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Method for preparing ordered mesoporous carbon

A mesoporous carbon and pre-carbonization technology, which is applied in the field of preparation of ordered mesoporous carbon materials, can solve the problems of low carbon yield and inability to obtain ordered mesoporous carbon materials, and achieve high carbon formation rate, low price, Effect of improving carbon yield

Inactive Publication Date: 2007-01-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method is simple in technology and avoids the waste of surfactant, its disadvantage is that the carbon yield is low, as only 16% triblock copolymer in the silicon / P123 compound mentioned in this document converted to carbon
Although the mesoporous carbon synthesized by this method has the characteristics of narrow pore size distribution, the pores of the obtained carbon are arranged in a disordered honeycomb shape, and this method cannot obtain ordered mesoporous carbon materials.

Method used

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  • Method for preparing ordered mesoporous carbon
  • Method for preparing ordered mesoporous carbon
  • Method for preparing ordered mesoporous carbon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Dissolve 4g of P123 (analytical grade, Aldrich) and 1g of sucrose in 160ml of hydrochloric acid solution with a molar concentration of 2M, stir well at 35°C, and after it dissolves, add 9.2ml of tetraethyl orthosilicate (with sucrose) dropwise The dosage ratio is 9.2ml / g), after continuing to stir for 24 hours, put it in an oven at 100°C for 24 hours to stand for crystallization, then filter, wash and dry at room temperature to obtain the sucrose / P123 / silicon ternary complex. Mix 1g of the ternary compound with 10ml of water and 1ml of sulfuric acid with a concentration of 98% and mix and stir for 12 hours. After filtering, put the resulting precipitate in an oven at 160°C for 6 hours for pre-carbonization; the ternary compound after pre-carbonization Under the protection of nitrogen, the temperature was raised to 800°C at a heating rate of 1°C / min for carbonization, and after 2 hours of heat preservation, it was naturally cooled to room temperature to obtain a carbon / si...

Embodiment 2

[0030] The operation method is the same as in Example 1, except that the dosage of P123 is 3.75g and the dosage of sucrose is 1.25g (the mass ratio of P123 to sucrose is 3:1, and the ratio of ethyl orthosilicate to sucrose is 7.4ml / g) , finally obtained 0.59g mesoporous carbon. XRD analysis test shows that the obtained material is a mesoporous carbon with two-dimensional hexagonal structure arrangement, d 100 8.2nm, unit cell parameter a 0 9.5nm.

Embodiment 3

[0032] The operation method is the same as that in Example 1, except that the sucrose / P123 / silicon ternary complex was synthesized by crystallization at a crystallization temperature of 80° C. for 24 hours, and finally 0.52 g of mesoporous carbon was obtained. XRD analysis test shows that the obtained material is a mesoporous carbon with two-dimensional hexagonal structure arrangement, d 100 7.8nm, unit cell parameter a 0 9.0nm.

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Abstract

The process of preparing ordered mesoporous carbon material includes the following steps: dissolving three block polyoxene-polypropylene epoxide-polyoxene copolymer and saccharide carbohydrate in the weight ratio of 3-4 in acid solution through stirring at 35 deg.c, adding silicon source in the amount of 7-10 ml for each gram of the saccharide carbohydrate, stirring for 24 hr; crystallizing the obtained solution inside a sealed still at 80-130 deg.c for 24-72 hr, filtering, washing and drying at room temperature to obtain ternary composition of saccharide carbohydrate, three block copolymer and silicon; and pre-carbonizing, carbonizing and eliminating silicon to obtain ordered mesoporous carbon material. The process has low cost, high carbon forming rate homogeneous pore size and other features.

Description

technical field [0001] The invention relates to a preparation method of an ordered mesoporous carbon material. The method is a ternary compound composed of sugar carbohydrates, polyoxyethylene-polyoxypropylene-polyoxyethylene triblock copolymer and silicon source. The composite is pre-carbonized, carbonized and desiliconized to obtain ordered mesoporous carbon. Background technique [0002] Ordered Mesoporous Carbon (OMC) is a kind of carbon material with regularly arranged pores, pore diameter between 2nm and 50nm, and uniform pore size. Since Professor Liu Long from South Korea first reported the synthesis of ordered mesoporous carbon using ordered mesoporous silicon as a hard template in 1999, his research has attracted great attention from academia and business circles. Ordered mesoporous carbon materials not only have the characteristics of high specific surface area and narrow pore size distribution, but also have hydrophobicity, chemical inertness, good hydrothermal ...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 宋怀河李丽霞陈晓红
Owner CHINA PETROLEUM & CHEM CORP
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