CN112919466A - Active carbon graphene modification method for preparing super capacitor - Google Patents
Active carbon graphene modification method for preparing super capacitor Download PDFInfo
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- CN112919466A CN112919466A CN202110229692.7A CN202110229692A CN112919466A CN 112919466 A CN112919466 A CN 112919466A CN 202110229692 A CN202110229692 A CN 202110229692A CN 112919466 A CN112919466 A CN 112919466A
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- activated carbon
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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
- C01B32/354—After-treatment
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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
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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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 an active carbon graphene modification method for preparing a super capacitor, which comprises the following steps: the method comprises the following steps of firstly, placing the activated carbon under the protection of nitrogen or argon at the temperature of 750-800 ℃ for deoxidation to obtain an activated carbon deoxidation material; secondly, cooling the activated carbon deoxidizing material, then soaking the activated carbon deoxidizing material in a nickel nitrate or iron nitrate or cobalt nitrate solution with the mass concentration of 0.5-5% for 1-3 hours, and drying the activated carbon deoxidizing material at the temperature of 100-120 ℃ until the water content is below 1% to obtain an activated carbon soaking material; and step three, placing the activated carbon impregnation material under the protection of argon at 800-1000 ℃, preserving the heat for 30-180 min, and then naturally cooling. The activated carbon generated by the method has low ash content, developed micropores and high iodine adsorption value, the adsorption capacity of the activated carbon is improved, the generated graphene can be well combined with the activated carbon, and the conductivity of the activated carbon is improved.
Description
Technical Field
The invention relates to the technical field of activated carbon modification, in particular to an activated carbon graphene modification method for preparing a super capacitor.
Background
The super capacitor is a novel energy storage device between a traditional capacitor and a rechargeable battery, and has the characteristics of quick charge and discharge of the capacitor and the energy storage characteristic of the battery. A supercapacitor is a novel component that stores energy through an interfacial double layer formed between electrodes and an electrolyte. When the electrode contacts with the electrolyte, the solid-liquid interface generates stable double-layer charges with opposite signs under the action of coulomb force, intermolecular force and atomic force, and the double-layer charges are called as an interface double electric layer. The electric double layer supercapacitor is considered to be 2 inactive porous plates suspended in an electrolyte, and a voltage is applied to the 2 plates. The potential applied to the positive plate attracts negative ions in the electrolyte and the negative plate attracts positive ions, thereby forming an electric double layer capacitor on the surfaces of the two electrodes. The electric double layer capacitor may be classified into a carbon electrode double layer supercapacitor, a metal oxide electrode supercapacitor, and an organic polymer electrode supercapacitor according to the difference in electrode materials.
Activated carbon is widely used as the most economical material in supercapacitor carbon electrodes. Various properties of the cheap electrode material active carbon directly influence the rapid popularization of the super capacitor in the civil energy storage field. At present, the defect of poor conductivity exists when the activated carbon is used as a super capacitor electrode compared with other carbon materials, and how to improve the conductivity of the activated carbon becomes one of hot spots of activated carbon research. The high conductivity of graphene has been paid attention to in the field of activated carbon, and people have mixed graphene oxide powder with activated carbon to improve the conductivity of activated carbon and obtained related patents, but because graphene oxide contains oxygen, the conductivity of graphene is greatly reduced, and graphene oxide and activated carbon are independent particles, so that a conductive bridge is difficult to generate, the resistivity is very high, and ideal conductivity is difficult to obtain.
Disclosure of Invention
It is an object of the present invention to address at least the above-mentioned deficiencies and to provide at least the advantages which will be described hereinafter.
The invention also aims to provide an activated carbon graphene modification method for preparing a super capacitor, which overcomes the defects that conductive bridges are difficult to generate and the activated carbon itself has poor conductivity as a super capacitor raw material due to the fact that activated carbon is difficult to be combined with graphene and mutually independent particles after being used as the super capacitor raw material for graphene modification.
In order to solve the technical problem, the invention provides a method for modifying activated carbon graphene for preparing a super capacitor, which comprises the following steps:
the method comprises the following steps of firstly, placing the activated carbon under the protection of nitrogen or argon at the temperature of 750-800 ℃ for deoxidation to obtain an activated carbon deoxidation material;
secondly, cooling the activated carbon deoxidizing material, then soaking the activated carbon deoxidizing material in a nickel nitrate or iron nitrate or cobalt nitrate solution with the mass concentration of 0.5-5% for 1-3 hours, and drying the activated carbon deoxidizing material at the temperature of 100-120 ℃ until the water content is below 1% to obtain an activated carbon soaking material;
and step three, placing the activated carbon impregnation material under the protection of argon at 800-1000 ℃, preserving the heat for 30-180 min, and then naturally cooling.
