Preparation method of millimeter-scale hierarchical pore carbon balls

A multi-level hole and millimeter-scale technology, applied in the field of material preparation, can solve the problems of difficult industrialization and application, easy production of environmental waste, and complicated preparation process, and achieve the effects of easy industrial expansion of production, low cost, and simple operation

Active Publication Date: 2015-12-23
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although many achievements have been made in the research of polymer-based spherical activated carbon, its preparation process is complicated, the control of pore structure is difficult, and it is easy to generate environmental waste, which is difficult to promote and apply in industrialization.

Method used

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  • Preparation method of millimeter-scale hierarchical pore carbon balls
  • Preparation method of millimeter-scale hierarchical pore carbon balls
  • Preparation method of millimeter-scale hierarchical pore carbon balls

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In the first step, accurately weigh 2.4g of PVDF and 0.3g of PVP, place them in a conical flask, add 12.5mL of N,N-dimethylformamide, and mechanically stir at 60°C until dissolved. In the second step, add 0.45g of phenolic resin and continue to stir until it dissolves evenly. In the third step, take 5mL of the above solution with a syringe and place it on the syringe pump, adjust the speed of the syringe pump to 0.5mL / min, squeeze out the droplet to 500mL of 5% volume isopropanol-95% volume deionized solution directly below the needle of the syringe Phase separation and gelation in water. In the fourth step, after 24 hours, the spherical polymer-based precursor is taken out and dried at room temperature. After drying, put it under a nitrogen atmosphere, raise the temperature to 900°C at a rate of 1°C / min, keep it for 3 hours, then cool it down to room temperature naturally, and take out the sample as a millimeter-scale hierarchical porous carbon sphere. The obtained m...

Embodiment 2

[0032] In the first step, accurately weigh 2.4g PES and 0.6g PVP, place them in a conical flask, add 12.2mL N,N-dimethylformamide, and mechanically stir at 60°C until dissolved. In the second step, add 0.45g of phenolic resin and continue to stir until it dissolves evenly. In the third step, take 5mL of the above solution with a syringe and place it on the syringe pump, adjust the speed of the syringe pump to 0.8mL / min, squeeze out the droplet to 500mL of 5% volume isopropanol-95% volume deionized Phase separation and gelation in water. In the fourth step, after 12 hours, the spherical polymer-based precursor is taken out and dried at room temperature. After drying, put it under a nitrogen atmosphere, raise the temperature to 600°C at a rate of 1°C / min, keep it for 3 hours, and then cool it down to room temperature naturally, and take out the sample as a millimeter-scale hierarchical porous carbon sphere. The obtained millimeter-scale hierarchical porous carbon spheres have ...

Embodiment 3

[0034] In the first step, accurately weigh 2.4g of PVDF and 0.3g of PVP, place them in a conical flask, add 12.5mL of N,N-dimethylformamide, and mechanically stir at 60°C until dissolved. In the second step, add 0.45g of phenolic resin and continue to stir until it dissolves evenly. In the third step, take 5mL of the above solution with a syringe and place it on the syringe pump, adjust the speed of the syringe pump to 1.0mL / min, squeeze out the droplet to 500mL of 25% volume isopropanol-75% volume deionized solution directly below the needle of the syringe Phase separation and gelation in water. In the fourth step, after 48 hours, the spherical polymer-based precursor is taken out and dried at room temperature. After drying, put it under a nitrogen atmosphere, raise the temperature to 900°C at a rate of 1°C / min, keep it for 3 hours, then cool it down to room temperature naturally, and take out the sample as a millimeter-scale hierarchical porous carbon sphere. The obtained ...

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Abstract

The invention discloses a preparation method of millimeter-scale hierarchical pore carbon balls. Macromolecule-based spherical activated carbon is prepared with a nonsolvent induced phase separation method in a membrane separation field, and balling obtained through suspension polymerization of phenolic resin is replaced; millimeter-scale spherical macromolecule-based precursors with very narrow particle size distribution are obtained through an injection pump extrusion process; a few of added pore forming agents form a rich pore structure; a little of added phenolic resin has a structure support action, and excellent sphericity degree and strength are kept; the prepared porous carbon balls have rich pore structures and high mesoporous content. The millimeter-scale hierarchical pore carbon balls are simple to prepare, and the preparation method has the advantages of simplicity and controllability in operation, low cost, easiness in industrial production expansion and the like; the prepared millimeter-scale hierarchical pore carbon balls have wide application prospect in the fields of catalysis, separation, restoring of polluted environment and the like.

Description

technical field [0001] The invention belongs to the preparation method of millimeter-scale hierarchical porous carbon spheres in the field of material preparation. Background technique [0002] Activated carbon is an important porous functional material, which is widely used in the fields of adsorption, decolorization, purification, separation, and catalysis in liquid and gas phases due to its rich pore structure, high specific surface area, good electrical conductivity, and chemical stability. , It is of great significance in food, medicine, chemical industry, environmental protection and other aspects. There are many activated carbon precursors, which are mainly divided into two categories: one is natural substances, including lignin, coconut shells, walnut shells, corn cobs, bamboo, petroleum pitch, coal, etc.; the other is synthetic materials, including phenolic resins, Polyacrylonitrile, cellulose, furfural, polyimide, etc. The former has abundant sources and low pric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 李健生齐俊文方小峰李阳王连军孙秀云沈锦优韩卫清刘晓东
Owner NANJING UNIV OF SCI & TECH
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