CN109110756B - Homogeneous corncob derived carbon electrode material and preparation method thereof - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000007772 electrode material Substances 0.000 title claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 37
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 20
- 239000005539 carbonized material Substances 0.000 claims abstract description 14
- 238000009826 distribution Methods 0.000 claims abstract description 14
- 239000002028 Biomass Substances 0.000 claims abstract description 12
- 238000012216 screening Methods 0.000 claims abstract description 12
- 230000003213 activating effect Effects 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000010000 carbonizing Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 30
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 238000003763 carbonization Methods 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001994 activation Methods 0.000 claims description 7
- 239000011148 porous material Substances 0.000 claims description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 9
- 239000002243 precursor Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 240000008042 Zea mays Species 0.000 description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 3
- 235000005822 corn Nutrition 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 229920002488 Hemicellulose Polymers 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000011883 electrode binding agent Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
-
- 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
-
- 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
-
- 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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- 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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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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
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Abstract
The invention discloses a homogeneous corncob derived carbon electrode material for a super capacitor and a preparation method thereof. The preparation process comprises the following steps: firstly, crushing biomass corncobs, screening to obtain corncob powder particles with different particle size distribution ranges, and carbonizing at high temperature; then activating the obtained carbonized material powder particles by an activating agent at high temperature; and finally, acid washing and drying the activated product to obtain the homogeneous corncob derived carbon electrode material. When the homogeneous corncob-derived carbon electrode material is used as a supercapacitor electrode material, high specific capacitance and rate performance are shown. The method has the characteristics of simple process, rich raw materials, environmental friendliness, high additional value and the like.
Description
Technical Field
The invention relates to a biomass derived carbon electrode material and a preparation method thereof, in particular to a homogeneous corncob derived carbon electrode material and a preparation method thereof; belongs to the field of new energy materials.
Background
With the increasingly exhaustion of fossil energy and the increasing severity of environmental pollution, biomass-derived carbon supercapacitor electrode materials are favored by researchers due to the characteristics of wide raw material sources, low cost, renewability, no pollution and the like.
The biomass corncob is rich in source and developed in pores, the prepared active carbon not only reduces the environmental pollution caused by discarding or directly burning the biomass corncob, but also converts the biomass corncob into a high-performance supercapacitor electrode material, changes the corncob into valuable, improves the added value of the corncob, and realizes effective utilization of resources. Qu et al (Bioresource Technology, 2015, 189: 285-. The specific capacitance retention rate is up to 82%, and the rate performance is excellent. Li et al (Journal of Materials Chemistry A, 2017, 5: 3875-3887) first treated corncobs with concentrated sulfuric acid, then mixed with melamine and carbonized at high temperature to obtain mesoporous carbon with specific capacity up to 538F/g at a current density of 1A/g. Also, the corncob-derived charcoal exhibits excellent electrochemical properties.
Although the corncob-derived carbon shows good electrochemical performance of a supercapacitor, when high-performance corncob-derived porous activated carbon is obtained, the corncob is subjected to complicated pretreatment (such as corncob residue obtaining or acid treatment) or modification (such as melamine addition), so that a simple efficient preparation method of the biomass corncob electrode material is found, and the method has important scientific and social values for the development of the biomass corncob electrode material.
Disclosure of Invention
The invention aims to overcome the defects of the existing preparation technology and provides a simple and safe preparation method of homogeneous corncob-derived carbon electrode material. As is known to all, corncobs mainly comprise three components, namely cellulose, hemicellulose and lignin, and the microstructures of the three components are completely different, so that the corncobs with more uniform components are adopted as precursors in order to obtain homogeneous activated carbon. Usually, a chemical pretreatment method is adopted to obtain a corncob precursor with more uniform components, and then carbonization and activation are carried out to obtain an activated carbon material with better performance, and the activated carbon material has good consistency, but the waste liquid generated by the method can cause environmental pollution. In addition, since the corn cob has different microstructures such as cellulose, hemicellulose and lignin, and thus has different mechanical strengths, different components are partially formed into particles of different sizes during crushing. Therefore, the invention develops a simple physical screening method to easily obtain the homogeneous corncob precursor, thereby overcoming the defect that the homogeneous corncob precursor is difficult to obtain.