In the technical scheme, the deoxidized activated carbon is impregnated by ferric nitrate or nickel nitrate or cobalt nitrate, the impregnated activated carbon is graphitized at high temperature in an argon-filled environment, and graphene is generated along the impregnated surface. The activated carbon generated by the method has low ash content, developed micropores and high iodine adsorption value, the adsorption capacity of the activated carbon is improved, the generated graphene can be well combined with the activated carbon, and the conductivity of the activated carbon is improved. Under high temperature, NO-and carbon graphite generate pyridine-like groups and pyrrole-like groups, so that the capacitive performance of the electrode is improved. Due to the existence of metal ions on the surface of the activated carbon, the pseudo capacitance of the super capacitor is increased, and the specific capacity of the activated carbon electrode of the super capacitor is improved. Under the catalysis of metal ions, the temperature for graphitizing the surface of the activated carbon is reduced from 3000 ℃ of 2500 ℃ to 1000 ℃ of 800 ℃, and the energy consumption is saved.
Preferably, in the method for modifying graphene with activated carbon for preparing a supercapacitor, in the first step, the concentration of nitrogen or argon is 99.5%.
Preferably, in the method for modifying graphene as active carbon for preparing a super capacitor, coconut shells are used as a carbonized material, and the carbonized material is physically activated by a physical activation process using water vapor as a main activating agent to obtain the active carbon.
Preferably, in the method for modifying the graphene with the activated carbon for preparing the super capacitor, the cooling temperature of the deoxidized activated carbon material in the second step is 20-25 ℃ and normal temperature; and the natural cooling temperature in the third step is 20-25 ℃ normal temperature.
Preferably, in the method for modifying activated carbon graphene for preparing a supercapacitor, in the second step, the mass concentration of the nickel nitrate or ferric nitrate or cobalt nitrate solution is 3%.
Preferably, in the active carbon graphene modification method for preparing the super capacitor, in the third step, the active carbon impregnation material is placed under the protection of argon at 950 ℃, is subjected to heat preservation for 30-180 min, and is then naturally cooled.
The invention at least comprises the following beneficial effects:
the method comprises the steps of impregnating deoxidized activated carbon with ferric nitrate or nickel nitrate or cobalt nitrate, graphitizing the impregnated activated carbon at high temperature in an argon-filled environment, and generating graphene along an impregnated surface. The ash content of the activated carbon generated by the method is less than or equal to 0.2 percent, micropores are developed, the iodine adsorption value is more than or equal to 1800mg/g, the adsorption capacity of the activated carbon is improved, the generated graphene can be well combined with the activated carbon, the conductivity of the activated carbon is improved, and the conductivity is more than or equal to 450S/m. Under high temperature, NO-and carbon graphite generate pyridine-like groups and pyrrole-like groups, so that the capacitive performance of the electrode is improved. Due to the existence of metal ions on the surface of the activated carbon, the pseudo capacitance of the super capacitor is increased, and the specific capacity of the activated carbon electrode of the super capacitor is improved. Under the catalysis of metal ions, the temperature for graphitizing the surface of the activated carbon is reduced from 3000 ℃ of 2500 ℃ to 1000 ℃ of 800 ℃, and the energy consumption is saved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
Example 1
A graphene modification method of activated carbon for preparing a super capacitor comprises the following steps:
firstly, stirring and removing impurities from a carbonized coconut shell material, crushing, putting into an activation furnace, introducing high-temperature steam, and activating to obtain the activated carbon.
And secondly, introducing 99.5% of nitrogen into the totally closed pushed slab kiln, setting the temperature in the kiln to be 750 ℃, sequentially pushing the pushed slab material box filled with the activated material into and out of the pushed slab kiln, and treating for 20 minutes to complete the deoxidation of the activated material (20-60min) to obtain the activated carbon deoxidized material.
And thirdly, cooling the activated carbon deoxidizing material to the normal temperature of 20-25 ℃, soaking in a 3% nickel nitrate solution for 1h, and drying at the temperature of 100 ℃ until the water content is 1% to obtain the activated carbon soaking material.
And fourthly, placing the activated carbon impregnation material under the protection of argon at 800 ℃, preserving the heat for 30min, and then naturally cooling to normal temperature to obtain the activated carbon impregnation material.
And fifthly, grinding the graphene modified activated carbon to the fineness required by the super-capacitor activated carbon by using a superfine grinding machine, such as an impact mill and an air flow mill.
Example 2
A graphene modification method of activated carbon for preparing a super capacitor comprises the following steps:
firstly, stirring and removing impurities from a carbonized coconut shell material, crushing, putting into an activation furnace, introducing high-temperature steam, and activating to obtain the activated carbon.
And secondly, introducing 99.5% argon into the totally closed pushed slab kiln, setting the temperature in the kiln to be 800 ℃, sequentially pushing the pushed slab material box filled with the activated material into and out of the pushed slab kiln, and treating for 40 minutes to complete the deoxidation of the activated material to obtain the activated carbon deoxidized material.
And thirdly, cooling the activated carbon deoxidizing material to the normal temperature of 20-25 ℃, soaking in 0.5% ferric nitrate solution for 3 hours, and drying at the temperature of 120 ℃ until the water content is 0.5% to obtain the activated carbon impregnating material.
