CN112624111A - Preparation method of metal-catalyzed corn straw derived carbon electrode material - Google Patents
Preparation method of metal-catalyzed corn straw derived carbon electrode material Download PDFInfo
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- 235000002017 Zea mays subsp mays Nutrition 0.000 title claims abstract description 42
- 235000005822 corn Nutrition 0.000 title claims abstract description 42
- 239000010902 straw Substances 0.000 title claims abstract description 42
- 239000007772 electrode material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 10
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- 229910021645 metal ion Inorganic materials 0.000 claims description 10
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- 239000003575 carbonaceous material Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
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- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000004913 activation Effects 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims description 2
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- 238000000034 method Methods 0.000 abstract description 6
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- 238000012360 testing method Methods 0.000 abstract description 5
- 239000012776 electronic material Substances 0.000 abstract description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract 1
- 230000014759 maintenance of location Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- 229910052742 iron Inorganic materials 0.000 description 8
- 239000003990 capacitor Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
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- 239000002253 acid Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 4
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- 239000002803 fossil fuel Substances 0.000 description 3
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
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- 238000010586 diagram Methods 0.000 description 2
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- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- 239000011780 sodium chloride Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- 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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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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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- 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
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Abstract
The invention relates to a preparation method of a metal-catalyzed corn straw derived carbon electrode material, belonging to the technical field of new energy electronic materials. The obtained electrode material is cheap and easy to obtain, the process is simple, and the electrochemical performance is excellent. The preparation method comprises the following steps: pre-carbonizing the cleaned corn straw cores at 300 ℃ in Ar atmosphere; mixing the pre-carbonized product with 0.05 mol/L FeCl3·6H2O doping, drying and then mixing the sample with KOH in a ratio of 1:3, preserving the heat for 1 h at 700 ℃; the obtained product is washed by dilute hydrochloric acid solution, dried and subjected to sample preparation and test. The prepared metal-catalyzed corn straw derived carbon electrode material is prepared in 1 Ag‑1The specific capacitance value is 430.8 g‑1，10 A g‑1The capacity retention rate reaches 1 Ag‑174.2% of the total weight, the electrochemical performance was excellent. The metal-catalyzed straw-derived carbon electrode material prepared by the method has the advantages of low cost, stable structure, excellent electrochemical performance and high practical application value.
Description
Technical Field
The invention belongs to the technical field of new energy electronic materials, and relates to a preparation method of a corn straw derived carbon electrode material through metal catalysis.
Background
With the rapid development of the economy of China for the past decades, fossil fuels are widely exploited and utilized in various fields of economic construction of China. However, the development and use of fossil fuels without control causes serious damage to the natural environment and global warming of the climate, resulting in irreparable damage to the ecological environment. Therefore, the development of novel renewable energy storage devices, such as solar energy, wind energy, lithium ion batteries, super capacitors and the like, is considered as an effective measure for solving the problems of high pollution and high energy consumption of fossil fuels and realizing sustainable development of human beings. The super capacitor is favored by people due to the advantages of high charge-discharge rate, high specific capacity and the like, wherein the biomass material is widely distributed, cheap and easy to obtain, so the super capacitor is concerned by people in the research field of electrode materials.
The corn stalks are widely distributed in a wide area in northern China and consist of cellulose, hemicellulose and lignin, wherein the cellulose constitutes fibers, and the hemicellulose and the lignin are filled between microfine fibers and fiber cells as an adhesive, so that the plants are kept upright and have certain rigidity. The corn straw biomass carbon is prepared by carbonizing straws under the conditions of high temperature and oxygen deficiency, has the characteristics of developed pores, large specific surface area, rich organic functional groups on the surface and the like, and has the advantages of rich raw materials, low price and potential application prospect. In order to further develop the application of the corn stalks in the aspect of electrode materials of the super capacitor, the corn stalks are further researched to obtain better electrochemical performance. (preparation of pure plum, corn straw-based biomass carbon material and electrochemical performance research thereof [ D ] Jilin university, 2018.)
