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Preparation method of microporous carbon material

A technology of microporous carbon and phenolic compounds, applied in the field of preparation of microporous carbon materials, can solve the problems of high technical difficulty, poor safety performance, and high equipment requirements, and achieve the effects of simple conditions, convenient operation and abundant pores.

Inactive Publication Date: 2013-03-13
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods generally require a hydrothermal treatment process, but the hydrothermal method has disadvantages such as high equipment requirements, high technical difficulty, and poor safety performance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Measure according to the mass ratio of phenol: formaldehyde solution: water: sodium carbonate = 1:4:60:0.01, mix well, react at 85°C for 45min, and then cool to room temperature to obtain a phenolic prepolymer solution. Then measure according to the mass ratio of tartaric acid: zinc chloride: hydrochloric acid: water = 1:0.4:5:25, and mix evenly to obtain a mixed solution. Measure the mixed solution: the mass ratio of phenolic prepolymer solution = 1:2, add the mixed solution into the phenolic prepolymer solution, mix well, and polymerize at 85°C for 2 days, cool to room temperature after the reaction, and use the product Washed twice with methanol, and then dried at 40 °C for 24 h to obtain a blocky solid. In a tube furnace under the protection of nitrogen, the block solid is heated to 900°C for carbonization at a heating rate of 0.5°C / min, and finally cooled down to room temperature naturally to obtain a microporous carbon material. It has been determined that the ob...

Embodiment 2

[0021] Measure according to the mass ratio of resorcinol:formaldehyde solution:water:sodium carbonate=1:7.5:90:0.015, mix well, react at 85°C for 120min, then cool to room temperature to obtain phenolic prepolymer solution. Then measure according to the mass ratio of citric acid: zinc chloride: hydrochloric acid: water = 1:3:7.5:15, and mix evenly to obtain a mixed solution. Measure the mixed solution: the mass ratio of phenolic prepolymer solution = 1:6, add the mixed solution into the phenolic prepolymer solution, mix well, react and polymerize at 85°C for 4 days, cool to room temperature after the reaction, and use the product After washing with ethanol for 5 times, it was dried at 100°C for 2 h to obtain a blocky solid. In a tube furnace, protected by argon, the block solid is heated to 1000°C for carbonization at a heating rate of 10°C / min, and finally cooled down to room temperature naturally to obtain a microporous carbon material. It has been determined that the obtai...

Embodiment 3

[0023] Measure according to the mass ratio of phloroglucinol:formaldehyde solution:water:sodium carbonate=1:5:75:0.012, mix well, react at 85°C for 60min, and then cool to room temperature to obtain a phenolic prepolymer solution. Then measure according to the mass ratio of tartaric acid: zinc chloride: hydrochloric acid: water = 1:1.5:6:20, and mix evenly to obtain a mixed solution. Measure the mixed solution: the mass ratio of phenolic prepolymer solution = 1:3, add the mixed solution into the phenolic prepolymer solution, mix well, polymerize at 85°C for 3 days, cool to room temperature after the reaction, and use the product After washing with acetone for 3 times, it was dried at 80°C for 12 hours to obtain a blocky solid. In a tube furnace, under the protection of helium, the block solid is heated to 950°C for carbonization at a heating rate of 5°C / min, and finally the temperature is naturally cooled to room temperature to obtain a microporous carbon material. It has bee...

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Abstract

The invention relates to a preparation method of a microporous carbon material. The method comprises the steps of; weighing a phenolic compound,a formaldehyde solution, water and sodium carbonate in a weight ratio of 1:4-7.5:60-90:0.01-0.015, mixing, reacting at 85 DEG C for 45-120 min, and then cooling to room temperature to obtain a phenolic prepolymer solution; then weighing polyhydroxy acid, zinc chloride, hydrochloric acid and water in a weight ratio of 1:0.4-3:5-7.5:15-25, and mixing to obtain a mixed solution; weighing the mixed solution and the phenolic prepolymer solution in a weight ratio of 1:2-6, adding the mixed solution into the phenolic prepolymer solution, mixing evenly, conducting a polymerization reaction at 85 DEG C for 2-4 days, cooling to room temperature after the reaction, washing the products with a solvent with low surface tension for 2-5 times, and then drying at 40-100 DEG C for 2-24 h to obtain solid blocks; heating the solid blocks to 900-1000 DEG C for carbonization, with heating rate of 0.5-10 DEG C / min in a tube furnace under protection of inert gas; and finally naturally cooling to a room temperature to obtain the microporous carbon material. According to tests, the obtained microporous carbon material has regular microporous structure and specific surface area higher than 1000m<2> / g.

Description

technical field [0001] The invention relates to a preparation method of a microporous carbon material. Specifically, it refers to the use of the metal coordination between the polyhydroxy acid and the zinc ion, and the hydrogen bond interaction between the hydroxyl group in the phenolic compound and the hydroxyl group in the polyhydroxy acid to uniformly introduce the polyhydroxy acid zinc into the phenolic compound. In the polymer skeleton structure, the method of preparing microporous carbon materials by final carbonization treatment. Background technique [0002] Microporous carbon materials have very broad and very important application prospects in the fields of adsorption and separation, catalyst supports, electrode materials, etc. due to their high specific surface area and good chemical stability. For example, "Preparation method of activated carbon with high adsorption performance" (Chinese invention patent, patent number: 02157271.2), "Method for preparing alcohol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02C01B32/05
Inventor 刘明贤钱佳晟甘礼华
Owner TONGJI UNIV
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