CN110642238B - Graphene-like nitrogen-doped porous carbon material and preparation method and application thereof - Google Patents
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Abstract
The invention relates to a graphene-like nitrogen-doped porous carbon material and a preparation method and application thereof, and the method comprises the following steps: (1) melamine, PVP and ammonium chloride are used as raw materials, and are mixed and ground according to a certain proportion to obtain a mixture; (2) and (2) calcining the mixture obtained in the step (1) in an air atmosphere to obtain the graphene-like nitrogen-doped porous carbon material. The method comprises the steps of taking melamine, PVP and ammonium chloride as raw materials, mixing and grinding the raw materials according to a certain proportion, and directly placing the raw materials in an air atmosphere for calcination to obtain the graphene-like nitrogen-doped porous carbon material. In the preparation process, the graphene-like nitrogen-doped porous carbon material can be obtained by directly calcining without a drying process, so that the preparation period is shortened, and the preparation flow is simplified; the catalyst can be prepared by calcining in air atmosphere, and the preparation process is convenient; the obtained material has excellent electrochemistry and adsorption performance, and can be widely applied to super capacitors and organic pollutant adsorption.
Description
Technical Field
The invention relates to the technical field of preparation of graphene-like materials, in particular to a graphene-like nitrogen-doped porous carbon material and a preparation method and application thereof.
Background
The graphene-like porous carbon material has the advantages of high specific surface area, wide forbidden band width, strong in-plane electron transmission capability, long service life of photon-generated carriers and the like, attracts people to pay extensive attention, and is widely applied to the fields of capacitive sensors, photocatalytic degradation of organic pollutants and the like.
In order to further improve the performance of the graphene-like porous carbon material, at present, researches are carried out to dope nitrogen elements into the graphene-like porous carbon material by adopting different preparation methods to obtain the graphene-like nitrogen-doped porous carbon material. In the related art, the preparation method of the graphene-like nitrogen-doped porous carbon material comprises the following steps: adding resorcinol, HMT (hexamethylene tetramine), deionized water, ammonia water, melamine and TMB (3, 3',5,5' -Tetramethylbenzidine, 3,3',5,5' -Tetramethylbenzidine) trimethylbenzene into a round-bottom flask, reacting at 80 ℃ for 8h, centrifugally drying, heating to 900 ℃ at the heating rate of 1 ℃/min in a nitrogen atmosphere, and calcining for 3h to obtain the graphene-like nitrogen-doped porous carbon material.
According to the method for preparing the graphene-like nitrogen-doped porous carbon material, after the raw materials are mixed, the subsequent drying process is needed to calcine, so that the preparation time is long; in addition, in order to prevent the graphene-like material from being oxidized, inert gas needs to be introduced in the calcining process to ensure that the calcining process is carried out under the inert atmosphere, and the preparation process is inconvenient.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a graphene-like nitrogen-doped porous carbon material which is short in preparation time and free of inert gas protection.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
in a first aspect, a preparation method of a graphene-like nitrogen-doped porous carbon material is provided, which comprises the following steps:
(1) melamine, PVP (polyvinylpyrrolidone) and ammonium chloride are taken as raw materials, and are mixed and ground according to a certain proportion to obtain a mixture;
(2) and (2) calcining the mixture obtained in the step (1) in an air atmosphere to obtain the graphene-like nitrogen-doped porous carbon material.
As a further improvement of the invention, the method comprises the following steps:
(1) respectively weighing melamine, PVP and ammonium chloride according to a certain mass ratio, adding the melamine, the PVP and the ammonium chloride into a mortar, and grinding for a period of time to obtain a mixture;
(2) and (2) putting the mixture obtained in the step (1) into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating the muffle furnace from room temperature to a certain temperature, and preserving the temperature for a period of time to obtain the graphene-like nitrogen-doped porous carbon material.
As a further improvement of the invention, the mass ratio of the melamine, the PVP and the ammonium chloride is 1-3:1: 1-3.
As a further improvement of the invention, melamine, PVP and ammonium chloride were added to a mortar and ground for 1 min.
As a further improvement of the invention, the muffle furnace is heated from room temperature to 600-1000 ℃.
