CN113603086B - Tartary buckwheat-based activated carbon material and preparation method and application thereof - Google Patents
Tartary buckwheat-based activated carbon material and preparation method and application thereof Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
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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
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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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
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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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
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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 tartary buckwheat-based activated carbon material, a preparation method and application thereof; the preparation method of the tartary buckwheat-based activated carbon material comprises the steps of coarse carbon preparation, pickling impurity removal, activation, pickling purification, high-temperature carbon supplementing and the like. The invention obtains the low-cost active carbon material, improves the purity of the active carbon, reduces the volatile matters and ash content of the material and reduces the content of oxygen-containing groups, thereby improving the electrochemical cycling stability of the active carbon material.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to a tartary buckwheat-based active carbon material, a preparation method and application thereof.
Background
With the development of economy, the problem of energy shortage is becoming more serious. The country also proposes to develop new energy greatly to achieve the aims of 'carbon reaching peak' and 'carbon neutralization'. Therefore, it is urgent to find a low-cost, high-performance and environment-friendly energy storage device. Super capacitor is used as a novel energy storage element, and has attracted attention due to the advantages of short charging time, high power density, green environment protection and the like.
Compared with a water system, the organic super capacitor has higher voltage and energy density, and can better meet the application requirements of people in the aspect of energy storage. Supercapacitors are classified into an electric double layer capacitor type, a pseudocapacitance type, and an electric double layer/pseudocapacitance hybrid type. The double-layer super capacitor mainly uses active carbon as an electrode material, and biomass carbon is one of the sources of the active carbon, and has the advantages of wide sources, environmental protection, low cost and the like, and draws attention. Through retrieval, biomass such as rice hulls, pine nut shells, straws and the like are adopted in the prior art as raw materials for preparing the supercapacitor active carbon, but the prepared active carbon has low purity, high ash content, high volatile content, high oxygen-containing groups and poor cycle performance, and the service life of the double-layer supercapacitor is influenced. Particularly under the condition of organic high-voltage operation, the capacity of the carbon material is fast in decay, and impurities introduce defects into the carbon material, so that the carbon material cannot resist high voltage and has serious self-discharge phenomenon. In addition, in the initial operation stage, the existing active carbon electrode materials are subjected to the process of capacity rapid attenuation and stable circulation, which inevitably leads to the loss of specific capacity of the electrode materials and the reduction of the utilization efficiency of the materials. In summary, the preparation of the supercapacitor activated carbon with low cost, high purity, long cycle performance and high utilization rate and the simple and rapid preparation process are the problems which are urgently solved by the current industry.
Disclosure of Invention
The invention aims to provide a tartary buckwheat-based activated carbon material, a preparation method and application thereof, and the preparation method and application thereof are used for obtaining the low-cost activated carbon material, improving the purity of the activated carbon, reducing the volatile matters and ash content of the material and reducing the content of oxygen-containing groups, so that the electrochemical cycling stability of the activated carbon material is improved.
In order to achieve the above purpose, the present invention adopts the technical scheme that:
the invention discloses a preparation method of a tartary buckwheat-based activated carbon material, which comprises the following steps:
(1) Preparing coarse carbon: heating and carbonizing the tartary buckwheat base powder under the protection of inert gas to obtain coarse carbon powder;
(2) Acid washing and impurity removal: placing the crude carbon powder into acid liquor for washing;
(3) Activating: mixing the carbon material obtained after acid washing with alkali liquor, and then heating and activating under the protection of inert gas;
(4) Acid washing and purification: placing the activated carbon material obtained after activation into acid liquor for washing;
(5) High-temperature carbon supplement: and mixing the activated carbon material obtained after acid washing with a solid carbon supplementing agent, and calcining to obtain the tartary buckwheat-based activated carbon material.
In the step (1), the tartary buckwheat base powder is obtained by crushing one or more raw materials of tartary buckwheat, tartary buckwheat stems and tartary buckwheat husks to 80-200 meshes.
As a preferable technical scheme, in the step (1), the heating and carbonizing temperature is 400-800 ℃, and the heating and carbonizing time is 1-5 hours.
