CN111892051B - Biomass graded porous carbon for capacitor electrode material and preparation method thereof - Google Patents
Biomass graded porous carbon for capacitor electrode material and preparation method thereof Download PDFInfo
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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
- 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
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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
- 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
- H01G11/22—Electrodes
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- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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 provides biomass graded porous carbon for a capacitor electrode material and a preparation method thereof, wherein the method comprises the following steps: s1, adding camellia oleifera shell powder, urea and deionized water into a reaction kettle, heating to perform hydrothermal carbonization reaction, taking out products after the reaction, and respectively washing and drying to obtain hydrothermal carbonized products; s2, carbonizing the hydrothermal carbonized product and KOH, (NH) 4 ) 3 PO 4 Uniformly mixing, placing in a tube furnace, heating and activating under the protection of nitrogen atmosphere, and cooling to room temperature after activating to obtain an activated product; s3, soaking the activated product in hydrochloric acid solution to remove impurities, washing with deionized water, filtering and drying to obtain the graded porous carbon. The biomass hierarchical porous carbon prepared by the method is of a hierarchical porous structure comprising micropores, mesopores and macropores, and has the advantages of high capacity, good cycle performance and the like when being used as an electrode material of a supercapacitor.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to biomass hierarchical porous carbon for a capacitor electrode material and a preparation method thereof.
Background
The super capacitor is a novel energy storage device, has the advantages of quick charge and discharge, high efficiency, good stability and the like, has great market potential, and is a novel green energy source in the 21 st century. Currently, electrode materials for supercapacitors are mainly carbon materials, and active carbon materials are mainly used in the market, and the electrode materials for supercapacitors have the characteristics of low cost and high specific surface area, which are necessary for the electrode materials for supercapacitors. However, the conductivity of activated carbon is generally such that the microstructure exists mainly in the form of micropores, and therefore, there is a great resistance in the electrolyte, the process of impregnating the electrodes with the electrolyte is slow, and the process of storing and transporting charges is slow. Therefore, the electrode material with good performance and low cost is the main research direction in the field of the current super capacitor, so that the super capacitor with excellent performance and low cost can be prepared and can be widely applied to the market.
Through research on the supercapacitor electrode material, the porous carbon material is found to have an important influence on the electrochemical performance of the supercapacitor electrode material. The shell activated carbon is a porous carbon material prepared from carbon-containing organic matters through carbonization and activation processes, has better selective adsorption capacity and potential application value, and the oil tea shells are gradually valued due to high yield and low cost. The oil tea is a special woody edible oil tree seed in China, is mainly distributed in the provinces of Hunan, jiangxi, guangxi, guangdong, zhejiang, guizhou, yunnan and the like. The oil tea fruit consists of oil tea fruit shell and seed. The oil tea fruit shell accounts for more than 60% of the whole oil tea fruit mass, and the components of the oil tea fruit shell contain cellulose, hemicellulose, lignin, tannin and other substances. According to statistics, the existing national camellia oleifera cultivation area reaches 400 ten thousand hectares, and the annual camellia oleifera fruit bodies reach more than 560 ten thousand tons, which brings about 300 ten thousand tons of camellia oleifera shells. At present, oil tea kernels are used for processing into tea oil, shells often become residues, most of the residues are directly discarded or burnt, the processing belongs to typical rough production, the economic benefit is low, the additional value is not high, and great resource waste and environmental pollution are caused. Therefore, how to fully utilize the waste to prepare high added value products, such as report of preparing porous carbon by using camellia oleifera shells to be used as an electrode material of a supercapacitor, realizes intensive production, and is one of the key points of research of camellia oleifera industry.
Disclosure of Invention
In order to solve the technical problems, the first aspect of the invention provides a preparation method of biomass graded porous carbon for capacitor electrode materials, which comprises the following steps:
s1, adding camellia oleifera shell powder, urea and deionized water into a reaction kettle, heating to perform hydrothermal carbonization reaction, taking out products after the reaction, and respectively washing and drying to obtain hydrothermal carbonized products;
s2, willThe hydrothermal carbonized product prepared in the step S1, KOH and (NH) 4 ) 3 PO 4 Uniformly mixing, placing in a tube furnace, heating and activating under the protection of nitrogen atmosphere, and cooling to room temperature after activating to obtain an activated product;
s3, soaking the activated product prepared in the step S2 in hydrochloric acid solution to remove impurities, and then washing with deionized water, filtering and drying to obtain the graded porous carbon.