As a further improvement of the invention, the muffle furnace is heated to 600-1000 ℃ from room temperature and then is kept warm for 4-6 h.
As a further improvement of the invention, the temperature rise rate of the muffle furnace is 5-10 ℃/min.
As a further improvement of the invention, the method comprises the following steps:
(1) respectively weighing melamine, PVP and ammonium chloride according to the mass ratio of 1:1:1, adding the melamine, PVP and ammonium chloride into a mortar, and grinding for 1min to obtain a mixture;
(2) and (2) putting the mixture obtained in the step (1) into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating the muffle furnace to 900 ℃ from room temperature at a heating rate of 5 ℃/min, and then preserving heat for 5h to obtain the graphene-like nitrogen-doped porous carbon material.
In a second aspect, a graphene-like nitrogen-doped porous carbon material is provided, which is prepared by the preparation method of the first aspect.
In a third aspect, the application of the graphene-like nitrogen-doped porous carbon material in the super capacitor and the organic pollutant adsorption is provided.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
according to the graphene-like nitrogen-doped porous carbon material and the preparation method thereof, provided by the invention, melamine, PVP and ammonium chloride are used as raw materials, mixed and ground according to a certain proportion, and directly placed in an air atmosphere for calcination to obtain the graphene-like nitrogen-doped porous carbon material.
(1) The mixture obtained by grinding melamine, PVP and ammonium chloride can be directly calcined without a drying process, so that the graphene-like nitrogen-doped porous carbon material is obtained, the preparation period is shortened, and the preparation process is simplified.
(2) The preparation method comprises the following steps of taking trichlorocyanamide as a carbon source, a nitrogen source and a template, taking PVP as a carbon source and a pore-forming agent, taking ammonium chloride as a pore-forming agent, and providing an acid environment to be beneficial to carbonization in the calcining process, wherein in the calcining process, gases generated by decomposition of the PVP and the ammonium chloride promote the material to form a pore structure.
The existence of the ammonium chloride inhibits the peroxidation of the material and prevents the complete oxidation of the material, so that the graphene-like nitrogen-doped porous carbon material can be obtained even if the material is calcined in the air atmosphere, the calcination process does not need to be kept under the inert atmosphere, and the preparation process is convenient.
(3) The specific surface area of the prepared graphene-like nitrogen-doped porous carbon material can reach 800m2The catalyst has a structure of/g, and a mesoporous structure and a microporous structure exist at the same time, so that the catalyst has excellent electrochemical and adsorption properties: the specific capacitance of the super capacitor can reach 216F/g (the current density is 1A/g), and the methylene blue adsorption can reach 300 mg/g.
(4) The preparation method of the graphene-like nitrogen-doped porous carbon material provided by the method is simple and convenient, and the obtained material has excellent electrochemistry and adsorption properties and can be widely applied to super capacitors and organic pollutant adsorption, such as photocatalytic adsorption and electro-catalytic adsorption.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is an XRD pattern of the graphene-like nitrogen-doped porous carbon material obtained in example 1.
Fig. 2 is a raman spectrum of the graphene-like nitrogen-doped porous carbon material obtained in example 1.
Fig. 3 is a scanning electron microscope image of the graphene-like nitrogen-doped porous carbon material obtained in example 1.
Fig. 4 is a transmission electron microscope image of the graphene-like nitrogen-doped porous carbon material obtained in example 1.
Fig. 5 is an XPS chart of the graphene-like nitrogen-doped porous carbon material obtained in example 1.
Fig. 6 is a nitrogen adsorption and desorption curve diagram of the graphene-like nitrogen-doped porous carbon material obtained in example 1.
Fig. 7 is a pore size distribution diagram of the graphene-like nitrogen-doped porous carbon material obtained in example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail and fully with reference to the accompanying drawings and specific embodiments.
Example 1:
the preparation method of the graphene-like nitrogen-doped porous carbon material comprises the following steps:
(1) respectively weighing melamine, PVP and ammonium chloride according to the mass ratio of 1:1:1, adding the melamine, the PVP and the ammonium chloride into a mortar, and grinding for 1min to obtain a mixture.
(2) And (2) putting the mixture obtained in the step (1) into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating the muffle furnace to 900 ℃ from room temperature at a heating rate of 5 ℃/min, and then preserving heat for 5h to obtain the graphene-like nitrogen-doped porous carbon material.