In the step (2), the crude carbon powder is placed in hydrochloric acid solution with the mass fraction of 3% -20%, and is continuously soaked and washed for 5-24 hours at the temperature of 60-95 ℃, washed with water to be neutral, and then dried.
In the step (3), the carbon material obtained after acid washing is mixed with alkali liquor, soaked and dried, then heated to 600-1300 ℃ for activation for 1-5 hours under the protection of inert gas, washed with water to be neutral, and then dried.
In the step (3), the alkali solution is one or more of sodium hydroxide and potassium hydroxide solution.
In the step (4), the activated carbon material is placed in hydrochloric acid solution with the mass fraction of 3% -20%, and is continuously soaked and washed for 5-24 hours at the temperature of 60-95 ℃, washed with water to be neutral, and then dried.
In the step (5), the activated carbon material obtained after acid washing is mixed with the solid carbon supplementing agent according to the mass ratio of 1:1-1:10, and then the mixture is continuously calcined at 300-1300 ℃ for 1-5 hours, so that the tartary buckwheat-based activated carbon material is obtained.
In the step (5), the solid carbon supplementing agent is one or more of polyethylene, polypropylene and polybutylene.
The invention also discloses the tartary buckwheat-based activated carbon material prepared by the preparation method.
The invention also discloses application of the tartary buckwheat-based activated carbon material in a capacitor energy storage device.
The invention also discloses application of the tartary buckwheat-based activated carbon material in an electrode material.
The invention has the beneficial effects that:
1. the invention adopts the method of material pulverization, crude carbon preparation, acid washing impurity removal, activation, acid washing purification and high-temperature carbon supplement, and the specific surface area range of the prepared active carbon material is highly controllable (the conventional range is 1000-2000 m) 2 /g; maximum value: 2280m 2 And/g), the pore distribution is relatively uniform, the mesoporous is more, the average pore diameter is about 2.03-2.7nm, the ash content of the obtained material is as low as 0.09%, the volatile content is as low as 0.22%, and the oxygen content is lower.
2. The invention adopts polyethylene, polypropylene and the like as solid carbon-supplementing agents, can greatly simplify the process of adopting dangerous gas carbon sources (such as methane, ethylene and the like) in the traditional high-temperature carbon-supplementing process, can efficiently reduce volatile matters and oxygen-containing group content, and can repair the defects of macropores caused by alkali etching and improve the electrochemical cycling stability of the carbon material.
3. In the test of the organic super capacitor, after 20000 cycles of constant current density of 1A/g, the coulomb efficiency of the active carbon material prepared by the invention is 100%, the specific capacitance is 28.4F/g, and the capacity maintenance rate is more than 90%, so that the application index of the super capacitor active carbon can be fully satisfied. In the initial stage of the cycle, the assembled super capacitor does not have the phenomenon of abrupt attenuation of specific capacity.
4. The carbon raw material of the invention is tartary buckwheat crops (such as tartary buckwheat, tartary buckwheat stems, tartary buckwheat husks, and the like) planted in a large area in Chuan Yuan Qian region, the comprehensive cost is low, the invention has market competitiveness, and the tartary buckwheat contains abundant bioflavonoids, amino acids, oleic acid and linoleic acid, and also contains various inorganic elements such as calcium, phosphorus, iron, magnesium, copper, zinc, trace element selenium, and the like, so the tartary buckwheat can be used as the raw material to prepare the carbon material doped with special elements, thereby endowing the carbon material with new performances.
Drawings
FIG. 1 is a scanning electron microscope image I of the tartary buckwheat-based activated carbon material obtained in example 1;
FIG. 2 is a second SEM image of the tartary buckwheat-based activated carbon material obtained in example 1;
FIG. 3 is a CV curve of the tartary buckwheat-based activated carbon material obtained in example 1;
FIG. 4 is a graph showing the results of the charge-discharge stability test of the tartary buckwheat-based activated carbon material obtained in example 1.
