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Method for preparing ordered mesoporous carbon material

A mesoporous carbon and mesoporous technology, which is used in the preparation of ordered mesoporous carbon materials and the field of ordered mesoporous carbon material preparation, can solve the problems affecting the order degree and specific surface area of ​​mesoporous carbon materials, and hard template mesoporous channels. Filling up precursors, etc.

Inactive Publication Date: 2014-07-02
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The shortcoming of above-mentioned nano-casting method is that it is difficult to completely fill the precursor in the mesoporous channels of the hard template, thereby affecting the degree of order and the specific surface area of ​​the mesoporous carbon material (Zhao Dongyuan et al., ordered mesoporous molecular sieve materials, Higher Education Press , 2013, ISBN978‐7‐04‐036543‐6)

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Weigh 4.0g of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123) into a 250ml beaker, add 126ml of deionized water, and stir at room temperature until P123 is completely dissolved. Add 20ml of concentrated hydrochloric acid with a mass fraction of 37% to the beaker, continue to stir for 2 hours, while the temperature of the water bath rises to 35°C, and then add 9.2ml of ethyl orthosilicate dropwise while stirring vigorously (rotation speed 200‐300rpm), continue After vigorous stirring for 24 hours, the reaction solution was poured into a self-pressurized reactor, crystallized at 100°C for 12 hours, suction filtered, washed, and dried at 80°C for 6 hours, and the dried sample was calcined at 550°C for 6 hours to remove the template agent to obtain SBA ‐15 molecular sieve, the nitrogen adsorption and desorption isotherm test shows that the nitrogen adsorption pore volume is 1.01cm 3 / g;

[0027] Take 1.0g SBA‐15 powder, add figure 1 In ...

Embodiment 2

[0030] Weigh 3.2g CTAB into a 250ml beaker, add 152ml deionized water and 24.0g NaOH, continue to stir for 2h, add 15.2g tetraethyl orthosilicate, stir for 1h, pour the solution into a self-pressurized reaction kettle, at 110°C Crystallize for 72 hours, filter and wash with water, dry at room temperature, and then bake at 550°C for 6 hours to remove the template agent to obtain MCM-48 molecular sieve;

[0031] Take 1.0g MCM-48 powder, add figure 1 In the left bottle 1 of the shown vacuum vaporization-capillary condensation nano-casting device, inject 1.01ml of aniline liquid into the right bottle 2, connect the second valve 4, and connect the first valve 3 after sealing to evacuate. Move the whole device into the heating box, raise the temperature from room temperature to 185°C, and keep the temperature until the liquid in the bottle 2 on the right disappears, then take it out after natural cooling, add 25ml of 0.5M ammonium persulfate solution to the bottle 1 on the left, and...

Embodiment 3

[0033] Weigh 4.0g of P123 into a 250ml beaker, add 126ml of deionized water, seal and stir at room temperature until P123 is completely dissolved, then add 20ml of concentrated hydrochloric acid with a mass fraction of 37% to the beaker, and continue stirring for 2 hours, while the temperature of the water bath rises to 40 ℃, then add 9.2ml tetraethyl orthosilicate dropwise while stirring vigorously, continue to stir vigorously for 24h, then pour the reaction solution into a self-pressurized reactor, crystallize at 120°C for 24h, wash with suction and wash with water at 80°C After drying for 4 hours, bake at 550°C for 6 hours to remove the template agent to obtain SBA-15 molecular sieve; take 1.0g of SBA-15 powder, add figure 1 In bottle 1 on the left as shown, inject 0.5ml of freshly steamed aniline and 0.5ml of freshly steamed pyrrole liquid into bottle 2 on the right, connect the second valve 4, connect the first valve 3 to vacuum after sealing, and then put the whole pair o...

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Abstract

The invention discloses a method for preparing an ordered mesoporous carbon material. The method comprises the following steps: firstly, preparing a mesoporous silicon dioxide hard template material; determining the pore volume through a nitrogen adsorption-desorption isotherm; adding a precursor of which the volume is equal to the pore volume of the ordered mesoporous silica hard template; heating up to a boiling point of the precursor in a vacuum state; keeping the temperature for 0.5-3 hours; completely pouring the precursor into a template duct by vaporization-micro / mesoporous capillary condensation, hole surface wetting and migration in the hole, so as to achieve isometric impregnation; adding the impregnated powder to a polymerization initiator solution to polymerize and transform; drying in vacuum at 80-120 DEG C after filtering and washing; heating up to 800-1100 DEG C in a tube furnace; carrying out high-temperature carburization in an inert gas atmosphere; processing the obtained powder in an HF solution, filtering, washing and drying to prepare the ordered mesoporous carbon material. The prepared ordered mesoporous carbon material has super-high specific surface area and pore volume, and can be applied to adsorption, separation, catalysis, an electrode and the like.

Description

technical field [0001] The invention relates to an ordered mesoporous carbon material, in particular to a preparation method of an ordered mesoporous carbon material, belonging to the field of ordered mesoporous carbon material preparation. Background technique [0002] Ordered mesoporous carbon has the characteristics of mesoscopic ordered structure, regular pore structure, large pore volume and high specific surface area, and has broad applications in the fields of electrochemistry, catalysis, hydrogen storage, adsorption, and separation. [0003] The hard template method is an effective way to prepare ordered mesoporous carbon: first prepare ordered mesoporous template materials (such as SBA-15, MCM-48 and other mesoporous silica), and cast carbon sources (such as sucrose, furfuryl alcohol, etc.) followed by high-temperature carbonization, and finally the template was removed by hydrofluoric acid or a strong alkaline solution to obtain an ordered mesoporous carbon materia...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01B32/05
Inventor 梁振兴万凯
Owner SOUTH CHINA UNIV OF TECH
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