Wherein the mesh number of the oil tea fruit shell powder is 100-200 mesh.
The mass ratio of the oil tea fruit shell powder to the urea to the deionized water is 1 (1-10): 10-35.
Wherein the hydrothermal carbonization product, the KOH and the (NH) 4 ) 3 PO 4 The mass ratio of (2) is 1:2: (0.2-1).
Wherein the mass percentage concentration of the hydrochloric acid solution is 5-15%.
The temperature of the hydrothermal carbonization reaction is 160-200 ℃ and the time is 6-20 h.
Preferably, the method comprises the steps of,
the temperature of the hydrothermal carbonization reaction is 165 ℃,170 ℃,175 ℃,180 ℃,185 ℃,190 ℃ and 195 ℃;
the hydrothermal carbonization reaction time is 7h,8h,9h,10h,11h,12h,13h,14h,15h,16h,17h,18h,19h.
Wherein, the heating and activating process in the tube furnace comprises the following steps: at the heating rate of 3-5 ℃/min, firstly heating to 400-500 ℃ from room temperature, preserving heat for 20-40 min, further heating to 600-700 ℃ and preserving heat for 20-40 min, further heating to 750-850 ℃ and preserving heat for 40-80 min, and finally naturally cooling to room temperature.
The invention provides biomass graded porous carbon for a capacitor electrode material, wherein the pore structure of the graded porous carbon comprises micropores, mesopores and macropores, and the pore diameter range is 0.5 nm-1 um.
Wherein the graded porous carbon is applied to a supercapacitor as an electrode material.
The invention has the beneficial effects that:
according to the biomass porous carbon for the capacitor electrode material, the camellia oleifera shells are used as raw materials to prepare the biomass porous carbon for the capacitor electrode material, the raw materials are cheap and easy to obtain, the pore structure of the prepared biomass porous carbon is a hierarchical porous structure comprising micropores, mesopores and macropores, the porous structure can increase the specific surface area and the energy storage active point, and is beneficial to ion transmission and quickens electron transmission and ion diffusion, so that the specific capacitance and the energy density of the material are effectively improved, and the multiplying power performance of the material is improved; the biomass hierarchical porous carbon material is used as an electrode material of the supercapacitor, and has the advantages of high capacity, good cycle performance and the like.
Drawings
In order to more clearly illustrate the technical solutions of the present invention, the drawings that need to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort to those skilled in the art.
FIG. 1 is an SEM image of a hierarchical porous carbon material prepared by a method provided in example 1 of the present invention;
FIG. 2 is a CV graph of a hierarchical porous carbon prepared by the method provided in example 1 of the present invention as an electrode material for a supercapacitor;
fig. 3 is a charge-discharge graph of the hierarchical porous carbon prepared by the method provided in example 1 of the present invention as an electrode material of a supercapacitor.
Detailed Description
The following are preferred embodiments of the present invention, and it should be noted that modifications and variations can be made by those skilled in the art without departing from the principle of the present invention, and these modifications and variations are also considered as the protection scope of the present invention.
Example 1
The invention provides a preparation method of biomass graded porous carbon for a capacitor electrode material, which comprises the following steps:
s1, crushing dried camellia oleifera shells in a crusher, sieving by a 120-mesh sieve to obtain camellia oleifera shell powder, adding 1 part by weight of camellia oleifera shell powder, 8 parts by weight of urea and 25 parts by weight of deionized water into a reaction kettle, carrying out hydrothermal carbonization reaction for 12 hours at 180 ℃, taking out products after the reaction, and respectively washing and drying to obtain hydrothermal carbonized products;
s2, 1 part of the hydrothermal carbonized product prepared in the step S1, 2 parts of KOH and (NH) 4 ) 3 PO 4 Mixing and stirring 0.2 parts for 12 hours until the materials are uniformly mixed, placing the materials in a tube furnace, heating the materials from room temperature to 450 ℃ for 30 minutes at a heating rate of 5 ℃/min under the protection of nitrogen atmosphere, heating the materials to 650 ℃ for 30 minutes, heating the materials to 800 ℃ for 60 minutes, performing heating and activating reaction, and naturally cooling the materials to room temperature after the activation reaction is completed, so as to obtain an activated product;
s3, soaking the activated product prepared in the step S2 in hydrochloric acid solution with the concentration of 10% to remove impurities, and then washing with deionized water, filtering and drying to prepare the graded porous carbon.
