CN108821279A - Preparation method of three-dimensional porous carbon - Google Patents

Preparation method of three-dimensional porous carbon Download PDF

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Publication number
CN108821279A
CN108821279A CN201810943090.6A CN201810943090A CN108821279A CN 108821279 A CN108821279 A CN 108821279A CN 201810943090 A CN201810943090 A CN 201810943090A CN 108821279 A CN108821279 A CN 108821279A
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porous carbon
dimensional porous
preparation
room temperature
self
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CN108821279B (en
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陶呈安
肖涵波
王芳
王建方
李玉姣
阳绪衡
宋琛超
陈瑞
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National University of Defense Technology
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National University of Defense Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/318—Preparation characterised by the starting materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/312—Preparation
    • C01B32/342—Preparation characterised by non-gaseous activating agents
    • C01B32/348—Metallic compounds

Abstract

The invention discloses a preparation method of a three-dimensional porous carbon, which comprises the steps of uniformly mixing a sugar source, dopamine and ammonium chloride, raising the temperature of the obtained mixture from room temperature to 250-300 ℃ under the protection of inert atmosphere, then raising the temperature to 800-1200 ℃ at an accelerated speed, sintering at a constant temperature for 2-6 h, and cooling to room temperature to obtain the self-supporting three-dimensional porous carbon. The preparation method only needs one-step pyrolysis and does not need any additional step, and the specific surface area can be up to 2700m2Self-supporting three-dimensional porous carbon per gram.