Fig. 1 is an XRD pattern of the obtained graphene-like nitrogen-doped porous carbon material, and it can be seen from fig. 1 that a characteristic peak of 2 θ =26 ° exists in the XRD pattern and coincides with the diffraction peak position of the (002) crystal plane of graphene; FIG. 2 is a Raman spectrum of the obtained graphene-like nitrogen-doped porous carbon material, and it can be seen from FIG. 2 that the Raman spectrum is at 1363cm-1And 1612cm-1A near raman peak corresponding to a D peak and a G peak of graphene; fig. 3 and 4 are electron micrographs of the obtained graphene-like nitrogen-doped porous carbon material, respectively, and it can be seen from fig. 3 and 4 that the obtained nitrogen-doped porous carbon material has a multilayer structure; fig. 5 is an XPS chart of the obtained graphene-like nitrogen-doped porous carbon material, and it can be seen from fig. 5 that the obtained material contains a nitrogen element. Therefore, as can be seen from fig. 1 to 5, the graphene-like nitrogen-doped porous carbon material is obtained according to the present invention.
Fig. 6 and 7 are a nitrogen adsorption-desorption curve diagram and a pore size distribution diagram of the obtained graphene-like nitrogen-doped porous carbon material, respectively, and it can be seen from fig. 6 and 7 that the graphene-like nitrogen-doped porous carbon material has mesopores and micropores, and it can be seen from calculation that the specific surface area of the obtained graphene-like nitrogen-doped porous carbon material is 800m2/g。
Example 2:
the preparation method of the graphene-like nitrogen-doped porous carbon material comprises the following steps:
(1) respectively weighing melamine, PVP and ammonium chloride according to the mass ratio of 1:1:3, adding the melamine, the PVP and the ammonium chloride into a mortar, and grinding for 1min to obtain a mixture.
(2) And (2) putting the mixture obtained in the step (1) into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating the muffle furnace from room temperature to 600 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 6h to obtain the graphene-like nitrogen-doped porous carbon material.
Detected to obtainThe specific surface area of the graphene nitrogen-doped porous carbon material is 752m2/g。
Example 3:
the preparation method of the graphene-like nitrogen-doped porous carbon material comprises the following steps:
(1) respectively weighing melamine, PVP and ammonium chloride according to the mass ratio of 3:1:1, adding the melamine, the PVP and the ammonium chloride into a mortar, and grinding for 1min to obtain a mixture.
(2) And (2) putting the mixture obtained in the step (1) into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating the muffle furnace from room temperature to 1000 ℃ at a heating rate of 5 ℃/min, and then preserving heat for 4h to obtain the graphene-like nitrogen-doped porous carbon material.
Through detection, the specific surface area of the obtained graphene nitrogen-doped porous carbon material is 750m2/g。
Comparative example 1:
(1) respectively weighing melamine, PVP and ammonium chloride according to the mass ratio of 1:1:1, adding the melamine, the PVP and the ammonium chloride into a mortar, and grinding for 1min to obtain a mixture.
(2) And (2) placing the mixture obtained in the step (1) into a ceramic crucible, placing the ceramic crucible into a tubular furnace, introducing nitrogen, heating the tubular furnace from room temperature to 900 ℃ at the heating rate of 5 ℃/min under the nitrogen atmosphere, and then preserving heat for 5h to obtain the graphene-like nitrogen-doped porous carbon material.
