CN113511643B - Method for preparing high-capacitance carbon nanocages in green cycle mode and carbon nanocages - Google Patents
Method for preparing high-capacitance carbon nanocages in green cycle mode and carbon nanocages Download PDFInfo
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- CN113511643B CN113511643B CN202110527351.8A CN202110527351A CN113511643B CN 113511643 B CN113511643 B CN 113511643B CN 202110527351 A CN202110527351 A CN 202110527351A CN 113511643 B CN113511643 B CN 113511643B
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a method for preparing a high-capacitance carbon nanocage in a green circulation manner, which comprises the following steps: mixing basic magnesium carbonate and magnesium powder to obtain mixed powder; heating the mixed powder to 600-800 ℃ under the protection of inert gas, preserving heat for 1-2h, and cooling to room temperature to obtain black powder; adding deionized water into the black powder, stirring, heating to 80-100 deg.C, maintaining the temperature for 1-2h, and cooling to room temperature; stirring, continuously introducing carbon dioxide, filtering, and drying the filter to obtain carbon nanocages; collecting the filtered filtrate, stirring at 55-100 ℃, and preserving heat to obtain the basic magnesium carbonate. Drying the prepared basic magnesium carbonate to be used as a raw material, and then circularly preparing the carbon nanocages. The whole process is green, simple, convenient and quick, the alkali type magnesium carbonate raw material is continuously increased in the whole circulation process, and the prepared carbon nano cage can be used as an electrode material of a super capacitor and has excellent capacitance performance.
Description
Technical Field
The invention belongs to the technical field of porous carbon materials, and particularly relates to a method for preparing a high-capacitance carbon nanocage in an environment-friendly circulating manner and the carbon nanocage.
Background
The carbon-based super capacitor has the advantages of high power density, long cycle life and the like, and is applied to the fields of industrial production, aerospace, military equipment, energy, traffic and the like. The electrode material is one of the key factors determining the energy storage performance of the super capacitor; among them, porous carbon materials are widely used as electrode materials for supercapacitors because of their high specific surface area. Typical methods of making porous carbon materials include: an activation method, a hydrothermal carbonization method, a template method, and the like.
The template method has the advantages of controllable morphology, high specific surface area and the like, and is a potential strategy for preparing high-performance carbon materials. Wherein, CO is used 2 The template method for preparing the raw material is an emerging carbon material preparation method in recent years, has the advantages of wide raw material source, low price, convenient product post-treatment and the like, and is expected to become one of approaches for solving the problem of large-scale preparation of high-performance carbon materials. For example, in patent CN201210545871.2, metal magnesium is burned in a beaker filled with carbon dioxide gas, and the template is removed by hydrochloric acid to obtain nitrogen-doped mesoporous graphene.
Although the template method can effectively remove the greenhouse gas CO 2 Conversion to useful carbon materials, but also has disadvantages: (1) In the process of preparing the carbon material by the template method, the generated MgO template cannot be recycled, so that a large amount of waste of the template can be caused; (2) In the process of removing the MgO template, HF, HCl and other toxic reagents are used, which causes certain pollution to the environment. Therefore, a method for preparing the porous carbon material in a green cycle is needed to be designed.
Disclosure of Invention
Based on the technical problems, the invention provides a method for preparing a porous carbon material in a green cycle manner and the porous carbon material. The method of the invention overcomes the defects of environmental pollution and MgO template waste caused by using toxic reagents HF and HCl to remove the template in the existing template method, and realizes the cyclic preparation of the carbon nanocages. The whole process is green, simple, convenient and quick. The prepared carbon nanocages can be used as electrode materials of a super capacitor and show excellent double-layer capacitance performance.
The technical scheme of the invention is as follows:
the invention provides a method for preparing a high-capacitance carbon nanocage in a green circulation manner, which comprises the following steps: (1) Mixing basic magnesium carbonate and magnesium powder to obtain mixed powder; (2) Heating the mixed powder to 600-800 ℃ under the protection of inert gas, preserving heat for 1-2h, and cooling to room temperature to obtain black powder; (3) Adding deionized water into the black powder, stirring, heating to 80-100 deg.C, maintaining the temperature for 1-2h, and cooling to room temperature; (4) Stirring, continuously introducing carbon dioxide, filtering, and drying the filter to obtain carbon nanocages; (5) Collecting the filtered filtrate, stirring at 55-100 ℃, and preserving heat to obtain the basic magnesium carbonate.
