Method for preparing mesoporous carbon material

A carbon material and porous carbon technology, applied in the field of porous carbon material preparation, can solve the problems of high production cost, limited popularization and application, waste, etc., and achieve the effect of low cost and simple process

Inactive Publication Date: 2009-09-16
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material direct activation method in the conventional activation method uses zinc chloride as the activator, and the porous carbon prepared is mostly microporous carbon, and it is difficult to adjust the pore structure of the carbon material; although the secondary activation method can produce a high specific surface area Porous carbon, but the activators such as potassium hydroxide have strict requirements on the corrosion resistance of equipment, high production conditions, and it is difficult to adjust the pore structure of carbon materials
The organic gas (frozen) gel carbonization method requires special drying methods such as supercritical drying or freeze drying, and the equipment cost is high, and the specific surface area of ​​the prepared carbon material is not high
The hard template carbonization method places the carbon precursor in a porous inorganic template of silica or alumina, and then carbonizes and removes the mold. It is necessary to chemically remove the silica-based or alumina-based template after carbonization, resulting in waste
The soft template method uses surfactants such as block copolymers as structure-directing agents, and uses the self-assembly phenomenon of surfactants to direct the structure of carbon precursor polymers to achieve the purpose of controlling the pore structure of carbon materials. The production cost of block copolymer surfactants is still relatively high, which limits the popularization and application of this method

Method used

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  • Method for preparing mesoporous carbon material
  • Method for preparing mesoporous carbon material
  • Method for preparing mesoporous carbon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 5 g of phenolic resin, dissolve in 20 ml of ethanol; dissolve 10 g of polyethylene glycol with a molecular weight of 4000 in 30 ml of ethanol, mix the two solutions, and stir for 30 minutes. 0.5 g of sodium hydroxide was added thereto, and stirring was continued for 1 h. Ethanol was evaporated at 30-40°C for 5h, then dried in an oven at 90°C for 12h. Transfer to a tube furnace with 99.9% nitrogen protection, raise the temperature to 280°C at a rate of 10°C / min, hold for 1h, then raise the temperature to 900°C at a rate of 5°C / min, and hold for 1h. After cooling, the carbon material is taken out from the tube furnace, washed with water until the washing solution is neutral, and dried to obtain the product.

[0024] attached figure 1 It is the thermogravimetric analysis curve of the organic / organic compound. It can be seen from the figure that the thermally unstable polyethylene glycol decomposes before the gasification of the phenolic resin, and the gasification o...

Embodiment 2

[0026] Take 5 g of phenolic resin, dissolve in 20 ml of ethanol; dissolve 15 g of polyethylene glycol with a molecular weight of 4000 in 50 ml of ethanol, mix the two solutions, and stir for 30 minutes. 2.0 g of sodium hydroxide was added thereto, and stirring was continued for 1 h. Ethanol was evaporated at 30-40°C for 5h, then dried in an oven at 90°C for 12h. Transfer to a tube furnace with 99.9% nitrogen protection, heat up to 280°C at a rate of 10°C / min, hold for 2h, then raise the temperature to 900°C at a rate of 5°C / min, and hold for 1h. After cooling, the carbon material is taken out from the tube furnace, washed with water until the washing solution is neutral, and dried to obtain the product.

[0027] The carbon material prepared in this example has a specific surface area of ​​1100m 2 / g, average pore diameter 6.8nm, total pore volume 1.02cm 3 / g, mesopore volume 0.90cm 3 / g, the mesopore volume accounts for 88% of the total pore volume.

Embodiment 3

[0029] Take 5 g of phenolic resin, dissolve in 20 ml of ethanol; dissolve 15 g of polyethylene glycol with a molecular weight of 20,000 in 50 ml of ethanol, mix the two solutions, and stir for 30 minutes. 2.0 g of potassium hydroxide was added thereto, and stirring was continued for 1 h. Ethanol was evaporated at 30-40°C for 5h, then dried in an oven at 90°C for 12h. Transfer to a tube furnace with 99.9% nitrogen protection, raise the temperature to 300°C at a rate of 10°C / min, hold for 2h, then raise the temperature to 900°C at a rate of 5°C / min, and hold for 1h. After cooling, the carbon material is taken out from the tube furnace, washed with water until the washing solution is neutral, and dried to obtain the product.

[0030] The carbon material prepared in this example has a specific surface area of ​​1183m 2 / g, average pore diameter 5.6nm, total pore volume 1.15cm 3 / g, mesopore volume 0.95cm 3 / g, the mesopore volume accounts for 82% of the total pore volume.

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Abstract

The invention belongs to the technical field of porous carbon material preparation and provides a method for preparing a mesoporous carbon material. In the method, two polymers are mixed in certain solvent and can form the characteristic of a phase separation structure and thermal stability difference thereof; the polymer with high thermal stability is used as a carbon precursor; the thermally instable polymer which can be gasified during high-temperature treatment is used as pore former; two polymers are solved and mixed directly; certain quantity of solid alkali is added; the solvent is removed; the polymers are carbonized; and the mesoporous carbon material is obtained. The invention uses the synergic action of gasification pore-forming and chemical activation pore-forming to realize the forming of a pore structure of the carbon material and the control towards the pore structure of the carbon material. The specific area of the prepared carbon material is more than 1300m <2> / g, the average aperture is between 4nm and 10nm, and the proportion of the mesopore volume and the total pore volume is more than 80 percent. The method for preparing the mesoporous carbon material has the advantages of simple technology, wide raw material source, low cost, the obvious mesoporous characteristic of the prepared carbon material and the like, and the invention has good application prospect.

Description

[0001] Field: [0002] The invention belongs to the field of preparation of porous carbon materials, and in particular relates to a preparation method of mesoporous carbon. Background technique: [0003] Porous carbons are widely used in medicine, environment, energy and other fields because of their advantages such as wide source of raw materials, low price and good chemical stability. According to the pore structure of porous carbon, the International Union of Pure and Applied Chemistry divides porous carbon into three categories: microporous carbon (average pore diameter<2nm), mesoporous carbon (2nm<average pore diameter<50nm), macroporous carbon (average pore diameter >50nm). Applications in different fields have different performance requirements for porous carbon. For example, the adsorption of small organic molecules such as formaldehyde requires the use of microporous carbons; the adsorption of macromolecules such as dyes requires the use of mesoporous or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 侯朝辉阎建辉唐课文周宁波何斌鸿易健民邓春兴
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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