CN113078001A - Graphene oxide/polyaniline/nano-copper composite electrode coating - Google Patents
Graphene oxide/polyaniline/nano-copper composite electrode coating Download PDFInfo
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- CN113078001A CN113078001A CN202110366336.XA CN202110366336A CN113078001A CN 113078001 A CN113078001 A CN 113078001A CN 202110366336 A CN202110366336 A CN 202110366336A CN 113078001 A CN113078001 A CN 113078001A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 54
- 238000000576 coating method Methods 0.000 title claims abstract description 37
- 239000011248 coating agent Substances 0.000 title claims abstract description 36
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 36
- 239000010949 copper Substances 0.000 title claims abstract description 33
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 23
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 claims abstract description 8
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000003647 oxidation Effects 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- 239000000178 monomer Substances 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 239000002518 antifoaming agent Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007822 coupling agent Substances 0.000 claims description 8
- 239000003223 protective agent Substances 0.000 claims description 8
- PLUHAVSIMCXBEX-UHFFFAOYSA-N azane;dodecyl benzenesulfonate Chemical group N.CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 PLUHAVSIMCXBEX-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 239000005457 ice water Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 238000005576 amination reaction Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 125000003277 amino group Chemical group 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 8
- 239000000654 additive Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 5
- -1 polydimethylsiloxane Polymers 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004108 freeze drying Methods 0.000 description 4
- 239000012286 potassium permanganate Substances 0.000 description 4
- 239000004317 sodium nitrate Substances 0.000 description 4
- 235000010344 sodium nitrate Nutrition 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 1
- GUQAPPPKAMUNSP-UHFFFAOYSA-N aniline;nitric acid Chemical compound O[N+]([O-])=O.NC1=CC=CC=C1 GUQAPPPKAMUNSP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
Classifications
-
- 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
- H01G11/84—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
-
- 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
-
- 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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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a preparation method of a graphene oxide/polyaniline/nano-copper composite electrode coating, wherein the electrode coating is formed by compounding graphene oxide, polyaniline and nano-copper; the method is characterized in that: the coating is prepared by carrying out in-situ polymerization on aminated modified graphene oxide and polyaniline-nano copper, modifying the graphene oxide by using a silane coupling agent, and introducing amino groups on the surface of the graphene oxide to form graftable graphene oxide; the graftable graphene oxide and aniline monomer are mixed, ultrasonically dispersed, and ammonium persulfate and copper nitrate are added for common oxidation to obtain the graphene oxide/polyaniline/nano-copper composite electrode coating. The raw materials used by the preparation method are easy to obtain, the method is simple, and the prepared electrode coating has higher conductivity, chemical structure stability, multiple-cycle discharge loss rate and specific capacitance than a single material.
Description
Technical Field
The invention relates to the technical field of conductive coatings, in particular to a preparation method of a graphene oxide/polyaniline/nano-copper composite electrode coating.
Background
In modern society today, energy storage technology has become more and more a critical technology. China is a world large country for automobile production and sale, and nowadays, the energy problem and the environmental pollution problem are continuously aggravated, the development of new energy automobiles is an important strategy for meeting the national requirements of energy conservation, emission reduction and low-carbon economy, and the development key of the new energy automobiles lies in the progress and innovation of battery technology.
The super capacitor is used as a novel electric energy storage device with excellent performance between a battery and a traditional capacitor, and can completely meet the requirements of the battery of a new energy automobile due to the characteristics of large stored energy, large power density, high charging and discharging speed, economy and environmental protection, so that the super capacitor is concerned by broad students and researchers. The technical key of the super capacitor lies in the selection and preparation of electrode materials.
Polyaniline is a good conductive polymer, has the characteristics of low cost, unique doping mechanism, reversible oxidation reduction, easily available raw materials, simple synthesis method and good environmental stability, is widely concerned, but has poor chemical stability, structural stability and mechanical property; graphene is a substance with high specific surface area, high conductivity, and good chemical stability and structural stability, and a composite material made of the graphene and polyaniline can have the advantages of the graphene and the polyaniline.
According to the preparation method, a silane coupling agent is used for modifying graphene oxide, and amino groups are introduced to the surface of the graphene oxide to form graftable graphene oxide; the graftable graphene oxide and aniline monomer are mixed, ultrasonically dispersed, and ammonium persulfate and copper nitrate are added for common oxidation to obtain the graphene oxide/polyaniline/nano-copper composite electrode coating.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene oxide/polyaniline/nano-copper composite electrode coating; the raw materials used by the preparation method are easy to obtain, the method is simple, and the prepared electrode coating has higher conductivity, chemical structure stability, multiple-cycle discharge loss rate and specific capacitance than a single material.
