CN112509822A - Preparation method and application of electrode material of polyaniline grafted carbon nanotube - Google Patents

Preparation method and application of electrode material of polyaniline grafted carbon nanotube Download PDF

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CN112509822A
CN112509822A CN202011299051.0A CN202011299051A CN112509822A CN 112509822 A CN112509822 A CN 112509822A CN 202011299051 A CN202011299051 A CN 202011299051A CN 112509822 A CN112509822 A CN 112509822A
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carbon nanotube
polyaniline
electrode material
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李立健
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Huanyu Energy Saving Technology Guangzhou Co ltd
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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
    • H01G11/84—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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
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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
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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
    • 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
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • H—ELECTRICITY
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    • 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
    • H01G11/48—Conductive polymers
    • 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
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/13—Energy storage using capacitors

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Abstract

The invention relates to the technical field of super capacitors and discloses a polyaniline grafted carbon nanotube electrode material, which is characterized in that an aniline monomer and a diphenylamine group of a carbon nanotube are copolymerized through in-situ oxidative polymerization to obtain a polyaniline chemically grafted carbon nanotube, the polyaniline and the carbon nanotube are organically combined through the connection of chemical bonds to avoid the conditions of phase separation and falling off of the polyaniline and the carbon nanotube, a stable composite structure is formed, the overall structural stability of the electrode material is improved, the rapid loss of capacitance is avoided, the excellent electrochemical cycle stability is shown, the chemical bond grafting effect is realized, the agglomeration phenomenon of the carbon nanotube is reduced, meanwhile, the aniline and the carbon nanotube are more favorable for forming a three-dimensional conductive network, the transmission of electrons is promoted, electrolyte ions are diffused into the electrode, a better pseudocapacitance reaction is realized, and a better energy storage reaction is realized, resulting in higher pseudocapacitance and double layer capacitance.

Description

Preparation method and application of electrode material of polyaniline grafted carbon nanotube
Technical Field
The invention relates to the technical field of super capacitors, in particular to a preparation method and application of an electrode material of a polyaniline grafted carbon nanotube.
Background
With the increasing energy crisis and environmental pollution all over the world, the dependence on new energy and renewable clean energy is increasing, the development of novel sustainable energy storage and supply equipment becomes a research hotspot, the super capacitor is a novel energy storage device between the traditional capacitor and the battery, has the characteristics of large capacity, high energy density, large power density, long service life and the like compared with the traditional capacitor, has wide application prospect in the fields of electronic elements, portable electronic equipment, new energy automobiles, power generation devices and the like, and the influence of the electrode active material of the super capacitor on the electrochemical performance is the greatest.
The super capacitor can be divided into an electric double layer capacitor and a pseudo capacitor, the electric double layer capacitor mainly uses an active carbon-based material as an electrode material, and has the advantages of good conductivity, high specific surface area and the like, but the actual specific capacitance of the active carbon-based material is not high, the pseudocapacitance capacitor mainly uses transition metal oxide and conductive polymer as electrode materials, wherein the polyaniline, polypyrrole, polythiophene and other conductive polymers can generate rapid and reversible redox reaction, the theoretical specific capacitance is very high, but the polyaniline-based electrode material matrix is easy to be lost, the electrochemical cycle stability is poor, the active carbon-based material and the conductive polymer are compounded at present, the advantages of double electric layer capacitance and pseudo capacitance are integrated, the development of super capacitor electrode materials with fast charge-discharge rate, high specific capacitance and excellent cycle stability becomes a research hotspot.
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method and application of an electrode material of a polyaniline grafted carbon nanotube, and the electrode material has higher actual pseudo capacitance and double-layer capacitance and excellent electrochemical cycle stability.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the electrode material of the polyaniline grafted carbon nanotube comprises the following steps:
(1) adding p-aminodiphenylamine, an ethanol solvent and concentrated hydrochloric acid into a reaction beaker, and controlling the mass fraction of hydrochloric acid in the total solution to be 10-20%.
(2) Putting the solution into an ultrasonic disperser, performing ultrasonic treatment until the solution is uniformly dispersed, adding sodium nitrite into an ice-water bath system, stirring and reacting for 1-2h, slowly dropwise adding the dispersion liquid of the carbon nano tube uniformly dispersed by ultrasonic treatment, continuing to react for 2-5h, stirring and reacting for 10-20h at room temperature, heating to 70-80 ℃, stirring and reacting for 10-20h, filtering to remove the solvent, deionized water and ethanol, and washing to obtain the diphenylamine-based carbon nano tube.
