Method for preparing high-surface-area nitrogenous mesoporous carbon material

A high surface area, porous carbon technology, applied in the field of preparation of high surface area nitrogen-containing mesoporous carbon materials, can solve the problems that it is difficult to meet high surface area and high nitrogen content at the same time, the template agent cannot be reused, and the nitrogen content of carbon materials is low. , to achieve good application prospects, high mesopore rate, and large total pore volume

Inactive Publication Date: 2010-09-08
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In summary, in the current methods for preparing nitrogen-containing porous carbon materials, all rely on the synthesis of templates, using templates to form pores and adjust the pore size distribution, the process is cumbersome, the preparation cycle is long, and the templates cannot be reused. The economy is poor. In addition, reagents such as strong alkali or hydrofluoric acid must be used to remove the template agent. The operation is cumbersome, making it difficult to produce in batches.
However, the carbon material obtained by the subsequent nitrogen doping method has low nitrogen content and poor doping effect, and it is difficult to meet the requirements of high surface area, large pore diameter, large pore volume and high nitrogen content at the same time.

Method used

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  • Method for preparing high-surface-area nitrogenous mesoporous carbon material
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  • Method for preparing high-surface-area nitrogenous mesoporous carbon material

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Weigh 23.5g of melamine, 45g of urea and 153g of 37% formaldehyde solution (weight ratio is 100:183:650), add 100g of water (196.5g of water in the mixture at this time); adjust the pH value to 9 with sodium carbonate, stir to dissolve Completely, add 35g of potassium chloride (148 parts by weight), stir to dissolve, and adjust the pH to 3.5 with hydrochloric acid; transfer the mixed solution to a 55°C oil bath or water bath for heating, and at this time, the raw materials undergo a polymerization reaction, and after about 0.5 hours To obtain a white resinous mixture, raise the temperature to 80°C and keep it for 4 hours, then transfer it to an oven at 140°C for curing for 24 hours to obtain a white solid; transfer the white solid to a carbonization furnace, and raise the temperature to 850°C in flowing helium , carbonized at constant temperature for 0.5 hours, and cooled to room temperature; the carbonized solid product was taken out, boiled with dilute hydrochloric aci...

Embodiment 2

[0037] Weigh 32g of melamine, 0g of urea and 114g of 37% formaldehyde solution (weight ratio is 100:0:356.), add 200g of water (272g of water in the mixture at this time); adjust the pH value to 8 with sodium hydroxide, stir to dissolve Completely, add 445g of zinc chloride (1390 parts by weight), stir to dissolve, and then adjust the pH to 3.5 with hydrochloric acid; transfer the mixed solution to a 40°C oil bath or water bath for heating, and at this time, the raw materials undergo a polymerization reaction, about 0.1 hours Afterwards, a white resinous mixture was obtained, which was heated to 60° C. and maintained for 6 hours, and then transferred to a 180° C. oven for solidification for 12 hours to obtain a tan solid; the tan solid was transferred to a carbonization furnace, and the temperature was raised to Carbonize at 500°C for 12 hours at a constant temperature, cool to room temperature; take out the carbonized solid product, boil it with dilute hydrochloric acid and di...

Embodiment 3

[0039] Take by weighing 47.5g of melamine, 15g of urea and 120g of 37% formaldehyde solution (weight ratio is 100:32:255), add 100g of water (175g of water in the mixture at this moment); adjust the pH value to 10.5 with ammonia water, stir and dissolve completely, Add 213g of calcium chloride (453 parts by weight), stir and dissolve, then adjust the pH to 5 with hydrochloric acid; transfer the mixed solution to an 80°C oil bath or water bath for heating, at this time, the raw materials undergo a polymerization reaction, and after about 0.5 hours, The white resinous mixture was heated to 90°C and kept for 0.1 hour, then transferred to a 220°C oven for solidification for 4 hours to obtain a white solid; the white solid was transferred to a carbonization furnace, and the temperature was raised to 800°C in flowing argon, Carbonize at constant temperature for 2 hours, cool to room temperature; take out the carbonized solid product, boil it with dilute hydrochloric acid and distille...

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Abstract

The invention discloses a method for preparing a high-surface-area nitrogenous mesoporous carbon material. The method prepares the nitrogenous mesoporous carbon material by using melamine, urea and formaldehyde as raw materials, using metal chloride as a template agent and an active agent, and performing the steps of dissolution, polymerization, solidification, carbonization, washing, drying and the like. The raw materials are rich in sources and have low prices; the metal chloride used as the template agent and the active agent has a low price and can be recycled; the whole preparation method is simple and feasible; and the prepared nitrogenous mesoporous carbon material has a specific area of 500 to 1,500 m<2> / g, a total pore volume of 1.0 to 3.0 cm<3> / g, a mesoporous ratio of 80 to 92 percent, an adjustable pore diameter of between 2.5 nm to a plurality of microns and the nitrogen content (atomic percent) of 5 to 28 percent at, and is expected to be widely applied in the fields of adsorbents, catalyst carriers, electrode materials and the like.

Description

technical field [0001] The present invention relates to a method for preparing a nitrogen-containing mesoporous carbon material with a high surface area, and more specifically relates to a process of dissolving, polymerizing, curing, The invention relates to a method for preparing a nitrogen-containing mesoporous carbon material through steps such as carbonization, water washing, and drying, and belongs to the field of porous and new carbon materials. Background technique [0002] Porous carbons have high specific surface area and well-developed pores, and are widely used as adsorbents, catalyst supports, electrode materials for batteries and supercapacitors, etc. The most common porous carbon material is activated carbon, which is widely used, but because activated carbon is mainly microporous, it is difficult to meet the increasing performance requirements. For example, in the field of capacitor materials, although microporous carbon has an ultra-high specific surface are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B31/08
Inventor 沈俭一黄玉安杨丰白志平
Owner NANJING UNIV
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