FIG. 5 is a CV curve of the tartary buckwheat-based activated carbon material obtained in example 2;
FIG. 6 is a graph showing the results of the charge-discharge stability test of the tartary buckwheat-based activated carbon material obtained in example 2;
FIG. 7 is a CV plot of the tartary buckwheat-based activated carbon material obtained in example 3;
FIG. 8 is a graph showing the results of the charge-discharge stability test of the tartary buckwheat-based activated carbon material obtained in example 3.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent.
Example 1
(1) Preparing coarse carbon: carbonizing 80-mesh tartary buckwheat powder at a constant temperature of 3 ℃/min to 400 ℃ for 2 hours under an argon atmosphere to obtain coarse carbon powder;
(2) Acid washing and impurity removal: naturally cooling the crude carbon powder, taking out, placing the crude carbon powder and 10wt% hydrochloric acid into a high-pressure reaction kettle, continuously soaking and washing for 24 hours at 80 ℃, washing with water to be neutral, and drying;
(3) Activating: mixing and soaking the carbon material obtained after acid washing and sodium hydroxide for 2 hours according to the mass ratio of 1:1.5, then drying, heating to 900 ℃ at 3 ℃/min under argon atmosphere, preserving heat for 2 hours, washing with water to be neutral, and then drying;
(4) Acid washing and purification: placing the activated carbon material obtained after activation and 10wt% hydrochloric acid into a high-pressure reaction kettle, continuously soaking and washing for 24 hours at 80 ℃, washing with water to be neutral, and then drying;
(5) High-temperature carbon supplement: mixing the activated carbon material obtained after acid washing with polypropylene according to the mass ratio of 1:8, calcining at 900 ℃ and preserving heat for 2 hours, thereby obtaining the tartary buckwheat-based activated carbon material.
The scanning electron microscope images of the tartary buckwheat-based active carbon material obtained in the embodiment 1 are shown in fig. 1 and 2, and the specific surface area of the tartary buckwheat-based active carbon material can reach 2289m after test 2 Per g, an average pore diameter of about 2.03nm,
the tartary buckwheat-based activated carbon material obtained in the example 1 is tested for ash content according to a GB/T1429 method and for volatile matters according to a YB/T5189 method, and the test result shows that the ash content is as low as 0.09% and the volatile matters are as low as 0.22%.
Uniformly mixing the tartary buckwheat-based activated carbon material obtained in the example 1 with conductive carbon black, sodium carboxymethylcellulose (CMC) and Styrene Butadiene Rubber (SBR) according to a certain proportion, adding an aqueous solvent to prepare negative electrode slurry, and uniformly coating the negative electrode slurry on an aluminum foil (the coating thickness is about 300 mu m; the surface load of the activated carbon is higher than 5 mg/cm) 2 ) Drying in vacuum drying oven at 90deg.C for 12 hr, rolling, and punchingAnd cutting to obtain the electrode plate. And (3) respectively taking the obtained electrode plates as positive and negative electrodes, and assembling the electrode plates into a full-cell device (comprising 2025/2032 button cells, winding cells, soft-packed cells and the like) in a glove box with an argon protective atmosphere of which the water and the oxygen are less than 0.1ppm, wherein the electrolyte is purchased new-world-side 3702 electrolyte. Electrochemical testing at a scan rate of 10mV/s was performed through a CHI660D electrochemical workstation, and the resulting cyclic voltammogram is shown in FIG. 3; the constant current charge and discharge performance test of the whole battery is carried out by adopting the Wuhan blue electric battery test system, and the battery cycle test result is shown in figure 4 under the 1A/g running condition, and the result shows that after 20000 cycles, the coulombic efficiency is 100%, and the capacity retention rate is more than 90%.