And (4) drying the basic magnesium carbonate obtained in the step (5) and then taking the dried basic magnesium carbonate as a raw material, thus circularly preparing the carbon nanocages. The drying temperature and time of the basic magnesium carbonate are not particularly limited, and can be adjusted according to actual needs, for example, drying for 8-12h at 80-100 ℃.
Preferably, in the step (1), the mass ratio of the magnesium powder to the basic magnesium carbonate is 1:1-12; preferably, the mass ratio of the magnesium powder to the basic magnesium carbonate is 1:1-8.
Preferably, in the step (2), the inert gas is argon or helium; more preferably, the inert gas is high purity argon having a purity of 99.99%.
Preferably, in the step (2), the temperature rising rate is 5-15 ℃/min.
Preferably, in the step (3), the adding amount of the deionized water is 1-3.
Preferably, in the step (4), the stirring speed is 800-1200r/min; the introduction time of the carbon dioxide is 1-2h; the drying temperature is 80-100 ℃, and the drying time is 8-12h.
Preferably, in step (5), the stirring rate is 300 to 800r/min.
Preferably, the magnesium powder has an average particle size of 100 to 200 mesh.
The invention also provides a carbon nanocage prepared according to the method.
Has the advantages that:
the invention provides a method for preparing carbon nanocages in a green cycle manner, which comprises the steps of mixing magnesium powder (Mg) and basic magnesium carbonate (4 MgCO) 3 ·Mg(OH) 2 ·4H 2 O) mixing, high-temperature burning to generate magnesium oxide (MgO) template and carbon precursor carbon dioxide (CO) 2 ) Carbon precursor carbon dioxide reacts with magnesium powder in the raw materials to generate a magnesium oxide template and a carbon composite (C @ MgO), and the generated carbon is coated on the magnesium oxide template; the magnesium oxide template in the product further reacts with deionized water and carbon dioxide to form carbon nano cages after the carbon template is stripped, and the magnesium oxide template is converted into basic magnesium carbonate raw materials again, so that the continuous cycle preparation of the carbon nano cages is realized, and the alkali type magnesium carbonate raw materials are increased continuously in the whole cycle process.
The method is simple and easy to implement, and the mixed powder of the basic magnesium carbonate and the magnesium powder is used as the raw material, so that the source is wide. The method not only realizes the cyclic regeneration of the basic magnesium carbonate raw material, but also overcomes the pressure of environmental protection caused by using a large amount of HF and HCl when the magnesium oxide template is removed, and successfully converts greenhouse gas carbon dioxide into the carbon nanocages with excellent capacitance performance, and the whole process is green and environment-friendly.
The carbon nanocages prepared by the method have micropores, mesopores and macropores, are mainly mesoporous, have large specific surface area and excellent capacitance performance, can be used as electrode materials of super capacitors, and show excellent double electric layer capacitance performance.
In a preferable scheme, the ratio of magnesium powder to basic magnesium carbonate is controlled, so that the carbon nanocage material with few layers can be obtained, and the capacitance performance of the carbon nanocage material is more excellent.
Drawings
FIGS. 1a-b are Transmission Electron Microscope (TEM) photographs of carbon nanocages obtained in the first and tenth cycles of example 1 of the present invention;
FIG. 2 is X-ray diffraction (XRD) patterns of the carbon nanocages and the raw material obtained in example 1 of the present invention, which are repeated the first time and the tenth time;
FIG. 3a is a cyclic voltammogram of the carbon nanocages in KOH electrolyte obtained in the first and tenth cycles of example 1 of the present invention;
FIG. 3b is the mass specific capacitance of the carbon nanocages obtained in the first and tenth cycles of example 1 of the present invention at different current densities;
FIG. 4 is a reaction scheme of the present invention;
Detailed Description
Hereinafter, the technical solution of the present invention will be described in detail by specific examples, but these examples should be explicitly proposed for illustration, but should not be construed as limiting the scope of the present invention.
