Carbon material preparation method

A carbon material and carbonization temperature technology, which is applied in the field of preparation of heteroatom-doped carbon materials, can solve the problems of difficulty in controlling the pore structure of carbon materials, low heating rate of carbonization by soft template method, and difficulty in obtaining mesoporous carbon materials. Narrow mesopore pore size distribution, improved hydrophilicity, and fewer steps

Inactive Publication Date: 2018-12-25
HUNAN UNIV
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  • Abstract
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Problems solved by technology

Commonly used templates include hard or soft templates. The hard template method requires multiple steps of synthesizing the template, introducing the precursor into the template, polymerizing, carbonizing, and removing the template, which is very time-consuming and requires the use of toxic hydrogen fluoride or highly corrosive strong alkali; and although the soft template method does not need to remove the template, it generally uses toxic and volatile formaldehyde, and the carbonization heating rate of the whole soft template method is very low
Therefore, although the hard template method or the soft template method can generally obtain carbon materials with a mesoporous structure, they are not suitable for large-scale preparation.
The activation method is similar to high-temperature carbonization, and generally needs to be used for strong alkali KOH or CO 2 and other gases, the whole process is complicated
At the same time, the activation method is generally difficult to control the pore structure of carbon materials, and it is difficult to obtain mesoporous carbon materials with narrow pore size distribution.
In addition, in order to achieve the doping of heteroatoms in carbon materials such as nitrogen or oxygen, it is often necessary to use special precursors or post-treatment methods (i.e., use NH 3 Or acetonitrile and other processed carbon materials that have been synthesized), not only the process is cumbersome, but also easy to destroy the structure of the carbon material, thereby affecting its performance

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preparation example Construction

[0028] The preparation method of the oxygen-doped carbon material provided by the present invention includes: 1) selection and preparation of the precursor: selecting a suitable precursor or synthesizing a special precursor; preparation of the oxygen-doped carbon material: 2) high-temperature carbonization: The precursor is placed in a crucible and covered with a crucible lid, and then placed in a muffle furnace. Under an air atmosphere, a heating program is set to raise the temperature to the carbonization temperature at a certain heating rate, and then cool down to the carbonization temperature after a certain period of time. After washing and drying at room temperature, the oxygen-doped carbon material is obtained.

[0029] During the entire preparation process, the relative ratio of the mass of the precursor to the volume of the crucible, the structure and type of the precursor, the heating rate of carbonization, the carbonization temperature and the holding time will affec...

Embodiment 1

[0032] This embodiment provides a method for preparing an oxygen-doped carbon material and the prepared oxygen-doped carbon material.

[0033] Weigh 2g of sulfuric acid-treated sucrose, place them in 15mL, 20mL, 30mL, and 50mL crucibles respectively, cover the crucible lids, put them into a muffle furnace, set the heating program: heat up to 900°C at a rate of 20°C / min, and They were respectively kept warm for 0 min, and were taken out after cooling, and a nitrogen-oxygen-doped mesoporous carbon material was obtained after grinding. The results showed that the yields of the obtained carbon materials were 43.1% (15mL crucible), 41.8% (20mL crucible), 40.2% (30mL crucible), 36.3% (50mL crucible).

Embodiment 2

[0035] This embodiment provides a nitrogen and oxygen doped mesoporous carbon material and a preparation method thereof.

[0036]Weigh 0.05 mol of p-phenylenediamine and dissolve in 30 mL of methanol, weigh 0.1 mol of sulfuric acid and dissolve in 50 mL of deionized water. In an ice-water bath, slowly drop the p-phenylenediamine methanol solution into the sulfuric acid solution, stir and react at room temperature for 1 hour, distill off the solvent under reduced pressure, and dry in vacuum to obtain the precursor p-phenylenediamine dihydrogensulfate. Put 2 g of p-phenylenediamine dihydrogensulfate obtained in a crucible, cover the crucible lid, put it into a muffle furnace, set the temperature rise program: raise the temperature to 900°C at a rate of 20°C / min, and keep warm for 0min, 30min, 60min, 90min, then lower the temperature to room temperature, take it out, and get a nitrogen-oxygen-doped mesoporous carbon material after grinding. According to different holding times, ...

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Abstract

The invention discloses a carbon material preparation method which is characterized in that a precursor is placed into a crucible or a container with a crucible function and covered with a crucible cover, the precursor and the crucible or the container are placed into a muffle furnace or a similar muffle furnace environment, the precursor is directly carbonized at high temperature, insulated for aperiod of time at the carbonization temperature, cooled to room temperature and finally washed and dried to obtain a needed carbon material. High-temperature carbonization is directly performed in air atmosphere in the muffle furnace, reaction conditions are easily controlled, severe conditions such as a tubular furnace and inert gases such as argon or nitrogen are omitted, the preparation methodis simple, fewer in steps, strong in operability, easy in amplification preparation and adaptable to large-scale industrial production. The nitrogen-oxygen doped mesoporous carbon material prepared by the method is high in specific surface area, large in pore volume, narrow in mesoporous size distribution, strong in hydrophily and stably dispersed in water.

Description

technical field [0001] The invention relates to the technical field of a carbon material, especially a preparation method of a heteroatom-doped carbon material. Background technique [0002] In recent years, carbon materials such as carbon nanotubes, carbon fibers, and graphene have attracted much attention due to their many advantages such as good chemical and thermal stability, high electronic conductivity, low density, and heteroatom doping, and are widely used in gas Adsorption and separation, water purification, oil-water separation, chromatographic analysis, sensing, chemical catalysis and electrochemical clean energy and other fields. Especially in the field of energy storage and conversion, carbon materials themselves can be used as electrode materials for capacitors, lithium-ion batteries, lithium-sulfur batteries, sodium / potassium-ion batteries, etc., and can also be used as electrocatalysts for oxygen reduction, oxygen evolution, and hydrogen evolution. , carbon ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
CPCC01B32/05Y02P20/54
Inventor 张世国张妍邢忱
Owner HUNAN UNIV
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