To improve the electrochemical performance of corn stover-derived carbon electrode materials, Li et al have used corn stover with LiCl/ZnCl 2After mixing, the samples were heated at 800 ℃ for 10 h before mixing with K2C2O4、CaCO3Adding the materials according to the optimal proportion, carbonizing the materials at 800 ℃ for 2 hours, and then washing the materials by HCl and deionized water respectively, wherein the specific capacitance of the obtained product can reach 375F/g under the current density of 0.5A/g; gao et al freeze-dry corn stalks in liquid nitrogen, carbonize the sample at 1100 deg.C for one hour in Ar gas environment, and obtain a product at 0.2The specific capacitance can reach 116F/g under the current density of 5A/g; li et al prepared by mixing corn stover with K2C2O4、CaCO3Mixing and grinding, then carbonizing and preserving heat for one hour at 300 ℃, then preserving heat for two hours at 800 ℃, and obtaining the porous carbon material with the specific capacitance reaching 461F/g under the current density of 0.5A/g; wang et al added chopped corn stalks to a mixed solution of KCl and NaCl and soaked for 12 hours, then the mixture was carbonized by heat preservation at 800 ℃ for three hours in an air environment, the sample was washed with hydrochloric acid and dried, and the specific capacitance of the obtained sample was 407F/g at a current density of 1A/g. The invention takes the corn straws found in the farmland as the raw material, has rich sources, is cheap and is easy to obtain; the corn straw derived carbon electrode material catalyzed by metal ions obtained by doping metal ions with different concentrations, activating by KOH, carbonizing at high temperature and the like has excellent electrochemical performance as a super capacitor electrode material, the specific capacitance is 430.8F/g under the current density of 1A/g, and the specific capacitance is 320F/g under the current density of 10A/g; and 74.2% of the specific capacity under the current density of 1A/g can be reserved under the current density of 10A/g, and the high-power-factor-performance capacitor has good power performance.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method and application of a metal-catalyzed corn straw derived carbon electrode material with higher specific capacitance and better cycle performance.
The technical scheme of the invention is as follows:
according to the invention, the preparation method of the biomass porous carbon material comprises the following steps:
(1) cleaning and drying fresh straws by deionized water, cutting corn straw cores into pieces, putting the cut corn straw cores into a clean porcelain boat, moving the porcelain boat into an Ar atmosphere tube furnace, heating the porcelain boat to 300 ℃ at the heating rate of 5 ℃/min, and preserving heat for 1 h at the temperature to obtain a pre-carbonized corn straw core product;
(2) taking 0.275g of the pre-carbonized corn straw core obtained in the step (1), and respectively mixing with 25ml of FeCl with the concentration of 0.04-0.06 mol/L3· 6H2Mixing O solution, stirring for 24 hr, centrifuging, and collecting the filtrate at 55Drying in a drying oven at the temperature of DEG C;
(3) immersing the dried metal ion-doped pre-carbonized product obtained in the step (2) into a KOH solution (the mass ratio of the pre-carbonized product to KOH is 1: 0.5-1: 5), stirring for one hour, and then putting the mixed solution into a 55 ℃ drying oven for drying:
(4) activating the sample obtained in the step (3) for 1-3 hours at 650-750 ℃ in Ar atmosphere;
(5) washing the product obtained in the step (4) by using a dilute hydrochloric acid solution, and then washing the product by using deionized water and absolute ethyl alcohol until the solution is neutral;
(6) and (5) drying the product obtained in the step (5) at 55 ℃ for 12 h to obtain the metal catalytic straw derived carbon material.
According to the present invention, it is preferable that the concentration of the metal ions doped in the step (2) is 0.05 mol/L.
According to the present invention, it is preferred that the mass ratio of the pre-carbonized product to KOH in step (3) is 1: 3.
According to the present invention, it is preferred that the activation temperature in step (4) is 700 ℃.
According to the present invention, it is preferable that the activation time in the step (4) is 1 hour.
The technical advantages of the invention are as follows:
(1) the invention has the advantages of wide sources of raw materials, low price, easy obtainment, simple preparation process and controllability, and can change the catalytic action on the corn straw derived carbon by changing the concentrations of different metal ions.