The pore structure of the hierarchical porous carbon prepared in example 1 comprises micropores, mesopores and macropores, and the pore diameter range is 0.5 nm-1 um.
Fig. 1 is an SEM image of the graded porous carbon material prepared in example 1, and it can be seen from the image that the material obtained in this example has a porous structure, has a connected three-dimensional structure, and is beneficial for electrolyte ions to enter the porous material.
FIG. 2 is a CV plot in a 6M KOH electrode solution of a supercapacitor electrode material prepared by using the fractionated porous carbon obtained in example 1, as can be seen when the sweep rate is 10mV s -1 When the porous carbon-based electrode shows a nearly rectangular cyclic voltammetry curve, the porous carbon material has a special hierarchical porous structure and nitrogen and oxygen groups rich in the surface, so that the overall capacitance performance of the porous carbon material is improved. When the scanning speed is from 10mV s -1 Increase to 20mV s -1 、50mV s -1 、100mV s -1 To 200mV s -1 When the cyclic voltammogram still shows a rectangular shape, electricity is shownExcellent rate performance.
FIG. 3 is a graph showing charge and discharge of the hierarchical porous carbon prepared in example 1 as an electrode material for a supercapacitor in a 6M KOH electrode solution, as can be seen from the graph, when the current density is 1A g -1 Time specific capacitance of 253 Fg -1 When the current density is 10A g -1 The time specific capacitance was 230 Fg -1 Is of current density 1A g -1 90.9% of the time specific capacitance, and exhibits higher specific capacitance and excellent rate capability.
Example 2
The invention provides a preparation method of biomass graded porous carbon for a capacitor electrode material, which comprises the following steps:
s1, crushing dried camellia oleifera shells in a crusher, sieving by a 100-mesh sieve to obtain camellia oleifera shell powder, adding 1 part of camellia oleifera shell powder, 2 parts of urea and 12 parts of deionized water into a reaction kettle according to weight, performing hydrothermal carbonization reaction for 18 hours at 160 ℃, taking out products after the reaction, and respectively washing and drying to obtain hydrothermal carbonized products;
s2, 1 part of the hydrothermal carbonized product prepared in the step S1, 2 parts of KOH and (NH) 4 ) 3 PO 4 Mixing and stirring 0.2 parts for 10 hours until the materials are uniformly mixed, placing the materials in a tube furnace, heating the materials from room temperature to 420 ℃ for 40 minutes at a heating rate of 3 ℃/min under the protection of nitrogen atmosphere, heating the materials to 630 ℃ for 25 minutes, heating the materials to 780 ℃ for 50 minutes, performing heating and activating reaction, and naturally cooling the materials to room temperature after the activation reaction is completed, so as to obtain an activated product;
s3, soaking the activated product prepared in the step S2 in 8% hydrochloric acid solution to remove impurities, and then washing with deionized water, filtering and drying to obtain the graded porous carbon.
The pore structure of the hierarchical porous carbon prepared in example 2 comprises micropores, mesopores and macropores, and the pore diameter range is 0.5 nm-1 um. The hierarchical porous carbon prepared in example 1 was used as an electrode material for a supercapacitor when the current density was 1A g -1 The time specific capacitance was 240 Fg -1 When the current density is10A g -1 Time specific capacitance of 222 Fg -1 Is of current density 1A g -1 91.6% of the time specific capacitance, and exhibits higher specific capacitance and excellent rate capability.