And fourthly, placing the activated carbon impregnation material under the protection of argon at the temperature of 1000 ℃, preserving the heat for 180min, and naturally cooling to the normal temperature to obtain the activated carbon impregnation material.
And fifthly, grinding the graphene modified activated carbon to the fineness required by the super-capacitor activated carbon by using a superfine grinding machine, such as an impact mill and an air flow mill.
Example 3
A graphene modification method of activated carbon for preparing a super capacitor comprises the following steps:
firstly, stirring and removing impurities from a carbonized coconut shell material, crushing, putting into an activation furnace, introducing high-temperature steam, and activating to obtain the activated carbon.
And secondly, introducing 99.5% argon into the totally closed pushed slab kiln, setting the temperature in the kiln to be 760 ℃, sequentially pushing the pushed slab material box filled with the activated material into and out of the pushed slab kiln, and treating for 60 minutes to complete the deoxidation of the activated material to obtain the activated carbon deoxidized material.
And thirdly, cooling the activated carbon deoxidizing material to the normal temperature, soaking the activated carbon deoxidizing material in a 5% cobalt nitrate solution for 2 hours, and drying the activated carbon deoxidizing material at the temperature of 110 ℃ until the water content is 0.3% to obtain the activated carbon soaking material.
And fourthly, placing the activated carbon impregnation material under the protection of argon at 950 ℃, preserving the heat for 100min, and naturally cooling to normal temperature to obtain the activated carbon impregnation material.
And fifthly, grinding the graphene modified activated carbon to the fineness required by the super-capacitor activated carbon by using a superfine grinding machine, such as an impact mill and an air flow mill.
Example 4
A graphene modification method of activated carbon for preparing a super capacitor comprises the following steps:
firstly, stirring and removing impurities from a carbonized coconut shell material, crushing, putting into an activation furnace, introducing high-temperature steam, and activating to obtain the activated carbon.
And secondly, introducing 99.5% argon into the totally closed pushed slab kiln, setting the temperature in the kiln to 770 ℃, sequentially pushing the pushed slab material box filled with the activated material into and out of the pushed slab kiln, and treating for 40 minutes to complete the deoxidation of the activated material to obtain the activated carbon deoxidized material.
And thirdly, cooling the activated carbon deoxidizing material to the normal temperature, soaking in 5% nickel nitrate solution for 1.5h, and drying at the temperature of 115 ℃ until the moisture content is 0.7% to obtain the activated carbon soaking material.
And fourthly, placing the activated carbon impregnation material under the protection of argon at 900 ℃, preserving the heat for 50min, and naturally cooling to the normal temperature to obtain the activated carbon impregnation material.
And fifthly, grinding the graphene modified activated carbon to the fineness required by the super-capacitor activated carbon by using a superfine grinding machine, such as an impact mill and an air flow mill.
While embodiments of the invention have been disclosed above, it is not intended to be limited to the uses set forth in the specification and examples. It can be applied to all kinds of fields suitable for the present invention. Additional modifications will readily occur to those skilled in the art.
Claims (6)
1. A method for modifying activated carbon graphene for preparing a super capacitor is characterized by comprising the following steps:
the method comprises the following steps that firstly, the activated carbon is deoxidized under the protection condition of nitrogen or argon at the temperature of 750-800 ℃ to obtain an activated carbon deoxidized material;
secondly, cooling the activated carbon deoxidizing material, then soaking the activated carbon deoxidizing material in a nickel nitrate or iron nitrate or cobalt nitrate solution with the mass concentration of 0.5-5% for 1-3 hours, and drying the activated carbon deoxidizing material at the temperature of 100-120 ℃ until the water content is below 1% to obtain an activated carbon soaking material;
and step three, placing the activated carbon impregnation material under the protection of argon at 800-1000 ℃, preserving the heat for 30-180 min, and then naturally cooling.
2. The method for modifying graphene as active carbon for preparing super capacitor as claimed in claim 1, wherein coconut shell is used as carbonization material, and physical activation is carried out on the carbonization material by physical activation method process using water vapor as main activating agent to obtain the active carbon.
3. The graphene modification method for preparing activated carbon of super capacitor as claimed in claim 1, wherein in the first step, the concentration of nitrogen or argon is 99.5%.
4. The method for modifying activated carbon graphene for preparing a supercapacitor according to claim 1, wherein the cooling temperature of the activated carbon deoxidizing material in the second step is 20-25 ℃ at normal temperature; and the natural cooling temperature in the third step is 20-25 ℃ normal temperature.
5. The method for modifying activated carbon graphene for preparing a supercapacitor according to claim 1, wherein in the second step, the mass concentration of the nickel nitrate or ferric nitrate or cobalt nitrate solution is 3%.
6. The method for modifying activated carbon graphene for preparing a supercapacitor according to claim 1, wherein in the third step, the activated carbon impregnant is placed under the protection of argon at 950 ℃, is subjected to heat preservation for 30-180 min, and is then naturally cooled.
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