Example 2
(1) Preparing coarse carbon: carbonizing 80-mesh tartary buckwheat powder at a constant temperature of 3 ℃/min to 400 ℃ for 2 hours under an argon atmosphere to obtain coarse carbon powder;
(2) Acid washing and impurity removal: naturally cooling the crude carbon powder, taking out, placing the crude carbon powder and 10wt% hydrochloric acid into a high-pressure reaction kettle, continuously soaking and washing for 24 hours at 80 ℃, washing with water to be neutral, and drying;
(3) Activating: mixing and soaking the carbon material obtained after acid washing and sodium hydroxide for 2 hours according to the mass ratio of 1:1.5, then drying, heating to 1100 ℃ at 3 ℃/min under argon atmosphere, preserving heat for 2 hours, washing with water to be neutral, and then drying;
(4) Acid washing and purification: placing the activated carbon material obtained after activation and 10wt% hydrochloric acid into a high-pressure reaction kettle, continuously soaking and washing for 24 hours at 80 ℃, washing with water to be neutral, and then drying;
(5) High-temperature carbon supplement: mixing the activated carbon material obtained after acid washing with polypropylene according to the mass ratio of 1:8, calcining at 1100 ℃ and preserving heat for 2 hours, thereby obtaining the tartary buckwheat-based activated carbon material.
The specific surface area of the tartary buckwheat-based activated carbon material obtained in the embodiment 2 can reach 2087m 2 And/g, the average pore diameter is about 2.10 nm.
The tartary buckwheat-based activated carbon material obtained in the example 2 is tested for ash content according to a GB/T1429 method and for volatile content according to a YB/T5189 method, and the test result shows that the ash content is as low as 0.1% and the volatile content is as low as 1.15%.
Uniformly mixing the tartary buckwheat-based activated carbon material obtained in the example 2 with conductive carbon black, sodium carboxymethylcellulose (CMC) and Styrene Butadiene Rubber (SBR) according to a certain proportion, adding an aqueous solvent to prepare negative electrode slurry, and uniformly coating the negative electrode slurry on an aluminum foil (the coating thickness is about 300 mu m; the surface load of the activated carbon is higher than 5 mg/cm) 2 ) Drying for 12 hours at 90 ℃ in a vacuum drying oven, and rolling and blanking to obtain the electrode plate. And (3) respectively taking the obtained electrode plates as positive and negative electrodes, and assembling the electrode plates into a full-cell device (comprising 2025/2032 button cells, winding cells, soft-packed cells and the like) in a glove box with an argon protective atmosphere of which the water and the oxygen are less than 0.1ppm, wherein the electrolyte is purchased new-world-side 3702 electrolyte. Electrochemical testing at a scan rate of 10mV/s was performed through a CHI660D electrochemical workstation, and the resulting cyclic voltammogram is shown in FIG. 5; the constant current charge and discharge performance test of the whole battery is carried out by adopting the Wuhan blue electric battery test system, and the battery cycle test result is shown in figure 6 under the 1A/g running condition, and the result shows that after 20000 cycles, the coulombic efficiency is 100%, and the capacity retention rate is more than 89%.
Example 3
(1) Preparing coarse carbon: carbonizing 80-mesh tartary buckwheat powder at a constant temperature of 3 ℃/min to 400 ℃ for 2 hours under an argon atmosphere to obtain coarse carbon powder;
(2) Acid washing and impurity removal: naturally cooling the crude carbon powder, taking out, placing the crude carbon powder and 10wt% hydrochloric acid into a high-pressure reaction kettle, continuously soaking and washing for 24 hours at 80 ℃, washing with water to be neutral, and drying;
(3) Activating: mixing and soaking the carbon material obtained after acid washing and sodium hydroxide for 2 hours according to the mass ratio of 1:1.5, then drying, heating to 1300 ℃ at 3 ℃/min under argon atmosphere, preserving heat for 2 hours, washing with water to be neutral, and then drying;
(4) Acid washing and purification: placing the activated carbon material obtained after activation and 10wt% hydrochloric acid into a high-pressure reaction kettle, continuously soaking and washing for 24 hours at 80 ℃, washing with water to be neutral, and then drying;
(5) High-temperature carbon supplement: mixing the activated carbon material obtained after acid washing with polyethylene according to the mass ratio of 1:5, calcining at 1300 ℃ and preserving heat for 2 hours, thereby obtaining the tartary buckwheat-based activated carbon material.
The specific surface area of the tartary buckwheat-based activated carbon material obtained in the embodiment 3 can reach 1565m 2 And/g, the average pore diameter is about 2.18 nm.