Example 3
The invention provides a preparation method of biomass graded porous carbon for a capacitor electrode material, which comprises the following steps:
s1, crushing dried camellia oleifera shells in a crusher, sieving with a 150-mesh sieve to obtain camellia oleifera shell powder, adding 1 part of camellia oleifera shell powder, 4 parts of urea and 15 parts of deionized water into a reaction kettle according to weight, carrying out hydrothermal carbonization reaction for 10 hours at the temperature of 200 ℃, taking out products after the reaction, and respectively washing and drying to obtain hydrothermal carbonized products;
s2, 1 part of the hydrothermal carbonized product prepared in the step S1, 2 parts of KOH and (NH) 4 ) 3 PO 4 1 part of the mixture is mixed and stirred for 15 hours until the mixture is uniformly mixed, then the mixture is placed in a tube furnace, the temperature is firstly increased to 480 ℃ from room temperature for 20 minutes at a heating rate of 4 ℃/min under the protection of nitrogen atmosphere, the temperature is further increased to 700 ℃ for 40 minutes, the temperature is further increased to 850 ℃ for 70 minutes, the heating and activating reaction is carried out, and the mixture is naturally cooled to room temperature after the activation is completed, so that an activated product is prepared;
s3, soaking the activated product prepared in the step S2 in hydrochloric acid solution with the concentration of 15% to remove impurities, and then washing with deionized water, filtering and drying to prepare the graded porous carbon.
The pore structure of the hierarchical porous carbon prepared in example 3 comprises micropores, mesopores and macropores, and the pore diameter range is 0.5 nm-1 um. The hierarchical porous carbon prepared in example 1 was used as an electrode material for super capacitor when the current density was 1A g -1 The time specific capacitance is 180 Fg -1 When the current density is 10A g -1 The time specific capacitance is 125 Fg -1 Is of current density 1A g -1 69.4% of the time specific capacitance, and exhibits higher specific capacitance and excellent rate capability.
Example 4
The invention provides a preparation method of biomass graded porous carbon for a capacitor electrode material, which comprises the following steps:
s1, crushing dried camellia oleifera shells in a crusher, sieving with a 150-mesh sieve to obtain camellia oleifera shell powder, adding 1 part of camellia oleifera shell powder, 5 parts of urea and 20 parts of deionized water into a reaction kettle according to weight, carrying out hydrothermal carbonization reaction for 8 hours at the temperature of 200 ℃, taking out products after the reaction, and respectively washing and drying to obtain hydrothermal carbonized products;
s2, 1 part of the hydrothermal carbonized product prepared in the step S1, 2 parts of KOH and (NH) 4 ) 3 PO 4 Mixing and stirring 0.8 part for 10 hours until the materials are uniformly mixed, placing the materials in a tube furnace, heating the materials from room temperature to 460 ℃ for 40 minutes at a heating rate of 5 ℃/min under the protection of nitrogen atmosphere, heating the materials to 640 ℃ for 35 minutes, heating the materials to 780 ℃ for 50 minutes, performing heating and activating reaction, and naturally cooling the materials to room temperature after the activation reaction is completed, so as to obtain an activated product;
s3, soaking the activated product prepared in the step S2 in hydrochloric acid solution with the concentration of 10% to remove impurities, and then washing with deionized water, filtering and drying to prepare the graded porous carbon.
The pore structure of the hierarchical porous carbon prepared in example 4 comprises micropores, mesopores and macropores, and the pore diameter range is 0.5 nm-1 um. The hierarchical porous carbon prepared in example 1 was used as an electrode material for super capacitor when the current density was 1A g -1 The time specific capacitance is 238 Fg -1 When the current density is 10A g -1 The time specific capacitance is 215 Fg -1 At a current density of 0.5. 0.5A g -1 90.3% of the time specific capacitance, and exhibits higher specific capacitance and excellent rate capability.
Example 5
The invention provides a preparation method of biomass graded porous carbon for a capacitor electrode material, which comprises the following steps:
s1, crushing dried camellia oleifera shells in a crusher, sieving by a 200-mesh sieve to obtain camellia oleifera shell powder, adding 1 part by weight of camellia oleifera shell powder, 10 parts by weight of urea and 35 parts by weight of deionized water into a reaction kettle, carrying out hydrothermal carbonization reaction for 15 hours at the temperature of 190 ℃, taking out products after the reaction, washing with water, and drying to obtain hydrothermal carbonized products;
s2, 1 part of the hydrothermal carbonized product prepared in the step S1, 2 parts of KOH and (NH) 4 ) 3 PO 4 Mixing and stirring 0.8 part for 12 hours until the materials are uniformly mixed, placing the materials in a tube furnace, heating the materials from room temperature to 480 ℃ for 40 minutes at a heating rate of 4 ℃/min under the protection of nitrogen atmosphere, heating the materials to 700 ℃ for 30 minutes, heating the materials to 800 ℃ for 55 minutes, performing heating and activating reaction, and naturally cooling the materials to room temperature after the activation reaction is completed, so as to obtain an activated product;
s3, soaking the activated product prepared in the step S2 in hydrochloric acid solution with the concentration of 15% to remove impurities, and then washing with deionized water, filtering and drying to prepare the graded porous carbon.