Example 1
(1) Taking 2g of basic magnesium carbonate and 0.5g of magnesium powder, uniformly mixing, and putting into a porcelain boat; wherein the purity of the metal magnesium powder is 99.9 percent, and the average grain diameter is 100 meshes;
(2) Putting the porcelain boat into a vacuum tube furnace, vacuumizing, introducing high-purity argon (with the purity of 99.99%), heating to 800 ℃ at the speed of 10 ℃/min under the protection of the argon, preserving the temperature for 2 hours, cooling to room temperature, and taking out a black product;
(3) Pouring the product into a beaker, adding 500mL of deionized water, putting the beaker into a heat collection type constant temperature heating magnetic stirrer, stirring at the stirring speed of 800r/min at 80 ℃, preserving the temperature for 2 hours, and then cooling to room temperature;
(4) Continuously introducing CO into the solution for two hours under the stirring condition (the stirring speed is 800 r/min) 2 Filtering, and drying the filter body in a vacuum drying oven at 80 ℃ for 8h to obtain a black carbon material, namely the carbon nanocages;
(5) And stirring the obtained filtrate for 2 hours at 80 ℃ at a stirring speed of 500r/min by using a heat collection type constant temperature heating magnetic stirrer to obtain the basic magnesium carbonate.
Putting the basic magnesium carbonate obtained in the step (5) into a vacuum drying oven, and drying for 8 hours at 90 ℃; mixing with magnesium powder, and repeating the steps 1-5 to obtain the carbon nanocages prepared circularly.
Example 2
(1) Taking 4g of basic magnesium carbonate and 4g of magnesium powder, uniformly mixing, and putting into a porcelain boat; wherein the purity of the metal magnesium powder is 99.9 percent, and the average grain diameter is 100 meshes;
(2) Putting the porcelain boat into a vacuum tube furnace, vacuumizing, introducing high-purity argon (with the purity of 99.99%), heating to 800 ℃ at the speed of 15 ℃/min under the protection of the argon, preserving heat for 2 hours, cooling to room temperature, and taking out a black product;
(3) Pouring the product into a beaker, adding 500mL of deionized water, putting the beaker into a heat collection type constant temperature heating magnetic stirrer, stirring at the stirring speed of 800r/min at 80 ℃, preserving the temperature for 2 hours, and then cooling to room temperature;
(4) Continuously introducing CO into the solution for two hours under the stirring condition (the stirring speed is 800 r/min) 2 Filtering, and drying the filter body in a vacuum drying oven at 80 ℃ for 8h to obtain a black carbon material, namely the carbon nanocages;
(5) And stirring the obtained filtrate for 2 hours at 55 ℃ at a stirring speed of 800r/min by using a heat collection type constant temperature heating magnetic stirrer to obtain the basic magnesium carbonate.
Putting the basic magnesium carbonate obtained in the step (5) into a vacuum drying oven, and drying for 8 hours at 100 ℃; mixing with magnesium powder, and repeating the steps 1-5 to obtain the carbon nanocages prepared circularly.
Example 3
(1) Taking 6g of basic magnesium carbonate and 0.5g of magnesium powder, uniformly mixing, and putting into a porcelain boat; wherein the purity of the metal magnesium powder is 99.9 percent, and the average grain diameter is 200 meshes;
(2) Putting the porcelain boat into a vacuum tube furnace, vacuumizing, introducing helium, heating to 600 ℃ at the speed of 5 ℃/min under the protection of the helium, preserving heat for 1.5h, cooling to room temperature, and taking out a black product;
(3) Pouring the product into a beaker, adding 500mL of deionized water, putting the beaker into a heat collection type constant temperature heating magnetic stirrer, stirring at the stirring speed of 1200r/min at 100 ℃, preserving heat for 1h, and then cooling to room temperature;
(4) Continuously introducing CO into the solution for 1 hour under the stirring condition (the stirring speed is 1200 r/min) 2 Filtering, and drying the filter body in a vacuum drying oven at 100 ℃ for 12h to obtain a black carbon material, namely the carbon nanocages;
(5) And stirring the obtained filtrate for 2 hours at 100 ℃ at a stirring speed of 300r/min by using a heat collection type constant temperature heating magnetic stirrer to obtain the basic magnesium carbonate.
