%-99.8%) and high specific surface area (400-1200m 2 / g), a wide range of density changes (0.05 ~ 1.00g / cm 3 ), low thermal conductivity (10-40mW / m k), controllable pore structure and pore size distribution, good electrical conductivity, stable chemical properties, etc. It is a functional material with many excellent properties. It is used in hydrogen storage materials and catalysts. Carriers, heat insulation materials, adsorption materials, supercapacitors, rechargeable battery electrodes and other fields have broad application prospects. In 1989, Pekala et al. of Lawrence Livermore Laboratory in th...

Claims

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Application Information

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IPC IPC(8): C01B31/02
CPCC01P2004/03C01P2006/10C01P2006/12C01P2006/16
Inventor 常海涛
Owner TAISHAN MEDICAL UNIV
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