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Method for synthesizing mesoporous carbon material

A synthesis method and mesoporous carbon technology, applied in the preparation/purification of carbon, can solve the problems of waste of raw materials, difficult recovery of organic solvents, environmental pollution, etc., and achieve the effect of accelerating the volatilization rate and avoiding the difficulty of solvent recovery

Active Publication Date: 2017-03-29
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The existing EISA method for synthesizing mesoporous carbon requires a large amount of organic solvent. Since the solution evaporates naturally at room temperature on the surface of a wide container, the organic solvent is difficult to recover, which wastes raw materials and pollutes the environment.

Method used

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  • Method for synthesizing mesoporous carbon material
  • Method for synthesizing mesoporous carbon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 0.8g of F127 to 40g of deionized water and stir to dissolve, then add 4.0g of water-soluble phenolic resin to the solution, stir to dissolve at 40°C, continue to stir for 1h, pour the solution into an enamel tray, put it in a vacuum oven, and put it in a vacuum oven at 70 After vacuuming and evaporating the water solvent at ℃ for 10h, heat at normal pressure and 150℃ for 10h for further thermal polymerization, and then heat up and roast in a tube furnace under the protection of nitrogen at a heating rate of 1℃ / min. 3h, kept at 600°C for 2h to obtain ordered mesoporous carbon with a pore diameter of 3.2nm and a specific surface area of ​​620m 2 / g, pore volume 0.482cm 3 / g.

Embodiment 2

[0024] Add 1.5g of F127 and 0.5g of P123 into 100g of deionized water and stir to dissolve, then add 5.0g of soluble phenolic resin to the solution, stir and dissolve at 30°C to obtain a transparent solution, continue stirring for 0.5h, pour the solution into an enamel tray, and place In a vacuum oven, vacuum evaporate the water solvent at 25°C for 15h, heat at 100°C for 36h at normal pressure for further thermal polymerization, and then heat up and roast in a tube furnace under the protection of nitrogen. The heating rate is 2°C / min. Keep at 450°C for 3h and at 800°C for 2h to obtain ordered mesoporous carbon with a pore size of 3.6nm and a specific surface area of ​​630m 2 / g, pore volume 0.571cm 3 / g. Such as figure 1 The adsorption-desorption isotherm in is type Ⅳ with a hysteresis loop, indicating that the obtained sample is a mesoporous material. Such as figure 2 As shown in the small-angle XRD pattern of the prepared mesoporous carbon sample, there are three obviou...

Embodiment 3

[0026] Add 1.0g of P123 to 100g of deionized water and stir to dissolve, then add 0.5g of furan resin to the solution, stir and dissolve at 30°C to obtain a transparent solution, continue to stir for 0.5h, pour the solution into an enamel tray, and place it in a vacuum oven. After evaporating the water solvent at 60°C for 10h, heat at 80°C for 60h at normal pressure for further thermal polymerization, and then heat up and roast in a tube furnace under the protection of nitrogen. The heating rate is 2°C / min and kept at 350°C. 3h, kept at 700°C for 3h to obtain ordered mesoporous carbon with a pore size of 3.0nm and a specific surface area of ​​720m 2 / g, pore volume 0.598cm 3 / g.

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Abstract

The invention relates to a method for synthesizing a mesoporous carbon material. The method comprises the following steps: dissolving a carbon precursor and a template agent in water to form a uniform liquid which is prepared from 0.5-10 mass percent of the carbon precursor, 0.2-2 mass percent of the template agent and the balance of an aqueous liquid; spinning or directly pouring the prepared liquid to the surface of a container to form a coating; putting the coated container in a closed device, and vacuumizing at room temperature to 70 DEG C until the solvent moisture is completely volatilized; further thermally polymerizing and curing the obtained sample at 80-150 DEG C for 10-60 hours; and roasting the cured sample at 600-1000 DEG C under protection of nitrogen atmosphere to obtain the ordered mesoporous carbon material. According to the preparation method, the ordered mesoporous carbon material is synthesized by adopting water as a solvent through an evaporation-induced self-assembly (EISA) method, and the evaporation speed of the solvent is accelerated under slight heating and vacuumizing conditions, so that the problems of solvent reclaiming difficulty, raw material waste and environment pollution caused by adopting organic solvents in the prior art can be avoided.

Description

technical field [0001] The present invention relates to a method for synthesizing mesoporous carbon materials, in particular to using water as a solvent in the process of synthesizing mesoporous carbon materials by a solvent evaporation-induced self-assembly (EISA) method, and speeding up the volatilization rate of water by vacuumizing and slightly heating . Background technique [0002] Ordered mesoporous carbon is a new type of material developed in the past ten years. It has the characteristics of uniform pore size distribution, large specific surface area and pore volume, orderly pore structure, high mechanical strength, and good thermal stability. It is used in catalysis, adsorption, and separation. , gas storage, electrochemistry and other aspects have good application prospects. [0003] The synthesis of ordered mesoporous carbon mainly includes hard template method and soft template method. The hard template method requires the synthesis of hard template ordered me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
CPCC01P2002/72C01P2006/12C01P2006/14C01P2006/16
Inventor 崔凤霞李荣李军陈玮娜段大勇
Owner CHINA PETROLEUM & CHEM CORP
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