When the corncob-derived carbon electrode material prepared by the method is used as a supercapacitor electrode material, the electrochemical performance is excellent due to the uniform and consistent microstructure. The method has the characteristics of simple equipment and process, low production cost, environmental friendliness, large-scale production and the like. The preparation method comprises the following steps:
cleaning, drying and crushing the collected biomass corncobs, and screening by adopting sieves with different meshes to obtain corncob powder particles with different particle size distribution ranges;
secondly, placing the screened biomass corncob particles into a tubular furnace, and carbonizing at high temperature in a nitrogen atmosphere to obtain a carbonized material;
mixing the carbonized material and the activating agent according to different mass ratios, fully grinding, and activating at high temperature in a nitrogen atmosphere to obtain an activated product;
and step four, soaking the obtained activated product in different acid solutions, then alternately cleaning the activated product by using deionized water and alcohol, and finally drying the activated product in a drying oven at the temperature of 50-150 ℃ to obtain the homogeneous corncob derived carbon electrode material.
The obtained homogeneous corncob derived carbon electrode material has uniform microstructure, especially pore distribution state, and uniform particle size distribution of activated carbon particles.
In the first step, the mesh number of the sieve is 10-400 meshes, and the particle size distribution range of the corncob powder particles is 0.03-2 mm.
In the second step, the temperature rise rate of the high-temperature carbonization is 3-20 ℃/min, the carbonization temperature is 600-1000 ℃, and the heat preservation time is 1-24 h.
In the third step, the mass ratio of the carbonized material to the activating agent is 1: 1-1: 6, the heating rate of high-temperature activation is 3-20 ℃/min, the activation temperature is 600-1000 ℃, and the heat preservation time is 1-24 h.
In the third step, the activating agent is one or more of potassium hydroxide, sodium hydroxide, zinc chloride and magnesium chloride. The selected active agent can be selected according to the particle size distribution range, and the corncob-derived carbon supercapacitor electrode material with better performance can be obtained.
In the fourth step, the acid solution is hydrochloric acid or sulfuric acid, the concentration is 1M-6M, and the soaking time is 1-24 h. According to different selected activating agents, different acids are selected, and the corncob-derived carbon supercapacitor electrode material with better performance can be obtained.
The invention has the beneficial effects that:
1. the invention obtains the homogeneous corncob precursor by a simple physical screening method, further realizes the preparation of the homogeneous corncob derived carbon electrode material, and overcomes the defect that the environment is polluted by the homogeneous corncob precursor obtained by the conventional chemical method.
2. The homogeneous corncob-derived carbon electrode material prepared by the invention has uniform and consistent components of the used precursor, so that activated carbon particles with uniform carbonization degree and activation degree can be obtained in the subsequent carbonization and activation processes.
3. The homogeneous corncob-derived carbon electrode material prepared by the invention has a uniform microstructure, so that when the homogeneous corncob-derived carbon electrode material is used as a supercapacitor electrode material, each carbon particle can be fully utilized to store energy in an electrochemical reaction process.
4. The invention has the advantages of rich raw materials, simple preparation process, lower cost, cleanness, environmental protection and easy realization of industrialization.
The conception, specific material structure and technical effects of the present invention will be further described in conjunction with the accompanying drawings to fully understand the objects, features and effects of the present invention.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a homogeneous corncob-derived carbon electrode material prepared in example 1 of the present invention.
FIG. 2 is a graph showing the pore size distribution of the homogeneous corncob-derived carbon electrode material prepared in example 1 of the present invention.
FIG. 3 is a constant current charge/discharge curve of the homogeneous corncob-derived carbon electrode material prepared in example 1 of the present invention at a current density of 0.5-5A/g.
FIG. 4 is a graph of rate capability of homogeneous corncob-derived carbon electrode material prepared in example 1 of the present invention.
FIG. 5 is a Scanning Electron Microscope (SEM) image of a homogeneous corncob-derived carbon electrode material prepared in example 2 of the present invention.
Detailed Description
The present invention is further described in detail by the embodiments, with reference to the drawings in the specification, but the present application is not limited to these embodiments.
Example 1
Cleaning, drying and crushing the collected corncobs, and screening to obtain corncob powder particles of 10-18 meshes; transferring the obtained corncob powder particles into a tubular furnace, heating to 800 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, preserving heat for 2 h, and carrying out carbonization treatment; mixing the obtained carbonized material with KOH according to the mass ratio of 1: 3, mixing, fully grinding, heating to 800 ℃ at the heating rate of 5 ℃/min in the nitrogen atmosphere, and keeping the temperature for 2 hours to obtain an activated product; soaking the obtained activated product in 1 mol/L HCl solution, then alternately cleaning with deionized water and alcohol, and finally drying in a drying oven at 60 ℃ to obtain the homogeneous corncob-derived carbon electrode material.
