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Preparation method of graded porous carbon

A technology of hierarchical porous and foaming agent, applied in carbon preparation/purification, etc., can solve the problems of accelerated desalination speed, low ion diffusion resistance, small specific surface area of ​​mesoporous carbon, etc., and achieve the effect of improving uniformity

Pending Publication Date: 2020-06-16
ZHENGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] When porous carbon is used in capacitive desalination and other fields, its microporous carbon can provide a large specific surface area, which is beneficial to increase the amount of desalination, but the micropore diameter is small (the pore diameter is less than 2nm), which is not conducive to the transmission of ions; the mesoporous carbon has a large pore diameter (The pore size is 2-50nm), the ion diffusion resistance is small, which is conducive to rapid desalination, and its surface area utilization rate is high, but the specific surface area of ​​mesoporous carbon is small, and the desalination amount is limited; the specific surface area of ​​macroporous carbon (pore size greater than 50nm) is very small. Limited, unable to contribute to desalination, but large pores will reduce the ion transmission path and speed up desalination

Method used

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  • Preparation method of graded porous carbon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 0.1g of potassium carbonate powder with a particle size of 1000 mesh to 10g of low-temperature coal tar pitch, grind it evenly, put it into the reaction kettle under nitrogen, the pressure in the kettle is 1.0Mpa, and heat it to 80℃ at a speed of 5℃ / min. Constant temperature magnetic stirring for 30min, then heating to 340°C at a speed of 5°C / min, reacting for 1h, then heating to 850°C at a speed of 20°C / min, reacting for 1h, cooling down to room temperature naturally, taking it out and putting in 1M Soak in hydrochloric acid for 6 hours, wash with water until nearly neutral, and dry to obtain a specific surface area of ​​500m 2 / g, the pore volume is 0.45cm 3 / g, the average pore diameter of micropores is 0.78nm, the average pore diameter of mesopores is 2.9nm, there are 70-100nm macropores, and the total average pore diameter is 2.1nm hierarchical porous carbon.

Embodiment 2

[0030] Add 10g of potassium carbonate powder with a particle size of 200 mesh to 10g of medium-temperature coal tar pitch, grind it evenly, put it into a reaction kettle under nitrogen, and heat it to 100℃ at a speed of 20℃ / min at a constant temperature of 5.0Mpa. Stir mechanically for 24 hours, then heat up to 340°C at a rate of 10°C / min, react for 1 hour, then heat up to 900°C at a rate of 30°C / min, react for 2 hours, cool down to room temperature naturally, take it out and put in 1M hydrochloric acid Soak in neutral water for 6 hours, wash with water until nearly neutral, and dry to obtain a specific surface area of ​​1200m 2 / g, the pore volume is 0.75cm 3 / g, the average pore diameter of micropores is 0.9nm, the average pore diameter of mesopores is 3.8nm, there are 80-120nm macropores, and the total average pore diameter is 2.9nm.

Embodiment 3

[0032] Add 100g of potassium citrate powder with a particle size of 100 mesh to 10g of high-temperature coal tar pitch, grind it evenly, put it into a reaction kettle under argon, and heat it to 150℃ at a speed of 0.1℃ / min at a pressure of 0.1Mpa. , ultrasonic at constant temperature for 5 hours, then heated to 250°C at a speed of 50°C / min, reacted for 1h, then heated to 700°C at a speed of 5°C / min, reacted for 1h, cooled down to room temperature naturally, took it out and put in 1M Soak in hydrochloric acid for 8 hours, wash with water until nearly neutral, and dry to obtain a specific surface area of ​​1500m 2 / g, the pore volume is 1.50cm 3 / g, the micropore average aperture is 0.78nm, the mesopore average aperture is 6.7nm, there are 300-1100nm macropores, and the total average aperture is the hierarchical porous carbon of 4.5nm (such as figure 1 shown).

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Abstract

The invention discloses a preparation method of graded porous carbon. According to the technical scheme, the preparation method comprises the steps: firstly, adding a foaming agent into a low-melting-point solid carbon-containing substance, and mixing for later use; then under a certain pressure and atmosphere, heating to a temperature T1, and homogenizing for t1; and under a certain pressure andatmosphere, heating to a temperature T2, carrying out a reaction for t2, heating to a temperature T3, carrying out a reaction for t3, cooling to room temperature, cleaning and drying to obtain the graded porous carbon. The basic concept of the invention comprises that a macroporous structure is formed by a foaming technology, the porosity of the carbon material is further increased by utilizing generated reducing gas, and then more micropores and small mesopores are generated by utilizing cracking and intercalation of anode ions under heat treatment to form porous carbon with a micropore-mesopore-macroporous hierarchical pore structure. The method has the advantages of being high in operability, large in aperture adjusting range, accurate in regulation and control and the like.

Description

technical field [0001] The invention relates to a method for preparing hierarchical porous carbon, which belongs to the field of carbon material preparation. Background technique [0002] Due to the characteristics of good thermal stability, high mechanical stability, excellent electrical conductivity, well-developed pore structure, and large specific surface area, porous carbon materials have shown great application potential in the fields of adsorption, separation, catalysis, gas storage, and energy storage and conversion. . Especially in the field of energy storage and conversion, porous carbon materials can play an important role as active materials, conductive agents, coating layers, flexible substrates, carriers, etc. [0003] When porous carbon is used in capacitive desalination and other fields, its microporous carbon can provide a large specific surface area, which is beneficial to increase the amount of desalination, but the micropore diameter is small (the pore d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
CPCC01B32/05
Inventor 高彪峰陈垒张志华郭恒陈喜平陈静波杨建红何季麟
Owner ZHENGZHOU UNIV
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