(3) Adding diphenylamine-based carbon nanotubes and deionized water into a reaction beaker, performing ultrasonic treatment until the mixture is uniformly dispersed, adding concentrated hydrochloric acid and aniline, controlling the concentration of hydrochloric acid in the total solution to be 2-3%, dropwise adding an ammonium persulfate solution in an ice-water bath system, reacting for 4-8h, then reacting for 8-12h at room temperature, filtering to remove the solvent, and washing with deionized water and ethanol to obtain the polyaniline grafted carbon nanotubes.
(4) Mixing the electrode material of the polyaniline grafted carbon nanotube with an ethanol solvent, uniformly dispersing by ultrasonic, coating the slurry on the surface of a glassy carbon electrode, and drying to obtain the electrode material of the polyaniline grafted carbon nanotube, wherein the electrode material is applied to a super capacitor.
Preferably, the mass ratio of the p-aminodiphenylamine to the sodium nitrite to the carbon nanotube is 500-620:220-280: 100.
Preferably, the supersound deconcentrator includes the water bath, water bath both sides fixedly connected with ultrasonic emitter, and water bath below is provided with the heat-conducting plate, and the heat-conducting plate below is provided with the heating plate, heat-conducting plate top and base fixed connection, base top swing joint has the pivot, pivot fixedly connected with limiting plate, is provided with the reaction beaker between the limiting plate.
Preferably, the mass ratio of the diphenylamine-based carbon nanotubes to the aniline and the ammonium persulfate in the step (3) is 5-20:100: 225-240.
(III) advantageous technical effects
Compared with the prior art, the invention has the following chemical mechanism and beneficial technical effects:
the polyaniline grafted carbon nanotube electrode material has the advantages that amino of p-aminodiphenylamine and sodium nitrite are subjected to diazotization reaction in a hydrochloric acid system to generate a diazo diphenylamine intermediate, diazo groups are removed to form carbocations to attack carbon on the carbon nanotube to obtain the diphenylamine-based carbon nanotube, a diphenylamine group is grafted to a matrix of the carbon nanotube, in-situ oxidative polymerization is carried out to copolymerize an aniline monomer and the diphenylamine group to obtain the polyaniline chemically grafted carbon nanotube, polyaniline and the carbon nanotube are organically combined through the connection of chemical bonds to avoid the conditions of phase separation and falling of the polyaniline and the carbon nanotube, a stable composite structure is formed, the swelling phenomenon of polyaniline molecules in electrolyte is reduced, the breaking and degradation of molecular chains are caused, the overall structural stability of the electrode material is improved, and the rapid loss of capacitance is avoided, the electrochemical cycle stability is excellent, the grafting effect of chemical bonds is realized, the agglomeration phenomenon of the carbon nano tubes is reduced, meanwhile, three-dimensional conductive networks are formed by the aniline and the carbon nano tubes, the transmission of electrons is promoted, electrolyte ions are diffused into the electrodes, and a better pseudocapacitance reaction is generated, so that a better energy storage reaction is performed, and a higher pseudocapacitance and a double-layer capacitance are generated.
Drawings
FIG. 1 is a schematic diagram of an ultrasonic disperser;
FIG. 2 is a schematic top view of a stopper plate structure;
fig. 3 is a limiting plate adjustment schematic.
1-ultrasonic disperser; 2-water bath; 3-an ultrasonic transmitter; 4-a heat-conducting plate; 5-heating a sheet; 6-a base; 7-a rotating shaft; 8-a limiting plate; 9-reaction beaker.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: a polyaniline graft carbon nanotube electrode material is prepared by the following steps:
(1) adding p-aminodiphenylamine, an ethanol solvent and concentrated hydrochloric acid into a reaction beaker, and controlling the mass fraction of hydrochloric acid in the total solution to be 10-20%.
(2) Placing the solution in an ultrasonic disperser, performing ultrasonic treatment until the solution is uniformly dispersed, wherein the ultrasonic disperser comprises a water bath, two sides of the water bath are fixedly connected with ultrasonic emitters, a heat conducting plate is arranged below the water bath, a heating plate is arranged below the heat conducting plate, the upper part of the heat conducting plate is fixedly connected with a base, a rotating shaft is movably connected above the base, a limiting plate is fixedly connected with the rotating shaft, a reaction beaker is arranged between the limiting plates, sodium nitrite is added into an ice-water bath system, stirring and reacting are performed for 1-2h, then the uniformly ultrasonically dispersed carbon nanotube dispersion liquid is slowly dripped, the mass ratio of the p-aminodiphenylamine, the sodium nitrite and the carbon nanotube is 500-, And washing with deionized water and ethanol to obtain the diphenylamine-based carbon nanotube.
