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Ultramicroporous carbon material and preparation method thereof

A technology of microporous carbon and carbon materials, applied in chemical instruments and methods, carbon compounds, inorganic chemistry, etc., can solve problems such as equipment corrosion, environmental pollution, and insufficient pore structure development.

Inactive Publication Date: 2018-03-23
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method can produce a well-developed pore structure, the activation effect is better, but the traditional activation process consumes a large amount of KOH, which is usually 3 to 4 times the mass ratio of the carbon precursor for physical grinding, which increases the preparation cost and causes The equipment is corroded, causing great pollution to the environment, and the micropores constructed are mainly concentrated in 1-2nm, and the pore structure is still not developed enough

Method used

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  • Ultramicroporous carbon material and preparation method thereof
  • Ultramicroporous carbon material and preparation method thereof
  • Ultramicroporous carbon material and preparation method thereof

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preparation example Construction

[0026] The invention provides a method for preparing a very microporous carbon material, comprising the following steps:

[0027] (1) After mixing monosaccharides, unsaturated organic acids and water, perform a hydrothermal reaction to obtain a hydrothermal carbon material;

[0028] (2) performing a replacement reaction after mixing the hydrothermal carbon material obtained in the step (1) with alkali metal hydroxide and water to obtain a replacement carbon material;

[0029] (3) Activating the substituted carbon material obtained in the step (2) to obtain a very microporous carbon material.

[0030] The invention mixes monosaccharides, unsaturated organic acids and water and then performs hydrothermal reaction to obtain hydrothermal carbon materials. In the present invention, the monosaccharide preferably includes one or more of glucose, fructose, galactose, ribose and deoxyribose. In the present invention, the source of the monosaccharide is not particularly limited, and c...

Embodiment 1

[0049] Add 6g of glucose to 60mL of aqueous solution, stir until clear liquid, add 0.06g (1% of the mass of glucose) of acrylic acid and stir evenly, put polytetrafluoroethylene in the reaction kettle, hydrothermally treat at 200°C for 12h, and finally obtain The solution was filtered, washed, and then dried at 80° C. for 10 h to obtain a hydrothermal carbon material.

[0050] Prepare KOH into 30 mL of an aqueous solution with a concentration of 0.03 mol / L, add the above hydrothermal carbon material, then stir in a 70°C water bath for 10 hours, centrifuge until the washing liquid is neutral, and then dry the solid in an oven at 80°C .

[0051] Afterwards, the solid was activated in a tubular resistance furnace, heated to 600°C under a nitrogen atmosphere, and kept at a constant temperature for 8 hours. Finally, the obtained sample was stirred in 10% dilute hydrochloric acid for 1 hour, and dried to obtain the AcA1 sample.

Embodiment 2

[0053] Add 6g of glucose to 60mL of aqueous solution, stir until clear liquid, add 0.12g (2% of the mass of glucose) of acrylic acid and stir evenly, put polytetrafluoroethylene in the reaction kettle, hydrothermally treat at 180°C for 16h, and finally obtain The solution was filtered, washed, and then dried at 80° C. for 10 h to obtain a hydrothermal carbon material.

[0054] Prepare KOH into 30 mL of an aqueous solution with a concentration of 0.06 mol / L, add the above-mentioned hydrothermal carbon material, then stir in a water bath at 80°C for 8 hours, centrifuge until the washing liquid is neutral, and then dry the solid in an oven at 80°C .

[0055] Afterwards, the solid was activated in a tube-type resistance furnace, heated to 700°C under a nitrogen atmosphere, and kept at a constant temperature for 6 hours. Finally, the obtained sample was placed in 10% dilute hydrochloric acid and stirred for 1 hour, then dried to obtain the AcA2 sample.

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Abstract

The invention provides a preparation method of an ultramicroporous carbon material, comprising the following steps: mixing monosaccharide, nonsaturated organic acid and water and carrying out a hydrothermal reaction to obtain a hydrothermal carbon material; mixing the hydrothermal carbon material with alkali metal hydroxide and water and carrying out a displacement reaction to obtain a displacement carbon material; and activating to obtain the ultramicroporous carbon material. By mixing nonsaturated organic acid during the hydrothermal carbonization process, a functional group capable of alkali metal ion displacement is formed on the surface of the carbon material. Thus, ion exchange sites are provided for a subsequent ionic type chemical activation method, and atomic-scale dispersion of alkali metal ions is finally realized. In addition, use amount of an activator can be effectively reduced, and the porous carbon material rich in ultramicropores is finally synthesized. Experimental results show that the use amount (converted to use amount of an industrial KOH chemical activation method) of the activator used in the preparation method is about 0.3% of mass of a carbon precursor andthe prepared ultramicroporous carbon material is rich in ultramicropores with the pore diameter being 0.7 nm and below.

Description

technical field [0001] The invention relates to the technical field of preparation of porous carbon materials, in particular to a very microporous carbon material and a preparation method thereof. Background technique [0002] CO 2 As the most important greenhouse gas, its content in the atmosphere is increasing day by day, leading to a series of environmental problems such as global warming, which seriously threatens the survival and development of human beings. Therefore, CO 2 The capture and storage of water has become particularly important. Currently, CO 2 Capture technologies mainly include absorption method, membrane separation method and adsorption method. The absorption method is highly corrosive to equipment, has high regeneration energy consumption, and is also restricted by temperature; the membrane separation method generally has a high cost, which limits its application; and the adsorption method shows great advantages and is favored by researchers. The cor...

Claims

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Application Information

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IPC IPC(8): C01B32/348
Inventor 刘振阎子峰刘欣梅王有和张震
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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