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Preparation method for heteratom-containing ordered mesoporous carbon with high specific capacitance

A technology with high specific capacitance and heteroatoms, which is applied in the field of mesoporous carbon preparation, can solve the problems of difficult control of the physical structure and surface chemical structure of mesoporous carbon, low specific surface area of ​​mesoporous carbon, and long synthesis cycle, etc. Large-scale production, high specific capacitance, and simple operation

Inactive Publication Date: 2012-08-01
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the specific surface area of ​​the mesoporous carbon prepared by these methods is low or the inorganic template needs to be prepared first, the process is complicated, the synthesis cycle is long, the product cost is high, and the physical structure and surface chemical structure of the synthesized mesoporous carbon are not easy to control

Method used

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  • Preparation method for heteratom-containing ordered mesoporous carbon with high specific capacitance
  • Preparation method for heteratom-containing ordered mesoporous carbon with high specific capacitance

Examples

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Effect test

Embodiment 1

[0031] Melt 4.2g of phenol and add 30wt% Na 2 CO 3 0.5g aqueous solution, stirred for 10min, added 5.0g of 37wt% formaldehyde aqueous solution, reacted at 72°C for 30min, added 0.3g of ammonium phosphate, and continued to react for 40min. Adjust the pH of the solution to 7, and dehydrate under reduced pressure for 1 h. The resulting resin was dissolved in tetrahydrofuran.

[0032] Dissolve 1.0g of F127 in tetrahydrofuran, add 0.9g of silica sol and stir for 2h, then add 4.0g of tetrahydrofuran solution of phosphorus-containing phenolic resin, stir for 10min, transfer to a petri dish to evaporate the solvent for 6h, and solidify at 100°C for 48h. Carbonization at 900°C for 1h under an inert atmosphere. The carbonized sample was treated with hydrofluoric acid to remove silicon, washed and dried to obtain phosphorus-containing ordered mesoporous carbon, and the properties of mesoporous carbon are shown in Table 1.

Embodiment 2

[0034] Melt 8.5g of phenol, add 2.6g of 20wt% NaOH aqueous solution, stir for 30min, add 9.0g of 37wt% formaldehyde aqueous solution, react at 78°C for 20min, add 0.8g of phosphoric acid, and continue the reaction for 60min. Adjust the pH value of the solution to 9, and distill under reduced pressure for 2 h. The resulting resin was dissolved in ethanol.

[0035] Dissolve 1.8g of HD2018 in ethanol, add 2.0g of TEOS and stir for 1h, then add 5.0g of ethanol solution of phosphorus-containing phenolic resin, stir for 30min, transfer to a petri dish to evaporate the solvent for 8h, and solidify at 120°C for 18h. Carbonization at 800°C for 3h under an inert atmosphere. The carbonized sample was treated with 30wt% NaOH solution to remove silicon, and after washing and drying, ordered mesoporous carbon containing phosphorus was obtained. The properties of mesoporous carbon are shown in Table 1.

Embodiment 3

[0037] Melt 5.8g of phenol, add 0.4g of concentrated ammonia water, stir for 20min, add 4.5g of 37wt% formaldehyde solution, react at 85°C for 40min, add 0.8g of melamine, and continue to react for 20min. Adjust the pH value of the solution to 8, and distill under reduced pressure for 1 h. The resulting resin was dissolved in ethanol.

[0038] Dissolve 1.5g of P123 in ethanol, add 1.5g of TEOS and stir for 1.5h, then add 5.0g of ethanol solution of nitrogen-containing phenolic resin, stir for 40min, transfer to a petri dish to evaporate the solvent for 10h, and solidify at 150°C for 12h. Carbonization at 1100°C for 0.5h under an inert atmosphere. The carbonized sample was treated with 35wt% NaOH solution to remove silicon, washed and dried to obtain nitrogen-containing ordered mesoporous carbon. The properties of mesoporous carbon are shown in Table 1.

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Abstract

The invention relates to a preparation method for heteratom-containing ordered mesoporous carbon with high specific capacitance. The method comprises: melting phenol; adding a catalyst; uniformly stirring, and adding an aqueous solution of formaldehyde; carrying out a reaction for 10-60 minutes at a temperature of 65-90 DEG C; adding a heteroatom compound; continuously carrying out the reaction for 10-60 minutes, and stopping the stirring; adjusting the pH value of the solution to more than or equal to 7.0; carrying out decompression dehydration to obtain a resin; dissolving the resulting resin in an organic solvent to obtain a uniformly heteratom-containing phenol formaldehyde resin solution; dissolving a block copolymer in a solvent to form a uniform solution; adding an oligomer of silicon to the resulting uniform solution, and stirring for 0.5-4 hours; then adding the resulting solution to the heteratom-containing phenol formaldehyde resin solution; uniformly stirring, and volatilizing the solvent for 6-18 hours; curing for 6-48 hours; carrying out carbonization for 0.1-3 hours at a temperature of 600-1200 DEG C under inert atmosphere; adopting hydrofluoric acid or a concentrated alkali solution to treat the carbonized sample, removing the silicon, washing and drying to obtain the heteratom-containing ordered mesoporous carbon. The method of the present invention has advantages of simple process and low cost, and the produced carbon has high specific capacitance.

Description

technical field [0001] The invention belongs to a preparation method of mesoporous carbon, in particular to a preparation method of ordered mesoporous carbon containing heteroatoms with high specific capacitance. technical background [0002] Supercapacitors have attracted extensive attention due to their high energy density, fast charge-discharge rate, and long cycle life, which can be used in many fields. The key factor affecting the performance of supercapacitors is the electrode material. Ordered mesoporous carbon has a high specific surface area and a suitable pore structure, which can still meet the rapid migration of electrolyte ions under the condition of high current charge and discharge, and maintain a good charge. Chemical properties, so it is often used as a supercapacitor electrode material. However, the specific capacitance of pure ordered mesoporous carbons is low, and only electric double layer capacitance exists. [0003] The introduction of certain hetero...

Claims

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Application Information

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IPC IPC(8): C01B31/02H01G9/042C01B32/05
Inventor 宋燕翟晓玲智林杰史景利郭全贵
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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