(3) Adding diphenylamine-based carbon nanotubes and deionized water into a reaction beaker, performing ultrasonic treatment until the mixture is uniformly dispersed, adding concentrated hydrochloric acid and aniline, controlling the concentration of hydrochloric acid in the total solution to be 2-3%, dropwise adding an ammonium persulfate solution in an ice-water bath system, reacting for 4-8h, reacting for 8-12h at room temperature, filtering to remove the solvent, and washing with deionized water and ethanol to obtain the polyaniline grafted carbon nanotubes.
(4) Mixing the electrode material of the polyaniline grafted carbon nanotube with an ethanol solvent, uniformly dispersing by ultrasonic, coating the slurry on the surface of a glassy carbon electrode, and drying to obtain the electrode material of the polyaniline grafted carbon nanotube, wherein the electrode material is applied to a super capacitor.
Example 1
(1) Adding p-aminodiphenylamine, an ethanol solvent and concentrated hydrochloric acid into a reaction beaker, and controlling the mass fraction of the hydrochloric acid in the total solution to be 20%.
(2) The solution is placed in an ultrasonic disperser to be ultrasonically dispersed uniformly, the ultrasonic disperser comprises a water bath tank, ultrasonic emitters are fixedly connected with two sides of the water bath tank, a heat conducting plate is arranged below the water bath tank, a heating plate is arranged below the heat conducting plate, the upper part of the heat conducting plate is fixedly connected with a base, a rotating shaft is movably connected above the base, a limiting plate is fixedly connected with the rotating shaft, a reaction beaker is arranged between the limiting plates, adding sodium nitrite into an ice-water bath system, stirring and reacting for 2 hours, slowly dropwise adding dispersion liquid of the carbon nano tube uniformly dispersed by ultrasonic, wherein the mass ratio of the p-aminodiphenylamine to the sodium nitrite to the carbon nano tube is 620:280:100, the reaction is continued for 5 hours, then the reaction is stirred at the room temperature for 12 hours, heating to 80 ℃, stirring for reaction for 15h, filtering to remove the solvent, deionized water and ethanol for washing, and obtaining the diphenylamine-based carbon nanotube.
(3) Adding diphenylamine-based carbon nanotubes and deionized water into a reaction beaker, performing ultrasonic treatment until the mixture is uniformly dispersed, adding concentrated hydrochloric acid and aniline, controlling the concentration of hydrochloric acid in the total solution to be 2.5%, dropwise adding an ammonium persulfate solution in an ice-water bath system, reacting for 4 hours, reacting for 12 hours at room temperature, filtering to remove a solvent, and washing with deionized water and ethanol to obtain the polyaniline grafted carbon nanotubes.
(4) Mixing the electrode material of the polyaniline grafted carbon nano tube with an ethanol solvent, uniformly dispersing by ultrasonic, coating the slurry on the surface of a glassy carbon electrode, and drying to obtain the electrode material of the polyaniline grafted carbon nano tube.
Example 2
(1) Adding p-aminodiphenylamine, an ethanol solvent and concentrated hydrochloric acid into a reaction beaker, and controlling the mass fraction of hydrochloric acid in the total solution to be 15%.
(2) The solution is placed in an ultrasonic disperser to be ultrasonically dispersed uniformly, the ultrasonic disperser comprises a water bath tank, ultrasonic emitters are fixedly connected with two sides of the water bath tank, a heat conducting plate is arranged below the water bath tank, a heating plate is arranged below the heat conducting plate, the upper part of the heat conducting plate is fixedly connected with a base, a rotating shaft is movably connected above the base, a limiting plate is fixedly connected with the rotating shaft, a reaction beaker is arranged between the limiting plates, adding sodium nitrite into an ice-water bath system, stirring and reacting for 2 hours, slowly dropwise adding dispersion liquid of the carbon nano tube uniformly dispersed by ultrasonic, wherein the mass ratio of the p-aminodiphenylamine to the sodium nitrite to the carbon nano tube is 550:250:100, the reaction is continued for 2 hours, then the reaction is stirred at the room temperature for 15 hours, heating to 75 ℃, stirring for reaction for 20h, filtering to remove the solvent, deionized water and ethanol for washing, and obtaining the diphenylamine-based carbon nanotube.
(3) Adding diphenylamine-based carbon nanotubes and deionized water into a reaction beaker, performing ultrasonic treatment until the mixture is uniformly dispersed, adding concentrated hydrochloric acid and aniline, controlling the concentration of hydrochloric acid in the total solution to be 3%, dropwise adding an ammonium persulfate solution in an ice-water bath system, wherein the mass ratio of the diphenylamine-based carbon nanotubes to the aniline to the ammonium persulfate is 12:100:235, reacting for 8 hours, then reacting for 10 hours at room temperature, filtering to remove the solvent, and washing with the deionized water and ethanol to obtain the polyaniline grafted carbon nanotubes.