(2) The metal-catalyzed corn straw derived carbon electrode material prepared by the invention has a three-dimensional porous shape.
(3) The metal-catalyzed corn straw derived carbon electrode material prepared by the invention has the advantages of stable structure, excellent electrochemical performance, good cycle performance, high specific capacitance and the like, and is very suitable for being applied to the field of supercapacitors as an electrode material.
Drawings
FIG. 1 is a scanning electron microscope image of the metal-catalyzed straw-derived carbon material prepared in example 1 of the present invention.
FIG. 2 is a constant current impulse discharge diagram of the metal-catalyzed straw-derived carbon material prepared in example 1 and comparative example of the present invention.
FIG. 3 is a specific capacitance diagram of the metal-catalyzed straw-derived carbon material prepared in example 1 of the present invention and a comparative example.
Detailed Description
The present invention will be further described with reference to the following embodiments and drawings, but is not limited thereto.
Meanwhile, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1:
putting the cleaned corn straw cores into a clean porcelain boat, putting the porcelain boat into an atmosphere tube furnace, heating to 300 ℃ at a heating rate of 5 ℃/min under Ar atmosphere, preserving heat for 1 h at the temperature, and carrying out a pre-carbonization process; taking 0.275g of pre-carbonized corn straw core and 25ml of FeCl with the concentration of 0.05 mol/L3· 6H2Mixing the O solution, stirring for 24 hours, centrifuging and drying in an oven at 55 ℃; immersing the pre-carbonized product doped with the dried metal ions into KOH solution (m)Pre-carbonized product：mKOH=1: 3), after magnetically stirring for one hour, putting the mixed solution into an oven at 55 ℃ for drying; transferring the dried sample into an iron crucible, putting the iron crucible into an atmosphere tube furnace, heating to 700 ℃ at the heating rate of 5 ℃/min under the Ar atmosphere, and preserving heat for 1 h at the temperature to obtain a product; and finally, carrying out acid washing on the product by using 1 mol/L HCl solution, and drying the product to carry out sample preparation test.
Example 2:
putting the cleaned corn straw cores into a clean porcelain boat, putting the porcelain boat into an atmosphere tube furnace, heating to 300 ℃ at a heating rate of 5 ℃/min under Ar atmosphere, preserving heat for 1 h at the temperature, and carrying out a pre-carbonization process; taking 0.275g of pre-carbonized corn straw core and 25ml of FeCl with the concentration of 0.04 mol/L3· 6H2Mixing the O solution, stirring for 24 hours, centrifuging and drying in an oven at 55 ℃;immersing the pre-carbonized product doped with the dried metal ions into KOH solution (m)Pre-carbonized product：mKOH=1: 3), after magnetically stirring for one hour, putting the mixed solution into an oven at 55 ℃ for drying; transferring the dried sample into an iron crucible, putting the iron crucible into an atmosphere tube furnace, heating to 700 ℃ at the heating rate of 5 ℃/min under the Ar atmosphere, and preserving heat for 1 h at the temperature to obtain a product; and finally, carrying out acid washing on the product by using 1 mol/L HCl solution, and drying the product to carry out sample preparation test.
Example 3:
putting the cleaned corn straw cores into a clean porcelain boat, putting the porcelain boat into an atmosphere tube furnace, heating to 300 ℃ at a heating rate of 5 ℃/min under Ar atmosphere, preserving heat for 1 h at the temperature, and carrying out a pre-carbonization process; taking 0.275g of pre-carbonized corn straw core and 25ml of FeCl with the concentration of 0.06 mol/L3· 6H2Mixing the O solution, stirring for 24 hours, centrifuging and drying in an oven at 55 ℃; immersing the pre-carbonized product doped with the dried metal ions into KOH solution (m)Pre-carbonized product：mKOH=1: 3), after magnetically stirring for one hour, putting the mixed solution into an oven at 55 ℃ for drying; transferring the dried sample into an iron crucible, putting the iron crucible into an atmosphere tube furnace, heating to 700 ℃ at the heating rate of 5 ℃/min under the Ar atmosphere, and preserving heat for 1 h at the temperature to obtain a product; and finally, carrying out acid washing on the product by using 1 mol/L HCl solution, and drying the product to carry out sample preparation test.