The pore structure of the hierarchical porous carbon prepared in example 5 comprises micropores, mesopores and macropores, and the pore diameter range is 0.5 nm-1 um. The hierarchical porous carbon prepared in example 1 was used as an electrode material for super capacitor when the current density was 1A g -1 The time specific capacitance was 275 Fg -1 When the current density is 10A g -1 Time specific capacitance of 251 Fg -1 At a current density of 0.5. 0.5A g -1 91.3% of the time specific capacitance, and exhibits higher specific capacitance and excellent rate capability.
The foregoing examples merely illustrate specific embodiments of the invention, which are described in greater detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (7)
1. The preparation method of the biomass graded porous carbon for the capacitor electrode material is characterized by comprising the following steps of:
s1, adding camellia oleifera shell powder, urea and deionized water into a reaction kettle, heating to perform hydrothermal carbonization reaction, taking out products after the reaction, and respectively washing and drying to obtain hydrothermal carbonized products;
s2, mixing the hydrothermal carbonized product prepared in the step S1 with KOH, (NH) 4 ) 3 PO 4 Uniformly mixing, placing in a tube furnace, heating and activating under the protection of nitrogen atmosphere, and cooling to room temperature after activating to obtain an activated product; the hydrothermal carbonization product, the KOH and the (NH) 4 ) 3 PO 4 The mass ratio of (2) is 1:2 (0.2-1);
s3, soaking the activated product prepared in the step S2 in hydrochloric acid solution to remove impurities, and then washing with deionized water, filtering and drying to obtain the graded porous carbon.
2. The method for preparing biomass-based hierarchical porous carbon for capacitor electrode materials according to claim 1, wherein the method comprises the steps of: the mesh number of the oil tea fruit shell powder is 100-200 meshes.
3. The method for preparing biomass-based hierarchical porous carbon for capacitor electrode materials according to claim 1, wherein the method comprises the steps of: the mass ratio of the oil tea fruit shell powder to the urea to the deionized water is 1 (1-10): 10-35.
4. The method for preparing biomass-based hierarchical porous carbon for capacitor electrode materials according to claim 1, wherein the method comprises the steps of: the mass percentage concentration of the hydrochloric acid solution is 5-15%.
5. The method for preparing biomass-based hierarchical porous carbon for capacitor electrode materials according to any one of claims 1 to 4, characterized by comprising the steps of: the temperature of the hydrothermal carbonization reaction is 160-200 ℃ and the time is 6-20 h.
6. The method for preparing biomass-classified porous carbon for capacitor electrode material according to any one of claims 1 to 4, wherein the process of heating and activating in the tube furnace is: at the heating rate of 3-5 ℃/min, firstly heating to 400-500 ℃ from room temperature, preserving heat for 20-40 min, further heating to 600-700 ℃ and preserving heat for 20-40 min, further heating to 750-850 ℃ and preserving heat for 40-80 min, and finally naturally cooling to room temperature.
7. A biomass-fractionated porous carbon for capacitor electrode materials prepared by the method of any one of claims 1 to 6, characterized in that: the pore structure of the graded porous carbon comprises micropores, mesopores and macropores, and the pore diameter range is 0.5 nm-1 um.
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| JP2017052706A (en) * | 2015-09-07 | 2017-03-16 | 一丸ファルコス株式会社 | Cosmetic composition containing granules |
| CN106587047A (en) * | 2016-12-12 | 2017-04-26 | 张家港智电芳华蓄电研究所有限公司 | Preparation method for nanoporous carbon |
| CN109987604A (en) * | 2019-04-26 | 2019-07-09 | 江苏大学 | A kind of porous carbon materials and preparation method thereof |
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