The invention adopts the following technical scheme for realizing the purpose:
a preparation method of a graphene oxide/polyaniline/nano-copper composite electrode coating comprises the following steps: 10% -45% of graphene oxide; 30% -70% of polyaniline; 1% -10% of nano copper; 1% -1.5% of reducing agent; 1% -2% of a coupling agent.
Further, the graphene oxide is modified graphene oxide through amination.
Further, the polyaniline is prepared by an in-situ polymerization method.
Further, the nano copper is obtained by adding copper nitrate in the in-situ polymerization process and co-oxidizing, and the particle size is 50-100 nm.
Further, the coupling agent is a silane coupling agent.
Further, the defoaming agent is polydimethylsiloxane.
Further, the protective agent is ammonium dodecylbenzene sulfonate.
A preparation method of graphene oxide/polyaniline/nano-copper composite electrode paint comprises the following steps
Preparing graphene oxide powder in step (1): preparing the flake graphite into graphene oxide powder by a modified hummers method.
Preparing ammonia amination graphene oxide: preparing 1g of graphene oxide powder and 50ml of toluene into a solution, adding 0.1g of silane coupling agent KH550 into the solution, performing ultrasonic dispersion at normal temperature for 15min, and reacting the solution at 100 ℃ for 6h to obtain the aminated graphene oxide.
Preparing an aniline nitric acid solution: 0.05g of aniline was weighed and dissolved in 15ml of a 1mol/L nitric acid solution.
Preparing an in-situ polymerization oxidation liquid: weigh 0.05g ammonium persulfate and 0.084g CuNO3The resulting mixture was dissolved in 15ml of a 1mol/L nitric acid solution to prepare an oxidizing solution.
And (5) mixing the solutions obtained in the steps 2, 3 and 4, adding a defoaming agent and a protective agent, reacting in an ice-water bath for 6 hours, stirring at room temperature for 6 hours, and performing suction filtration. And (5) washing the product obtained in the step (5) by using distilled water and ethanol in sequence, and drying in vacuum to obtain the graphene oxide/polyaniline/nano-copper composite electrode coating.
Further, the step 1 specifically includes: taking a proper amount of concentrated sulfuric acid, sodium nitrate and 2g of flake graphite, uniformly mixing at 0 ℃, slowly dropwise adding 6g of potassium permanganate, reacting at 30 ℃ for 30min, adding a proper amount of deionized water and a hydrogen peroxide solution, continuously reacting for 10min, repeatedly washing the obtained product with the deionized water and a dilute hydrochloric acid solution, and finally freeze-drying to obtain the graphene oxide.
Further, the step 2 specifically includes: adding 1g of graphene oxide, 50ml of toluene solution and 0.1g of silane coupling agent KH550 into a 250ml beaker, performing ultrasonic dispersion for 15min, and stirring and reacting for 6h at 100 ℃ by using a magnetic stirrer to obtain the aminated modified graphene oxide.
Further, the step 3 specifically includes: adding 15ml of nitric acid solution with the concentration of 1mol/L into a 50ml beaker, adding 0.05g of aniline, and performing ultrasonic dispersion for 15 min.
Further, the step 4 specifically includes: adding 15ml of nitric acid solution with the concentration of 1mol/L into a 50ml beaker, and then adding 0.05g of ammonium persulfate and 0.084g of CuNO3And carrying out ultrasonic dispersion for 15 min.
Further, the step 5 specifically includes: and (3) slowly introducing the solution obtained in the step (3) and (4) into the beaker obtained in the step (2), adding a defoaming agent polydimethylsiloxane and a protective agent ammonium dodecylbenzene sulfonate, reacting for 6 hours in an ice-water bath, stirring for 6 hours on a magnetic stirrer, washing for 3 times by using distilled water and alcohol, and performing vacuum drying to obtain the electrode coating.
Has the advantages that:
compared with the prior art, the invention has the beneficial effects that: as a novel conductive coating, the amine-group-graftable polyaniline is introduced on the surface of graphene oxide by adding the silane coupling agent KH550, and the electrode coating can be obtained by adding the nano-copper and the amine-group-modified graphene oxide in the process of polyaniline in-situ polymerization reaction to generate polyaniline.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
The electrode coating comprises the following components in parts by mass: 30% graphene oxide; 60% of polyaniline; 5% of nano copper; 5% of additive.
