CN108821279B - Preparation method of three-dimensional porous carbon - Google Patents

Preparation method of three-dimensional porous carbon Download PDF

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CN108821279B
CN108821279B CN201810943090.6A CN201810943090A CN108821279B CN 108821279 B CN108821279 B CN 108821279B CN 201810943090 A CN201810943090 A CN 201810943090A CN 108821279 B CN108821279 B CN 108821279B
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porous carbon
dimensional porous
temperature
preparation
self
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CN108821279A (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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    • 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 three-dimensional porous carbon, and the preparation methodThe preparation method comprises the steps of uniformly mixing the sugar source, the dopamine and the 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

Preparation method of three-dimensional porous carbon
Technical Field
The invention belongs to the field of porous materials, relates to a preparation method of three-dimensional porous carbon, and particularly relates to a preparation method of self-supporting three-dimensional porous carbon with a high specific surface area.
Background
The self-supporting three-dimensional porous carbon material has characteristics of rich pore channel structure, high specific surface area, good conductivity and the like, so that the self-supporting three-dimensional porous carbon material has wide application in the fields of catalysis, energy, environment and the like. In order to make the porous carbon play a role to the maximum extent, the preparation of the three-dimensional porous carbon with high specific surface area has been the direction of people's efforts. The preparation methods of the self-supporting three-dimensional porous carbon at present can be roughly divided into four main categories: the method comprises the first self-assembly method of graphene oxide, the second chemical vapor deposition method, the third carbon precursor blowing conversion method and the fourth carbonization method of polymer foam, wherein the first self-assembly method of graphene oxide comprises a hydrothermal treatment method, a freeze drying method, a vacuum volatilization method, a dropping coating method and the like. However, these methods have the disadvantages of more steps, complicated process, difficulty in mass production, and insufficient specific surface area of the obtained product (generally less than 2000 m)2Per g), the additional use of acids (H) is also required3PO4) Or alkali (KOH) activation, etc.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of self-supporting three-dimensional porous carbon with high specific surface area, which only needs one-step pyrolysis and does not need any additional step to obtain the specific surface area up to 2700m2Self-supporting three-dimensional porous carbon per gram.
In order to solve the technical problems, the invention adopts the following technical scheme.
A preparation method of three-dimensional porous carbon comprises the following steps:
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.
In the preparation method of the three-dimensional porous carbon, the mass ratio of the sugar source to the dopamine is preferably 4-100: 1.
In the above method for preparing the three-dimensional porous carbon, preferably, the ratio of the total mass of the sugar source and the dopamine to the mass of the ammonium chloride is 0.2-5: 1.
In the preparation method of the three-dimensional porous carbon, preferably, when the room temperature is raised to 250-300 ℃, the heating rate is 1-10 ℃/min, and the temperature is kept for 0-3 h.
In the above preparation method of the three-dimensional porous carbon, preferably, in the accelerated temperature rise stage, the temperature rise rate is 2 ℃/min to 15 ℃/min, and the temperature rise rate in the accelerated temperature rise stage is greater than the temperature rise rate when the room temperature rises to 250 ℃ to 300 ℃.
In the above method for producing three-dimensional porous carbon, preferably, the sugar source includes one or more of glucose, fructose, sucrose and maltose.
In the above method for preparing three-dimensional porous carbon, preferably, the inert atmosphere is nitrogen.
Compared with the prior art, the invention has the advantages that:
(1) the self-supporting three-dimensional porous carbon obtained by the invention has very high specific surface area, and can reach 2700m under the condition of the invention2Per g, even above, the existing sugar foaming method only obtains more than 1000m of product2/g。
(2) The preparation method provided by the invention does not need any pretreatment or post-treatment step, and the self-supporting three-dimensional porous carbon with high specific surface area can be obtained by a one-step heating method.
(3) According to the invention, the self-supporting three-dimensional porous carbon with high specific surface area can be obtained without activating strong acid and alkali substances such as phosphoric acid or potassium hydroxide, so that the subsequent purification step is avoided, the loss of instruments and the pollution to products are reduced, and the process steps are simplified.
Drawings
Fig. 1 is an optical photograph of the three-dimensional porous carbon prepared in example 1 of the present invention.
Fig. 2 is a scanning electron micrograph of the three-dimensional porous carbon prepared in example 1 of the present invention.
Fig. 3 is a nitrogen adsorption/desorption curve of the three-dimensional porous carbon prepared in example 1 of the present invention.
Fig. 4 is an optical photograph of the three-dimensional porous carbon prepared in example 2 of the present invention.
Fig. 5 is a scanning electron micrograph of the three-dimensional porous carbon prepared in example 2 of the present invention.
Fig. 6 is a nitrogen adsorption/desorption curve of the three-dimensional porous carbon prepared in example 2 of the present invention.
Fig. 7 is an optical photograph of the three-dimensional porous carbon prepared in example 3 of the present invention.
Fig. 8 is a scanning electron micrograph of the three-dimensional porous carbon prepared in example 3 of the present invention.