Comparative example:
putting the cleaned corn straw cores into a clean porcelain boat, putting the porcelain boat into an atmosphere tube furnace, heating to 300 ℃ at a heating rate of 5 ℃/min under Ar atmosphere, preserving heat for 1 h at the temperature, and carrying out a pre-carbonization process; immersing the pre-carbonized product in KOH solution (m)Pre-carbonized product：mKOH=1: 3), after magnetically stirring for one hour, putting the mixed solution into an oven at 55 ℃ for drying; transferring the dried sample into an iron crucible, putting the iron crucible into an atmosphere tube furnace, heating to 700 ℃ at the heating rate of 5 ℃/min under the Ar atmosphere, and preserving heat for 1 h at the temperature to obtain a product; and finally, carrying out acid washing on the product by using 1 mol/L HCl solution, and drying the product to carry out sample preparation test.
Claims (2)
1. The preparation method of the metal-catalyzed corn straw derived carbon electrode material is characterized by wide raw material source, simple operation, low cost and easy obtainment and catalysis by metal ions with different concentrations.
2. A preparation method of the electrode material of the supercapacitor, which comprises the following steps:
(1) cleaning and drying fresh straws by deionized water, cutting corn straw cores into pieces, putting the cut corn straw cores into a clean porcelain boat, moving the porcelain boat into an Ar gas tube furnace, heating the porcelain boat to 300 ℃ at the heating rate of 5 ℃/min, and preserving heat for 1 h at the temperature to obtain a pre-carbonized corn straw core product;
(2) taking 0.275g of the pre-carbonized corn straw core obtained in the step (1), and respectively mixing with 25ml of FeCl with the concentration of 0.04-0.06 mol/L3· 6H2Mixing the O solution, stirring for 24 hours, centrifuging, and drying in an oven at 55 ℃;
(3) immersing the metal ion-doped pre-carbonized product obtained in the step (2) into a KOH solution (the mass ratio of the pre-carbonized product to KOH is 1: 0.5-1: 5), stirring for one hour, and then putting the mixed solution into a 55 ℃ oven for drying:
(4) activating the sample obtained in the step (3) for 1-3 hours at 650-750 ℃ in Ar atmosphere;
(5) washing the product obtained in the step (4) by using a dilute hydrochloric acid solution, and then washing the product by using deionized water and absolute ethyl alcohol until the solution is neutral;
(6) drying the product obtained in the step (5) at 55 ℃ for 12 h to obtain the metal-catalyzed corn straw porous carbon material;
according to the present invention, it is preferable that the concentration of the metal ions doped in the step (2) is 0.05 mol/L;
according to the present invention, it is preferred that the mass ratio of the pre-carbonized product to KOH in step (3) is 1: 3;
according to the present invention, it is preferable that the activation temperature in the step (4) is 700 ℃;
according to the present invention, it is preferable that the activation time in the step (4) is 1 hour;
the technical advantages of the invention are as follows:
(1) the preparation raw materials are wide in source, cheap and easy to obtain, the preparation process is simple, controllability is realized, and the catalytic action on the corn straw derived carbon can be changed by changing the types of different metal ions;
(2) the metal-catalyzed corn straw derived carbon electrode material prepared by the invention has a three-dimensional porous shape;
(3) the metal-catalyzed corn straw derived carbon electrode material prepared by the invention has the advantages of stable structure, excellent electrochemical performance, good cycle performance, high specific capacitance and the like, and is very suitable for being applied to the field of supercapacitors as an electrode material.
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Cited By (2)
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| CN113880086A (en) * | 2021-10-30 | 2022-01-04 | 中国海洋大学 | Preparation method of nitrogen-phosphorus co-doped biomass derived capacitive deionization electrode |
| CN117735527A (en) * | 2024-02-21 | 2024-03-22 | 山东埃尔派粉体科技股份有限公司 | Biomass hard carbon anode material, preparation method thereof and sodium ion battery based on biomass hard carbon anode material |
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