The Scanning Electron Microscope (SEM) image of the homogeneous corncob-derived carbon electrode material is shown in fig. 1, and it can be seen from fig. 1 that the microstructure and the particle size of the prepared activated carbon electrode material are relatively uniform. Fig. 2 is a pore size distribution curve diagram of the prepared homogeneous corncob-derived carbon electrode material, and it can be seen that the prepared activated carbon has a narrow pore size distribution range, indicating that the activated carbon has a relatively uniform and consistent pore size distribution. The electrode material, binder and conductive carbon were uniformly ground in a ratio of 80:10:10, coated on foamed nickel (1 × 1 cm) and dried (70 ℃) to prepare a working electrode, and the electrochemical performance was tested in a three-electrode system (platinum sheet as counter electrode, Ag/AgCl electrode as reference electrode, 1M sodium sulfate aqueous solution as electrolyte). When the current density of the electrode is 0.5A/g, the specific capacitance value of the electrode is 108F/g; when the current density is 5A/g, the specific capacitance value is 99F/g, the specific capacity retention rate is up to 91.7 percent, and the excellent rate capability is shown.
Example 2
Cleaning, drying and crushing the collected corncobs, and screening to obtain corncob powder particles of 170-200 meshes; transferring the obtained corncob powder particles into a tubular furnace, heating to 600 ℃ at a heating rate of 20 ℃/min in a nitrogen atmosphere, preserving heat for 24 hours, and carrying out carbonization treatment; mixing the obtained carbonized material with KOH according to the mass ratio of 1: 1, mixing, fully grinding, heating to 1000 ℃ at a heating rate of 10 ℃/min in a nitrogen atmosphere, and keeping the temperature for 12 hours to obtain an activated product; soaking the obtained activated product in 6 mol/L HCl solution, then alternately cleaning with deionized water and alcohol, and finally drying in a drying oven at 150 ℃ to obtain the homogeneous corncob-derived carbon electrode material.
The Scanning Electron Microscope (SEM) image of the homogeneous corncob-derived carbon electrode material is shown in fig. 5, and it can be seen from fig. 5 that the microstructure and the particle size of the prepared activated carbon electrode material are relatively uniform.
Example 3
Cleaning, drying and crushing the collected corncobs, and screening to obtain 325-400-mesh corncob powder particles; transferring the obtained corncob powder particles into a tubular furnace, heating to 1000 ℃ at a heating rate of 3 ℃/min in a nitrogen atmosphere, preserving heat for 1 h, and carrying out carbonization treatment; mixing the obtained carbonized material with KOH according to the mass ratio of 1: 6, mixing, fully grinding, heating to 600 ℃ at a heating rate of 20 ℃/min in a nitrogen atmosphere, and keeping the temperature for 24 hours to obtain an activated product; soaking the obtained activated product in 3 mol/L HCl solution, then alternately cleaning with deionized water and alcohol, and finally drying in a drying oven at 50 ℃ to obtain the homogeneous corncob-derived carbon electrode material.
Example 4
Collecting corn cobCleaning, drying, crushing and screening to obtain 10-18-mesh corncob powder particles; transferring the obtained corncob powder particles into a tubular furnace, heating to 800 ℃ at a heating rate of 10 ℃/min in a nitrogen atmosphere, preserving heat for 2 h, and carrying out carbonization treatment; mixing the obtained carbonized material with NaOH according to the mass ratio of 1: 3, mixing, fully grinding, heating to 800 ℃ at the heating rate of 5 ℃/min in the nitrogen atmosphere, and keeping the temperature for 2 hours to obtain an activated product; the obtained activated product is taken as 1 mol/L H2SO4Soaking in the solution, washing with deionized water and alcohol alternately, and drying in a drying oven at 60 deg.C to obtain homogeneous corn cob derived carbon electrode material.