Putting the basic magnesium carbonate obtained in the step (5) into a vacuum drying oven, and drying for 12h at the temperature of 80 ℃; mixing with magnesium powder, and repeating the steps 1-5 to obtain the carbon nanocages prepared circularly.
And (3) performance testing:
the carbon nanocages prepared in the 1 st and 10 th cycles of example 1 were tested for their performance, and the results are shown in FIGS. 1-4.
Fig. 1,1a and 1b are transmission electron micrographs of carbon nanocages prepared at 1 st cycle and 10 th cycle respectively (the material obtained at the nth cycle is denoted as Ren, and the material obtained at the 10 th cycle is denoted as Re 10), and it can be seen from the transmission electron micrographs that the porous carbon is stacked together in a cage shape.
FIG. 2,2a is the X-ray diffraction pattern of the feedstock obtained over multiple cycles, illustrating CO 2 The MgO template can be effectively removed and finally converted into the basic magnesium carbonate raw material through a series of steps; 2b is an X-ray diffraction pattern of the carbon nano cage obtained by multiple cycles, and only has two crystal faces of carbon materials (002) and (100).
FIG. 3, in which the porous carbon obtained in 3a by multiple cycles is at 100 mVs -1 The carbon nanocages are rectangular at the sweeping speed, which shows that the prepared carbon nanocages have good rate performance; 3b is the mass specific capacitance of the material under different current densities, and the mass specific capacitance of the prepared carbon nanocage is reduced smoothly along with the continuous increase of the current density, which can be attributed to that the material contains more mesopores, so that the ion transmission under the high current density is increased.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A method for preparing a high-capacitance carbon nanocage in a green circulation manner is characterized by comprising the following steps: (1) Mixing basic magnesium carbonate and magnesium powder to obtain mixed powder; (2) Heating the mixed powder to 600-800 ℃ under the protection of inert gas, preserving heat for 1-2h, and cooling to room temperature to obtain black powder; (3) Adding deionized water into the black powder, stirring, heating to 80-100 deg.C, maintaining the temperature for 1-2h, and cooling to room temperature; (4) Stirring, continuously introducing carbon dioxide, filtering, and drying the filter to obtain carbon nanocages; (5) Collecting the filtered filtrate, stirring at 55-100 ℃, and preserving heat to obtain basic magnesium carbonate; taking the obtained basic magnesium carbonate as a raw material in the step (1) to realize circular preparation;
in the step (1), the mass ratio of the magnesium powder to the basic magnesium carbonate is 1:1-12.
2. The method for preparing the carbon nanocages with high capacitance performance in a green cycle according to claim 1, wherein the mass ratio of magnesium powder to basic magnesium carbonate is 1:1-8.
3. The green cycle method for preparing carbon nanocages with high capacitance performance according to claim 1 or 2, wherein in the step (2), the inert gas is argon or helium.
4. The green cycle method for preparing carbon nanocages with high capacitance performance according to claim 1 or 2, wherein in the step (2), the inert gas is high-purity argon with the purity of 99.99%.
5. The green cycle method for preparing carbon nanocages with high capacitance performance according to claim 1 or 2, wherein in the step (2), the temperature rise rate is 5-15 ℃/min.
6. The green circulation method for preparing the carbon nanocages with high capacitance performance according to claim 1 or 2, wherein in the step (3), the addition amount of deionized water is 1-3; the stirring speed is 800-1200r/min.
7. The method for preparing the carbon nanocages with high capacitance performance in a green cycle according to claim 1 or 2, wherein in the step (4), the stirring speed is 800-1200r/min; the introduction time of the carbon dioxide is 1-2h; the drying temperature is 80-100 ℃, and the drying time is 8-12h.
8. The green cycle method for preparing carbon nanocages with high capacitance performance as claimed in claim 1 or 2, wherein in the step (5), the stirring speed is 300-800r/min.
9. The green cycle method for preparing carbon nanocages with high capacitance performance according to claim 1 or 2, wherein the average particle size of the magnesium powder is 100-200 meshes.
10. A carbon nanocage, wherein the carbon nanocage is produced by the method according to any one of claims 1 to 9.
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