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Preparation method of nitrogen-rich porous wood-based carbon material

A carbon material and wood technology, which is applied in the field of preparation of nitrogen-rich porous wood-based carbon materials, can solve the problems of many reaction steps, increased reaction cycle, unfriendly environment, etc., and achieves the effects of simple operation and high yield

Inactive Publication Date: 2019-05-17
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction requires the use of a large amount of resorcinol, formaldehyde, and guanidine carbonate. At the same time, there are many reaction steps, such as stirring, freeze-drying, activation treatment, carbonization, washing, and drying, which increases the reaction cycle.
[0008] In summary, the traditional methods for preparing nitrogen-rich porous carbon materials include template carbonization method, solvent evaporation self-assembly method, ice and silica double template method, mixing, molding, carbonization and water vapor activation followed by mixed acid oxidation and acetic acid Ferrous reduction method, the reaction process is often cumbersome and lengthy, and the raw materials involve azodicarbonamide, water-soluble phenolic resin, and guanine. Although the product has excellent performance, the unfriendly environment limits the practical application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0019] Use poplar bark as raw material, grind and screen wood flour of 40-80 meshes, Soxhlet extraction for 2 hours, mix well with melamine as nitrogen source at a ratio of 3:1, and heat up at 7°C / min under nitrogen atmosphere The temperature was raised to 550°C at a constant temperature for 2 hours for pre-carbonization. The obtained pre-carbonized product was mixed with KOH at a ratio of 1:4, then put into a ball mill jar, and ball milled at a speed of 500r / min for 2h. The ball-milled product was raised to 900°C at a heating rate of 5°C / min, activated at high temperature for 2 hours to obtain the target product, washed with deionized water and 1M HCl to neutrality, and dried at 80°C to obtain nitrogen-rich porous Wood-based carbon materials.

[0020] The wood-based carbon material obtained by this method has a yield of 66.80%, has a developed pore structure, and a specific surface area of ​​1356.82m 2 / g, the pore volume is 0.82cm 3 / g, the nitrogen content is 8.6%.

experiment example 2

[0022] Using straw as raw material, after grinding, sifting wood flour of 60-100 mesh, Soxhlet extraction for 2 hours, mixed fully with urea as nitrogen source at a ratio of 5:1, under nitrogen atmosphere, at a heating rate of 7°C / min Raise the temperature to 600°C and keep the temperature for 1h for pre-carbonization. The obtained pre-carbonized product was mixed with NaOH at a ratio of 1:2, then put into a ball mill jar, and ball milled at a speed of 700r / min for 3h. The ball-milled product was raised to 950°C at a heating rate of 5°C / min, activated at high temperature for 2 hours to obtain the target product, washed with deionized water and 1M HCl to neutrality, and dried at 80°C to obtain nitrogen-rich porous Wood-based carbon materials.

[0023] The wood-based carbon material obtained by this method has a yield of 62.13%, has a developed pore structure, and a specific surface area of ​​963.58m 2 / g, the pore volume is 0.72cm 3 / g, the nitrogen content is 9.1%.

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Abstract

The invention provides a preparation method of a nitrogen-rich porous wood-based carbon material. The method is characterized in that waste biomass resources of bark, straws, food residues and the like are used as raw materials; a solvent-free treatment method of pre-carbonization-ball milling-carbonization is used for preparing the nitrogen-rich porous wood-based carbon material. Firstly, the rawmaterials are subjected to grinding, sieving and extraction; the obtained treated raw materials are mixed with a certain quantity of nitrogen sources; pre-carbonization is firstly performed; productsafter the pre-carbonization are mixed with a certain amount of alkali; next, the materials are put into a ball milling machine for ball milling. The product after the ball milling is activated at different temperatures; obtained solid carbon products are washed by dilute hydrochloric acid and deionized water to the neutral state and are put into a drying box to be dried, and the nitrogen-rich porous wood-based carbon material with high-activity center and developed pore structures can be obtained. The operation process provided by the invention has the main characteristics that the pre-carbonization-ball milling-carbonization solvent-free treatment method is used; the waste biomass resources are used and are converted into functional carbon materials with high added values.

Description

Technical field: [0001] The invention relates to a preparation method of a nitrogen-rich porous wood-based carbon material Background technique: [0002] my country is rich in biomass resources, with crop straw and forestry logging and processing residues alone exceeding 1 billion tons per year. Among them, there are about 100 million tons of forestry logging residues and processing residues that can be collected and utilized. The amount of agricultural straw that can be collected is more than that of forestry residues. The total amount of agricultural and forestry residues that can be collected is about 200 million tons. How to effectively use agricultural and forestry waste Obtaining high value-added materials has become a research hotspot. Biomass-based porous carbon materials have many advantages such as developed specific surface area, good electrical conductivity, corrosion resistance, low cost, and environmental friendliness. They have received extensive attention an...

Claims

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Application Information

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IPC IPC(8): C01B32/324C01B32/348
Inventor 吴琼于世涛胡锦秋曹双双李露刘仕伟
Owner QINGDAO UNIV OF SCI & TECH