Fig. 9 is a nitrogen adsorption/desorption curve of the three-dimensional porous carbon prepared in example 3 of the present invention.
Fig. 10 is a scanning electron micrograph of the three-dimensional porous carbon prepared in comparative example 1.
Fig. 11 is a nitrogen adsorption/desorption curve of the three-dimensional porous carbon prepared in comparative example 1.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
The materials and equipment used in the following examples are commercially available.
The preparation method of the three-dimensional porous carbon comprises the following steps:
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.
In the preparation method, the mass ratio of the sugar source to the dopamine is 4-100: 1 (namely 99: 1-80: 20), and the mass ratio of the total mass of the sugar source and the dopamine to the mass of the ammonium chloride is 0.2-5: 1 (namely 1: 5-5: 1).
In the preparation method, when the room temperature is raised to 250-300 ℃, the heating rate is 1-10 ℃/min, and the temperature is kept for 0-3 h; and accelerating the temperature rise stage, wherein the temperature rise rate is 2-15 ℃/min, and the temperature rise rate of the stage is greater than the temperature rise rate when the room temperature rises to 250-300 ℃.
In the above preparation method, the sugar source comprises one or more of glucose, fructose, sucrose and maltose.
In the above production method, the inert atmosphere is preferably nitrogen.
Example 1:
the preparation method of the three-dimensional porous carbon comprises the following steps:
2g of glucose, 0.1g of dopamine and 2g of ammonium chloride are uniformly mixed, the obtained mixture is placed in a tube furnace, under the protection of nitrogen, the temperature is increased to 250 ℃ from room temperature at the speed of 2 ℃/min, then is continuously increased to 1000 ℃ at the speed of 4 ℃/min, the temperature is kept for 3 hours, and then the self-supporting three-dimensional porous carbon can be obtained after natural cooling to the room temperature.
The self-supported three-dimensional porous carbon prepared in this example was characterized, and fig. 1 is an optical photograph of the three-dimensional porous carbon, and fig. 2 is a scanning electron micrograph showing the three-dimensional porous carbonThe surface of the sample has a plurality of pore structures, and FIG. 3 is a nitrogen adsorption and desorption curve of the sample, and the BET specific surface area is 2600m2/g。
Example 2:
the preparation method of the three-dimensional porous carbon comprises the following steps:
2g of glucose, 0.02g of dopamine and 2g of ammonium chloride are uniformly mixed, the obtained mixture is placed in a tube furnace, under the protection of nitrogen, the temperature is raised to 250 ℃ from room temperature at the rate of 2 ℃/min, the temperature is kept for 2 hours, then the temperature is continuously raised to 1000 ℃ at the rate of 8 ℃/min, the temperature is kept for 3 hours, and then the mixture is naturally cooled to room temperature, so that the self-supporting three-dimensional porous carbon can be obtained.
The self-supported three-dimensional porous carbon prepared in this example was characterized, fig. 4 is an optical photograph of the self-supported three-dimensional porous carbon, fig. 5 is a scanning electron micrograph showing that the surface has a plurality of pore structures, fig. 6 is a nitrogen adsorption/desorption curve of the sample, and the BET specific surface area is 2700m2/g。
Example 3:
the preparation method of the three-dimensional porous carbon comprises the following steps:
2g of glucose, 0.2g of dopamine and 2g of ammonium chloride are uniformly mixed, the obtained mixture is placed in a tube furnace, under the protection of nitrogen, the temperature is increased to 250 ℃ from room temperature at a rate of 4 ℃/min, then the temperature is continuously increased to 1000 ℃ at a rate of 10 ℃/min, the temperature is kept for 3 hours, and then the self-supporting three-dimensional porous carbon can be obtained after natural cooling to room temperature.
The self-supporting three-dimensional porous carbon prepared in the embodiment is characterized, fig. 7 is an optical photograph of the self-supporting three-dimensional porous carbon, fig. 8 is a scanning electron microscope photograph showing that the surface has a plurality of pore channel structures, fig. 9 is a nitrogen adsorption and desorption curve of a sample, and the BET specific surface area is 2300m2/g。
Comparative example 1:
a method of preparing three-dimensional porous carbon substantially as described in example 1, except that: and (3) adding no dopamine, and only uniformly mixing glucose and ammonium chloride and placing the mixture in a tube furnace for treatment. FIG. 10 is a scanning electron micrograph showing the surfaceThe pore channel structure is less, FIG. 11 is a nitrogen adsorption and desorption curve of a sample, and the BET specific surface area of the obtained three-dimensional porous carbon is only 1000m2/g。
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed embodiments, or equivalent modifications, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.

Claims (5)

1. A preparation method of three-dimensional porous carbon comprises the following steps:
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 self-supporting three-dimensional porous carbon;
the mass ratio of the sugar source to the dopamine is 4-100: 1;
the mass ratio of the total mass of the sugar source and the dopamine to the mass of the ammonium chloride is 0.2-5: 1.
2. The preparation method of the three-dimensional porous carbon according to claim 1, wherein the temperature is raised to 250-300 ℃ at a rate of 1-10 ℃/min and maintained for 0-3 h.
3. The method for preparing three-dimensional porous carbon according to claim 2, wherein the temperature increase rate of the accelerated temperature increase stage is 2 ℃/min to 15 ℃/min, and the temperature increase rate of the accelerated temperature increase stage is greater than the temperature increase rate when the room temperature is increased to 250 ℃ to 300 ℃.
4. The method of making three-dimensional porous carbon according to claim 1, wherein the sugar source comprises one or more of glucose, fructose, sucrose and maltose.
5. The method for preparing three-dimensional porous carbon according to claim 1, wherein the inert atmosphere is nitrogen.
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