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A preparation method of millimeter-scale hierarchical porous carbon spheres

A multi-level pore, millimeter-scale technology, applied in the preparation/purification of carbon, can solve the problems of easy generation of environmental waste, difficult industrialization and application, difficult pore structure regulation, etc., and achieves easy industrial expansion of production and simple equipment requirements. , the effect of low cost

Active Publication Date: 2017-06-27
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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  • A preparation method of millimeter-scale hierarchical porous carbon spheres
  • A preparation method of millimeter-scale hierarchical porous carbon spheres
  • A preparation method of millimeter-scale hierarchical porous carbon spheres

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Experimental program
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Effect test

Embodiment 1

[0029] In the first step, accurately weigh 2.4g PVDF and 0.3g PVP, place them in a conical flask, add 12.5mL N,N-dimethylformamide, and stir mechanically 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 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 millimeter-scale hierarchical porous carbon spheres have a p...

Embodiment 2

[0032] Step 1: Accurately weigh 2.4g PES and 0.6g PVP, place them in a conical flask, add 12.2mL N,N-dimethylformamide, stir mechanically 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 a particle size...

Embodiment 3

[0034] In the first step, accurately weigh 2.4g PVDF and 0.3g PVP, place them in a conical flask, add 12.5mL N,N-dimethylformamide, and stir mechanically 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, and squeeze out the droplet to the 500mL 25% volume of isopropanol-75% volume of the solution directly below the needle of the syringe. Phase separation and gelation in deionized 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 ob...

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Abstract

The invention discloses a preparation method of millimeter-scale hierarchical porous carbon spheres. Using the non-solvent to phase separation method in the field of membrane separation to prepare polymer-based spherical activated carbon, replacing the ball formation of phenolic resin suspension polymerization; obtain a millimeter-scale spherical polymer-based precursor with a very narrow particle size distribution through the extrusion process of a syringe pump; A small amount of pore forming agent is added to form a developed pore structure; a small amount of phenolic resin is added to play a structural supporting role and maintain good sphericity and strength. The prepared porous carbon spheres have a rich pore structure and a high content of mesopores. The invention realizes the simple preparation of the millimeter-scale multi-level porous carbon sphere, and has the advantages of simple and controllable operation, low cost, easy industrialized expanded production, and the like. The prepared millimeter-scale hierarchical porous carbon spheres have broad application prospects in the fields of catalysis, separation, and environmental pollution remediation.

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 Patents(China)
IPC IPC(8): C01B32/05
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