The graphene oxide in the components is amino-modified graphene oxide, and the additive comprises 1% of coupling agent, 2% of defoaming agent and 2% of protective agent.
The graphene oxide/polyaniline/nano-copper composite electrode coating is prepared by the following steps:
step 1, taking a proper amount of concentrated sulfuric acid, uniformly mixing sodium nitrate and 2g of flake graphite at 0 ℃, then slowly dropwise adding 6g of potassium permanganate, reacting at 30 ℃ for 30min, adding a proper amount of deionized water and a hydrogen peroxide solution, continuing to react for 10min, repeatedly washing the obtained product with the deionized water and a dilute hydrochloric acid solution, and finally freeze-drying to obtain the graphene oxide.
And 2, adding 1g of graphene oxide, 50ml of toluene solution and 0.1g of silane coupling agent KH550 into a 250ml beaker, performing ultrasonic dispersion for 15min, and stirring and reacting for 6h at 100 ℃ by using a magnetic stirrer to obtain the aminated modified graphene oxide.
And 3, adding 10ml of nitric acid solution with the concentration of 1mol/L into a 50ml beaker, adding 0.03g of aniline, and performing ultrasonic dispersion for 15 min.
Step 4, adding 10ml of nitric acid solution with the concentration of 1mol/L into a 50ml beaker, and then adding 0.03g of ammonium persulfate and 0.08g of CuNO3And carrying out ultrasonic dispersion for 15 min.
And 5, slowly introducing the solution obtained in the step 3 and the step 4 into the beaker obtained in the step 2, adding 2ml of polydimethylsiloxane and 2ml of ammonium dodecylbenzene sulfonate, reacting for 6 hours in an ice-water bath, stirring for 6 hours on a magnetic stirrer, washing for 3 times by using distilled water and alcohol, and performing vacuum drying to obtain the electrode coating.
Example 2
The electrode coating comprises the following components in parts by mass: 45% graphene oxide; 45% of polyaniline; 5% of nano copper; 5% of additive.
The graphene oxide in the components is amino-modified graphene oxide, and the additive comprises 2% of a coupling agent, 1% of a defoaming agent and 2% of a protective agent.
The graphene oxide/polyaniline/nano-copper composite electrode coating is prepared by the following steps:
step 1, taking a proper amount of concentrated sulfuric acid, uniformly mixing sodium nitrate and 2g of flake graphite at 0 ℃, then slowly dropwise adding 6g of potassium permanganate, reacting at 30 ℃ for 30min, adding a proper amount of deionized water and a hydrogen peroxide solution, continuing to react for 10min, repeatedly washing the obtained product with the deionized water and a dilute hydrochloric acid solution, and finally freeze-drying to obtain the graphene oxide.
And 2, adding 1.2g of graphene oxide, 50ml of toluene solution and 0.15g of silane coupling agent KH550 into a 250ml beaker, performing ultrasonic dispersion for 15min, and stirring and reacting for 6h at 90 ℃ by using a magnetic stirrer to obtain the aminated modified graphene oxide.
And 3, adding 15ml of nitric acid solution with the concentration of 1mol/L into a 50ml beaker, adding 0.05g of aniline, and performing ultrasonic dispersion for 15 min.
Step 4, adding 15ml of nitric acid solution with the concentration of 1mol/L into a 50ml beaker, and then adding 0.05g of ammonium persulfate and 0.09g of CuNO3And carrying out ultrasonic dispersion for 15 min.
And 5, slowly introducing the solution obtained in the step 3 and the step 4 into the beaker obtained in the step 2, adding 1ml of polydimethylsiloxane and 2ml of ammonium dodecylbenzene sulfonate, reacting for 6 hours in ice-water bath, stirring for 6 hours on a magnetic stirrer, washing for 3 times by using distilled water and alcohol, and performing vacuum drying to obtain the electrode coating.
Example 3
The electrode coating comprises the following components in parts by mass: 55% graphene oxide; 35% of polyaniline; 5% of nano copper; 5% of additive.
The graphene oxide in the components is amino-modified graphene oxide, and the additive comprises 3% of a coupling agent, 1% of a defoaming agent and 1% of a protective agent.
The graphene oxide/polyaniline/nano-copper composite electrode coating is prepared by the following steps:
step 1, taking a proper amount of concentrated sulfuric acid, uniformly mixing sodium nitrate and 3g of flake graphite at 0 ℃, slowly dropwise adding 9g of potassium permanganate, reacting at 30 ℃ for 30min, adding a proper amount of deionized water and a hydrogen peroxide solution, continuously reacting for 10min, repeatedly washing the obtained product with the deionized water and a dilute hydrochloric acid solution, and finally freeze-drying to obtain the graphene oxide.