The tartary buckwheat-based activated carbon material obtained in the example 3 is tested for ash content according to a GB/T1429 method and for volatile matters according to a YB/T5189 method, and the test result shows that the ash content is as low as 0.043% and the volatile matters are as low as 1.34%.
Uniformly mixing the tartary buckwheat-based activated carbon material obtained in the example 3 with conductive carbon black, sodium carboxymethylcellulose (CMC) and Styrene Butadiene Rubber (SBR) according to a certain proportion, adding an aqueous solvent to prepare negative electrode slurry, and uniformly coating the negative electrode slurry on an aluminum foil (the coating thickness is about 300 mu m; the surface load of the activated carbon is higher than 5 mg/cm) 2 ) Drying for 12 hours at 90 ℃ in a vacuum drying oven, and rolling and blanking to obtain the electrode plate. And (3) respectively taking the obtained electrode plates as positive and negative electrodes, and assembling the electrode plates into a full-cell device (comprising 2025/2032 button cells, winding cells, soft-packed cells and the like) in a glove box with an argon protective atmosphere of which the water and the oxygen are less than 0.1ppm, wherein the electrolyte is purchased new-world-side 3702 electrolyte. Electrochemical testing at a scan rate of 10mV/s was performed through a CHI660D electrochemical workstation, and the resulting cyclic voltammogram is shown in FIG. 7; the constant current charge and discharge performance test of the whole battery is carried out by adopting the Wuhan blue electric battery test system, and the battery cycle test result is shown in figure 8 under the 1A/g running condition, and the result shows that after 20000 cycles, the coulombic efficiency is 100%, and the capacity retention rate is more than 90%.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A preparation method of a tartary buckwheat-based activated carbon material is characterized by comprising the following steps: the method comprises the following steps:
(1) Heating and carbonizing the tartary buckwheat base powder under the protection of inert gas, wherein the heating and carbonizing temperature is 400-800 ℃, and the heating and carbonizing time is 1-5 hours, so as to obtain coarse carbon powder;
(2) Placing the crude carbon powder into acid liquor for washing;
(3) Mixing the carbon material obtained after acid washing with alkali liquor, soaking, drying, heating to 600-1300 ℃ under the protection of inert gas, activating for 1-5 hours, washing with water to be neutral, and drying;
(4) Placing the activated carbon material obtained after activation into acid liquor for washing;
(5) Mixing the activated carbon material obtained after acid washing with a solid carbon supplementing agent in a mass ratio of 1:1-1:10, wherein the solid carbon supplementing agent is one or more of polyethylene, polypropylene and polybutylene, and then continuously calcining at 300-1300 ℃ for 1-5 hours to obtain the tartary buckwheat-based activated carbon material.
2. The method for preparing the tartary buckwheat-based activated carbon material according to claim 1, which is characterized in that: in the step (1), the tartary buckwheat base powder is obtained by crushing one or more raw materials of tartary buckwheat, tartary buckwheat stems and tartary buckwheat husks to 80-200 meshes.
3. The method for preparing the tartary buckwheat-based activated carbon material according to claim 1, which is characterized in that: in the step (2), the crude carbon powder is placed in hydrochloric acid solution with the mass fraction of 3% -20%, and is continuously soaked and washed for 5-24 hours at the temperature of 60-95 ℃, washed to be neutral by water, and then dried.
4. The method for preparing the tartary buckwheat-based activated carbon material according to claim 1, which is characterized in that: in the step (3), the alkali liquor is one or more of sodium hydroxide and potassium hydroxide solution.
5. The method for preparing the tartary buckwheat-based activated carbon material according to claim 1, which is characterized in that: in the step (4), the activated carbon material obtained after activation is placed in hydrochloric acid solution with the mass fraction of 3% -20%, and is continuously soaked and washed for 5-24 hours at the temperature of 60-95 ℃, washed to be neutral by water, and then dried.
6. A tartary buckwheat-based activated carbon material prepared by the preparation method of any one of claims 1 to 5.
7. The use of the tartary buckwheat-based activated carbon material of claim 6 in a capacitor energy storage device.
8. The use of the tartary buckwheat-based activated carbon material of claim 6 in an electrode material.
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