Example 5
Cleaning, drying and crushing the collected corncobs, and screening to obtain corncob powder particles of 10-18 meshes; transferring the obtained corncob powder particles into a tubular furnace, heating to 800 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, preserving heat for 2 h, and carrying out carbonization treatment; mixing the obtained carbonized material with ZnCl2According to the mass ratio of 1: 3, mixing, fully grinding, heating to 800 ℃ at a heating rate of 10 ℃/min in a nitrogen atmosphere, and keeping the temperature for 2 hours to obtain an activated product; soaking the obtained activated product in 1 mol/L HCl solution, then alternately cleaning with deionized water and alcohol, and finally drying in a drying oven at 60 ℃ to obtain the homogeneous corncob-derived carbon electrode material.
Example 6
Cleaning, drying and crushing the collected corncobs, and screening to obtain corncob powder particles of 10-18 meshes; transferring the obtained corncob powder particles into a tubular furnace, heating to 800 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, preserving heat for 2 h, and carrying out carbonization treatment; mixing the obtained carbonized material with MgCl2According to the mass ratio of 1: 3, mixing, fully grinding, heating to 800 ℃ at the heating rate of 5 ℃/min in the nitrogen atmosphere, and keeping the temperature for 2 hours to obtain an activated product; soaking the obtained activated product in 1 mol/L HCl solution, then alternately cleaning with deionized water and alcohol, and finally drying in a drying oven at 60 ℃ to obtain the homogeneous corncob-derived carbon electrode material.
Example 7
Cleaning the collected corncobWashing, drying, crushing and screening to obtain 10-18 mesh corncob powder particles; transferring the obtained corncob powder particles into a tubular furnace, heating to 800 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, preserving heat for 2 h, and carrying out carbonization treatment; mixing the obtained carbonized material with KOH and MgCl2According to the mass ratio of 1: 3, mixing, fully grinding, heating to 800 ℃ at the heating rate of 5 ℃/min in the nitrogen atmosphere, and keeping the temperature for 2 hours to obtain an activated product; soaking the obtained activated product in 1 mol/L HCl solution, then alternately cleaning with deionized water and alcohol, and finally drying in a drying oven at 60 ℃ to obtain the homogeneous corncob-derived carbon electrode material.
Claims (1)
1. A preparation method of homogeneous corncob-derived carbon electrode material is characterized by comprising the following steps:
cleaning, drying and crushing the collected biomass corncobs, and screening by adopting sieves with different meshes to obtain corncob powder particles with different particle size distribution ranges;
secondly, placing the screened biomass corncob particles into a tubular furnace, and carbonizing at high temperature in a nitrogen atmosphere to obtain a carbonized material;
mixing the carbonized material and the activating agent according to different mass ratios, fully grinding, and activating at high temperature in a nitrogen atmosphere to obtain an activated product;
soaking the obtained activated product in different acid solutions, then alternately cleaning the activated product by using deionized water and alcohol, and finally drying the activated product in a drying oven at the temperature of 50-150 ℃ to obtain a homogeneous corncob derived carbon electrode material;
the obtained homogeneous corncob derived carbon electrode material has uniform pore distribution state and uniform particle size distribution of activated carbon particles; in the first step, the mesh number of the sieve is 10-400 meshes, and the particle size distribution range of the corncob powder particles is 0.03-2 mm;
in the second step, the temperature rise rate of the high-temperature carbonization is 3-20 ℃/min, the carbonization temperature is 600-1000 ℃, and the heat preservation time is 1-24 h;
in the third step, the mass ratio of the carbonized material to the activating agent is 1: 1-1: 6, the heating rate of high-temperature activation is 3-20 ℃/min, the activation temperature is 600-1000 ℃, and the heat preservation time is 1-24 h;
in the third step, the activating agent is one or more of potassium hydroxide, sodium hydroxide, zinc chloride and magnesium chloride;
in the fourth step, the acid solution is hydrochloric acid or sulfuric acid, the concentration is 1M-6M, and the soaking time is 1-24 h.
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| CN109809403B (en) * | 2019-03-18 | 2022-04-26 | 中国药科大学 | Preparation method and application of biogas residue-based activated carbon with high adsorption performance |
| CN110165234A (en) * | 2019-05-22 | 2019-08-23 | 广州大学 | A kind of corncob electrode material and its preparation method and application |
| CN111924842A (en) * | 2020-08-17 | 2020-11-13 | 四川轻化工大学 | Lotus stalk-based electrode material and preparation method thereof |
| CN113845116A (en) * | 2021-09-16 | 2021-12-28 | 安徽理工大学 | Method for preparing electromagnetic wave absorbing material based on corncobs |
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