And 2, adding 1.5g of graphene oxide, 50ml of toluene solution and 0.2g of silane coupling agent KH550 into a 250ml beaker, performing ultrasonic dispersion for 15min, and stirring and reacting for 6h at 100 ℃ by using a magnetic stirrer to obtain the aminated modified graphene oxide.
And 3, adding 20ml of nitric acid solution with the concentration of 1mol/L into a 50ml beaker, adding 0.065g of aniline, and performing ultrasonic dispersion for 15 min.
Step 4, adding 20ml of nitric acid solution with the concentration of 1mol/L into a 50ml beaker, and then adding 0.065g of ammonium persulfate and 0.1g of CuNO3And carrying out ultrasonic dispersion for 20 min.
And 5, slowly introducing the solution obtained in the step 3 and the step 4 into the beaker obtained in the step 2, adding 1ml of polydimethylsiloxane and 1ml of ammonium dodecylbenzene sulfonate, reacting for 6 hours in ice-water bath, stirring for 6 hours on a magnetic stirrer, washing for 3 times by using distilled water and alcohol, and performing vacuum drying to obtain the electrode coating.
The invention is not the best known technology.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. A preparation method of graphene oxide/polyaniline/nano-copper composite electrode coating is characterized by comprising the following steps: the coating is prepared by in-situ polymerization of aminated modified graphene oxide and polyaniline-nano copper, and the electrode coating comprises the following components in percentage by mass: 10% -45% of graphene oxide; 30% -70% of polyaniline; 1% -10% of nano copper; 1% -3% of a coupling agent; 1% -3% of a coupling agent; 1% -3% of defoaming agent.
2. The graphene oxide/polyaniline/nano-copper composite electrode coating as claimed in claim 1, wherein: the graphene oxide is modified graphene oxide through amination.
3. The graphene oxide/polyaniline/nano-copper composite electrode coating as claimed in claim 1, wherein: the polyaniline is prepared by an in-situ polymerization method.
4. The graphene oxide/polyaniline/nano-copper composite electrode coating as claimed in claim 1, wherein: the nano copper is obtained by adding copper nitrate in the in-situ polymerization process and co-oxidizing, and the particle size is 50-100 nm.
5. The graphene oxide/polyaniline/nano-copper composite electrode coating as claimed in claim 1, wherein: the coupling agent is silane coupling agent which can be KH540, KH550, KH792 and KH 602.
6. The graphene oxide/polyaniline/nano-copper composite electrode coating as claimed in claim 1, wherein: the defoaming agent is an organic silicon defoaming agent.
7. The graphene oxide/polyaniline/nano-copper composite electrode coating as claimed in claim 1, wherein: the protective agent is ammonium dodecylbenzene sulfonate.
8. The graphene oxide/polyaniline/nano-copper composite electrode coating as claimed in claim 1, wherein: the preparation method comprises the following steps of (1) preparing the crystalline flake graphite into graphene oxide powder; (2) preparing 1g of graphene oxide powder and 50ml of toluene into a solution; (3) adding 0.1g of silane coupling agent into the solution in the step 2, and performing ultrasonic dispersion for 15min at normal temperature; (4) step 3, reacting the solution at 100 ℃ for 6 hours to obtain aminated graphene oxide; (5) weighing 0.05g of aniline monomer, and dissolving in 15ml of nitric acid solution with the concentration of 1 mol/L; (6) weigh 0.05g ammonium persulfate and 0.084g CuNO3Dissolving in 15ml nitric acid solution with the concentration of 1mol/L to prepare oxidation solution; (7) mixing the solutions obtained in the steps 4, 5 and 6, adding a defoaming agent and a protective agent, and putting the mixture in an ice-water bathThe reaction is carried out for 6h, and then the mixture is stirred for 6h at room temperature and filtered by suction. (8) And (3) washing the product obtained in the step (8) by using distilled water and ethanol in sequence, and drying in vacuum to obtain the graphene oxide/polyaniline/nano-copper composite electrode coating.
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| CN114242468A (en) * | 2021-12-28 | 2022-03-25 | 安徽理工大学 | Self-supporting three-dimensional graphene oxide/polyaniline/carbon quantum dot electrode material |
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| CN109559899A (en) * | 2018-12-04 | 2019-04-02 | 黑龙江大学 | The preparation method of the graphene-supported cupro-nickel solid solution composite material of polyaniline-coated |
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