Description

A kind of preparation method of three-dimensional porous carbon
Technical field
The invention belongs to field of porous materials, are related to a kind of preparation method of three-dimensional porous carbon, and in particular to a kind of high ratio The preparation method of the three-dimensional porous carbon of surface area self-supporting.
Background technique
The three-dimensional porous carbon material of self-supporting is because it is with cellular structure abundant, high-specific surface area, preferable electric conductivity Etc. characteristics have a wide range of applications it in fields such as catalysis, the energy, environment.In order to make it play a role to the maximum extent, make The three-dimensional porous carbon of standby high-specific surface area out always is the direction that people make great efforts.The preparation of the three-dimensional porous carbon of self-supporting at present Method can substantially be divided into four major class：First is that the self-assembly method of graphene oxide, including it is hydro-thermal process method, freeze-drying, true Empty volatility process and drop-coating etc., second is that chemical vapour deposition technique, third is that carbon matrix precursor air blowing conversion method, fourth is that foam of polymers Carbonizatin method.But that there is steps is more for these methods, method is complicated, it is difficult to which a large amount of preparations, products therefrom specific surface area are inadequate Height (generally less than 2000m2/ g), it is also necessary to it is additional to use acid (H3PO4) or alkali (KOH) activate the problems such as.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, a kind of high-specific surface area self-supporting is provided The preparation method of three-dimensional porous carbon, this method only need a step be pyrolyzed, should not any additional step, specific surface area height can be obtained Up to 2700m2The three-dimensional porous carbon of the self-supporting of/g.
In order to solve the above technical problems, the present invention uses following technical scheme.
A kind of preparation method of three-dimensional porous carbon, includes the following steps：
Sugar source, dopamine and ammonium chloride are uniformly mixed, by gained mixture under the protection of inert atmosphere, first by room temperature 250 DEG C~300 DEG C are increased to, then accelerated warming is cooled to room temperature, obtains to 800 DEG C~1200 DEG C, then Isothermal sinter 2h~6h To the three-dimensional porous carbon of self-supporting.
In the preparation method of above-mentioned three-dimensional porous carbon, it is preferred that the mass ratio of the sugar source and dopamine is 4~100: 1。
In the preparation method of above-mentioned three-dimensional porous carbon, it is preferred that the gross mass and ammonium chloride of the sugar source and dopamine Mass ratio be 0.2~5: 1.
In the preparation method of above-mentioned three-dimensional porous carbon, it is preferred that when the room temperature is increased to 250 DEG C~300 DEG C, heating Rate is 1 DEG C/min~10 DEG C/min, keeps the temperature 0~3h.
In the preparation method of above-mentioned three-dimensional porous carbon, it is preferred that the accelerated warming stage, heating rate be 2 DEG C/ Min~15 DEG C/min, and the heating rate in the stage is greater than the heating rate when room temperature is increased to 250 DEG C~300 DEG C.
In the preparation method of above-mentioned three-dimensional porous carbon, it is preferred that the sugar source includes glucose, fructose, sucrose and wheat One of bud sugar is a variety of.
In the preparation method of above-mentioned three-dimensional porous carbon, it is preferred that the inert atmosphere is nitrogen.
Compared with the prior art, the advantages of the present invention are as follows：
(1) the three-dimensional porous carbon for the self-supporting that the present invention obtains has very high specific surface area, in condition of the invention Under, it can reach 2700m2/ g even more than, the existing obtained product of sugar foaming only has more than 1000 m2/g。
(2) preparation method of the invention does not need any pre-treatment or post-processing step, is by the method that a step heats The three-dimensional porous carbon of the self-supporting of high-specific surface area can be obtained.
(3) present invention does not need to carry out activating using the strong acid such as phosphoric acid or potassium hydroxide alkaline matter that Gao Bibiao can be obtained The three-dimensional porous carbon of the self-supporting of area, avoids subsequent purification step, has both reduced loss to instrument and to product Pollution, also simplifies processing step.
Detailed description of the invention
Fig. 1 is the optical photograph of three-dimensional porous carbon prepared by the embodiment of the present invention 1.
Fig. 2 is the stereoscan photograph of three-dimensional porous carbon prepared by the embodiment of the present invention 1.
Fig. 3 is the nitrogen adsorption desorption curve of three-dimensional porous carbon prepared by the embodiment of the present invention 1.
Fig. 4 is the optical photograph of three-dimensional porous carbon prepared by the embodiment of the present invention 2.
Fig. 5 is the stereoscan photograph of three-dimensional porous carbon prepared by the embodiment of the present invention 2.
Fig. 6 is the nitrogen adsorption desorption curve of three-dimensional porous carbon prepared by the embodiment of the present invention 2.
Fig. 7 is the optical photograph of three-dimensional porous carbon prepared by the embodiment of the present invention 3.
Fig. 8 is the stereoscan photograph of three-dimensional porous carbon prepared by the embodiment of the present invention 3.
Fig. 9 is the nitrogen adsorption desorption curve of three-dimensional porous carbon prepared by the embodiment of the present invention 3.
Figure 10 is the stereoscan photograph of three-dimensional porous carbon prepared by comparative example 1.
Figure 11 is the nitrogen adsorption desorption curve of three-dimensional porous carbon prepared by comparative example 1.
Specific embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and It limits the scope of the invention.
Material employed in following embodiment and instrument are commercially available.
A kind of preparation method of three-dimensional porous carbon of the invention, includes the following steps：
Sugar source, dopamine and ammonium chloride are uniformly mixed, by gained mixture under the protection of inert atmosphere, first by room temperature 250 DEG C~300 DEG C are increased to, then accelerated warming is cooled to room temperature, obtains to 800 DEG C~1200 DEG C, then Isothermal sinter 2h~6h To the three-dimensional porous carbon of self-supporting.
In above-mentioned preparation method, the mass ratio of sugar source and dopamine is 4~100: 1 (i.e. 99: 1~80: 20), sugar source and more The gross mass of bar amine and the mass ratio of ammonium chloride are 0.2~5: 1 (i.e. 1: 5~5: 1).
In above-mentioned preparation method, when room temperature is increased to 250 DEG C~300 DEG C, heating rate is 1 DEG C/min~10 DEG C/min, Keep the temperature 0~3h；Accelerate to continue the temperature rise period, heating rate is 2 DEG C/min~15 DEG C/min, and the heating rate in the stage is greater than Room temperature is increased to heating rate at 250 DEG C~300 DEG C.
In above-mentioned preparation method, sugar source includes one of glucose, fructose, sucrose and maltose or a variety of.
In above-mentioned preparation method, inert atmosphere is preferably nitrogen.
Embodiment 1：
A kind of preparation method of three-dimensional porous carbon of the invention, includes the following steps：
Glucose 2g, dopamine 0.1g and ammonium chloride 2g are uniformly mixed, gained mixture is placed in tube furnace, in nitrogen Under the conditions of gas shielded, 250 DEG C first are increased to 2 DEG C/min by room temperature, then continues to rise to 1000 DEG C with 4 DEG C/min, constant temperature 3 Hour, then cooled to room temperature, the three-dimensional porous carbon of self-supporting can be obtained.
The three-dimensional porous carbon of self-supporting manufactured in the present embodiment is characterized, Fig. 1 is the optical photograph of three-dimensional porous carbon, Fig. 2 is stereoscan photograph, it can be seen that sample surfaces have many cellular structures, and Fig. 3 is the nitrogen adsorption desorption curve of sample, BET specific surface area is 2600m2/g。
Embodiment 2：
A kind of preparation method of three-dimensional porous carbon of the invention, includes the following steps：
Glucose 2g, dopamine 0.02g and ammonium chloride 2g are uniformly mixed, gained mixture is placed in tube furnace, Under the conditions of nitrogen protection, 250 DEG C first are increased to 2 DEG C/min by room temperature, 2 hours is kept the temperature, then continues to be warming up to 8 DEG C/min 1000 DEG C, constant temperature 3 hours, then cooled to room temperature, the three-dimensional porous carbon of self-supporting can be obtained.
The three-dimensional porous carbon of self-supporting manufactured in the present embodiment is characterized, Fig. 4 is the three-dimensional porous carbon of self-supporting Optical photograph, Fig. 5 are stereoscan photograph, it can be seen that there are many cellular structures on surface, and Fig. 6 is that the nitrogen adsorption of sample desorbs Curve, BET specific surface area 2700m2/g。
Embodiment 3：
A kind of preparation method of three-dimensional porous carbon of the invention, includes the following steps：
Glucose 2g, dopamine 0.2g and ammonium chloride 2g are uniformly mixed, gained mixture is placed in tube furnace, in nitrogen Under the conditions of gas shielded, 250 DEG C first are increased to 4 DEG C/min by room temperature, then continues to be warming up to 1000 DEG C with 10 DEG C/min, constant temperature 3 hours, then cooled to room temperature, can be obtained the three-dimensional porous carbon of self-supporting.
The three-dimensional porous carbon of self-supporting manufactured in the present embodiment is characterized, Fig. 7 is the three-dimensional porous carbon of self-supporting Optical photograph, Fig. 8 are stereoscan photograph, it can be seen that there are many cellular structures on surface, and Fig. 9 is that the nitrogen adsorption of sample desorbs Curve, BET specific surface area 2300m2/g。
Comparative example 1：
A method of three-dimensional porous carbon being prepared, preparation process is substantially the same manner as Example 1, and difference is only that：It does not add Dopamine is only handled uniformly mixed be placed in tube furnace of glucose and ammonium chloride.Figure 10 is stereoscan photograph, can be with See that surface cellular structure is less, Figure 11 is the nitrogen adsorption desorption curve of sample, its BET specific surface area of the three-dimensional porous carbon of gained Only 1000m2/g。
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form.Though So the present invention is disclosed as above with preferred embodiment, and however, it is not intended to limit the invention.It is any to be familiar with those skilled in the art Member, in the case where not departing from Spirit Essence of the invention and technical solution, all using in the methods and techniques of the disclosure above Appearance makes many possible changes and modifications or equivalent example modified to equivalent change to technical solution of the present invention.Therefore, Anything that does not depart from the technical scheme of the invention are made to the above embodiment any simple according to the technical essence of the invention Modification, equivalent replacement, equivalence changes and modification, all of which are still within the scope of protection of the technical scheme of the invention.