The specific surface area of the graphene-like nitrogen-doped porous carbon material obtained in the embodiment is 760m2 /g。
Experimental example 1: electrochemical performance characterization of graphene-like nitrogen-doped porous carbon material
Prior to performing the electrochemical test, the working electrode was first prepared: grinding the prepared electrode material into powder, drying at 105 ℃ for 8 hours, and removing water; secondly, mixing the dried electrode material powder with 5wt% of polytetrafluoroethylene solution according to the mass ratio of 95:100 (about 0.1g of electrode material powder, recording the mass m of the electrode material powder)1Mass m of solution of polytetrafluoroethylene2) Adding 40-50% of distilled watermL, mechanically stirring or electromagnetically stirring for 5 hours; thirdly, drying the mixed electrode material and the foam nickel sheet together at 105 ℃ for 8 hours, and removing moisture; fourthly, weighing the two foam nickel sheets and recording the mass m3Flattening the electrode material mixed with polytetrafluoroethylene, wrapping and clamping the electrode material in the weighed two foamed nickel sheets, and tabletting to prepare electrode sheets; fifthly, drying and dehydrating the electrode slice at 105 ℃, and recording the mass m of the electrode slice4(ii) a And sixthly, soaking the dried electrode slice in the electrolyte for 24 hours to perform electrochemical test. The active mass m in the electrode sheet is calculated according to the following formula:
electrochemical performance tests were performed using a standard three-electrode system on an electrochemical workstation (Gamry Interface 1000E), in which the prepared electrode sheet, platinum sheet and saturated calomel electrode were used as a working electrode, a counter electrode and a reference electrode, respectively, and 6mol/L KOH was used as an electrolyte, and the obtained results are shown in table 1.
TABLE 1
Experimental example 2: characterization of organic pollutant adsorption performance of graphene-like nitrogen-doped porous carbon material
The dosage of the fixed graphene nitrogen-doped porous carbon material is 10mg, the concentration of the adsorbed methylene blue solution is 100 mg/L, and the reaction is carried out for 90min under the dark condition, so that the adsorption value of the methylene blue is obtained, and the obtained results are shown in table 2.
TABLE 2
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A preparation method of a graphene-like nitrogen-doped porous carbon material is characterized by comprising the following steps:
(1) melamine, polyvinylpyrrolidone PVP and ammonium chloride are used as raw materials, and are mixed and ground according to a certain proportion to obtain a mixture;
(2) and (2) calcining the mixture obtained in the step (1) in an air atmosphere to obtain the graphene-like nitrogen-doped porous carbon material.
2. The preparation method of the graphene-like nitrogen-doped porous carbon material according to claim 1, comprising the following steps:
(1) respectively weighing melamine, PVP and ammonium chloride according to a certain mass ratio, adding the melamine, the PVP and the ammonium chloride into a mortar, and grinding for a period of time to obtain a mixture;
(2) and (2) putting the mixture obtained in the step (1) into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating the muffle furnace to a certain temperature from room temperature, and preserving the temperature for a period of time to obtain the graphene-like nitrogen-doped porous carbon material.
3. The preparation method of the graphene-like nitrogen-doped porous carbon material according to claim 2, wherein the mass ratio of the melamine to the PVP to the ammonium chloride is 1-3:1: 1-3.
4. The method for preparing a graphene-like nitrogen-doped porous carbon material according to claim 2, wherein melamine, PVP and ammonium chloride are added into a mortar and ground for 1 min.
5. The method for preparing the graphene-like nitrogen-doped porous carbon material according to claim 2, wherein a muffle furnace is heated from room temperature to 600-1000 ℃.
6. The preparation method of the graphene-like nitrogen-doped porous carbon material according to claim 5, wherein the muffle furnace is heated from room temperature to 600-1000 ℃ and then is kept for 4-6 h.
7. The method for preparing the graphene-like nitrogen-doped porous carbon material according to claim 2, wherein the temperature rise rate of the muffle furnace is 5-10 ℃/min.
8. The preparation method of the graphene-like nitrogen-doped porous carbon material according to claim 2, comprising the following steps:
(1) respectively weighing melamine, PVP and ammonium chloride according to the mass ratio of 1:1:1, adding the melamine, PVP and ammonium chloride into a mortar, and grinding for 1min to obtain a mixture;
(2) and (2) putting the mixture obtained in the step (1) into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating the muffle furnace to 900 ℃ from room temperature at a heating rate of 5 ℃/min, and then preserving heat for 5h to obtain the graphene-like nitrogen-doped porous carbon material.
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| CN114256468A (en) * | 2021-12-03 | 2022-03-29 | 北京科技大学 | Preparation method of platinum quantum dot loaded nitrogen-doped graphene-like carbon material |
| CN114715875A (en) * | 2022-03-31 | 2022-07-08 | 宁波大学 | Preparation method of thin-layer carbon-based material and application of thin-layer carbon-based material as battery material |
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