Claims (7)

1. a kind of preparation method of three-dimensional porous carbon, which is characterized in that include the following steps：
Sugar source, dopamine and ammonium chloride are uniformly mixed, by gained mixture under the protection of inert atmosphere, first increased by room temperature To 250 DEG C~300 DEG C, then accelerated warming to 800 DEG C~1200 DEG C, then Isothermal sinter 2h~6h, is cooled to room temperature, and is obtained certainly The three-dimensional porous carbon of support.
2. the preparation method of three-dimensional porous carbon according to claim 1, which is characterized in that the matter of the sugar source and dopamine Amount is than being 4~100: 1.
3. the preparation method of three-dimensional porous carbon according to claim 2, which is characterized in that the sugar source and dopamine it is total Quality and the mass ratio of ammonium chloride are 0.2~5: 1.
4. the preparation method of three-dimensional porous carbon according to any one of claims 1 to 3, which is characterized in that the room temperature When being increased to 250 DEG C~300 DEG C, heating rate is 1 DEG C/min~10 DEG C/min, keeps the temperature 0~3h.
5. the preparation method of three-dimensional porous carbon according to claim 4, which is characterized in that the accelerated warming stage rises Warm rate is 2 DEG C/min~15 DEG C/min, and the heating rate in the stage is greater than the room temperature when being increased to 250 DEG C~300 DEG C Heating rate.
6. the preparation method of three-dimensional porous carbon according to any one of claims 1 to 3, which is characterized in that the sugar source Including one of glucose, fructose, sucrose and maltose or a variety of.
7. the preparation method of three-dimensional porous carbon according to any one of claims 1 to 3, which is characterized in that the inertia Atmosphere is nitrogen.
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Cited By (1)

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CN110217786A (en) * 2019-05-30 2019-09-10 贵州梅岭电源有限公司 A kind of preparation method and application of supercapacitor high specific property electrode material

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CN107963621A (en) * 2017-11-27 2018-04-27 中南大学 Three-dimensional porous carbon material, preparation thereof and application thereof in sodium-ion battery
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110217786A (en) * 2019-05-30 2019-09-10 贵州梅岭电源有限公司 A kind of preparation method and application of supercapacitor high specific property electrode material
CN110217786B (en) * 2019-05-30 2022-09-20 贵州梅岭电源有限公司 Preparation method and application of electrode material with high specific property for supercapacitor

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