(4) Mixing the electrode material of the polyaniline grafted carbon nano tube with an ethanol solvent, uniformly dispersing by ultrasonic, coating the slurry on the surface of a glassy carbon electrode, and drying to obtain the electrode material of the polyaniline grafted carbon nano tube.
Example 3
(1) Adding p-aminodiphenylamine, an ethanol solvent and concentrated hydrochloric acid into a reaction beaker, and controlling the mass fraction of hydrochloric acid in the total solution to be 15%.
(2) The solution is placed in an ultrasonic disperser to be ultrasonically dispersed uniformly, the ultrasonic disperser comprises a water bath tank, ultrasonic emitters are fixedly connected with two sides of the water bath tank, a heat conducting plate is arranged below the water bath tank, a heating plate is arranged below the heat conducting plate, the upper part of the heat conducting plate is fixedly connected with a base, a rotating shaft is movably connected above the base, a limiting plate is fixedly connected with the rotating shaft, a reaction beaker is arranged between the limiting plates, adding sodium nitrite into an ice-water bath system, stirring and reacting for 1h, slowly dropwise adding dispersion liquid of the carbon nano tube uniformly dispersed by ultrasonic, wherein the mass ratio of the p-aminodiphenylamine to the sodium nitrite to the carbon nano tube is 620:280:100, the reaction is continued for 5 hours, then the reaction is stirred at the room temperature for 20 hours, heating to 80 ℃, stirring for reaction for 10h, filtering to remove the solvent, deionized water and ethanol for washing, and obtaining the diphenylamine-based carbon nanotube.
(3) Adding diphenylamine-based carbon nanotubes and deionized water into a reaction beaker, performing ultrasonic treatment until the mixture is uniformly dispersed, adding concentrated hydrochloric acid and aniline, controlling the concentration of hydrochloric acid in the total solution to be 3%, dropwise adding an ammonium persulfate solution in an ice-water bath system, reacting for 6 hours, reacting for 12 hours at room temperature, filtering to remove a solvent, and washing with deionized water and ethanol to obtain the polyaniline grafted carbon nanotubes.
(4) Mixing the electrode material of the polyaniline grafted carbon nano tube with an ethanol solvent, uniformly dispersing by ultrasonic, coating the slurry on the surface of a glassy carbon electrode, and drying to obtain the electrode material of the polyaniline grafted carbon nano tube.
Comparative example 1
(1) Adding p-aminodiphenylamine, an ethanol solvent and concentrated hydrochloric acid into a reaction beaker, and controlling the mass fraction of hydrochloric acid in the total solution to be 15%.
(2) The solution is placed in an ultrasonic disperser to be ultrasonically dispersed uniformly, the ultrasonic disperser comprises a water bath tank, ultrasonic emitters are fixedly connected with two sides of the water bath tank, a heat conducting plate is arranged below the water bath tank, a heating plate is arranged below the heat conducting plate, the upper part of the heat conducting plate is fixedly connected with a base, a rotating shaft is movably connected above the base, a limiting plate is fixedly connected with the rotating shaft, a reaction beaker is arranged between the limiting plates, adding sodium nitrite into an ice-water bath system, stirring and reacting for 1h, slowly dropwise adding dispersion liquid of the carbon nano tube uniformly dispersed by ultrasonic, wherein the mass ratio of the p-aminodiphenylamine to the sodium nitrite to the carbon nano tube is 450:200:100, the reaction is continued for 3 hours, then the reaction is stirred at the room temperature for 15 hours, heating to 80 ℃, stirring for reaction for 12h, filtering to remove the solvent, deionized water and ethanol for washing, and obtaining the diphenylamine-based carbon nanotube.
(3) Adding diphenylamine-based carbon nanotubes and deionized water into a reaction beaker, performing ultrasonic treatment until the mixture is uniformly dispersed, adding concentrated hydrochloric acid and aniline, controlling the concentration of hydrochloric acid in the total solution to be 2.5%, dropwise adding an ammonium persulfate solution in an ice-water bath system, reacting for 4 hours, reacting for 10 hours at room temperature, filtering to remove a solvent, and washing with deionized water and ethanol to obtain the polyaniline grafted carbon nanotubes.
(4) Mixing the electrode material of the polyaniline grafted carbon nano tube with an ethanol solvent, uniformly dispersing by ultrasonic, coating the slurry on the surface of a glassy carbon electrode, and drying to obtain the electrode material of the polyaniline grafted carbon nano tube.
Comparative example 2
(1) Adding p-aminodiphenylamine, an ethanol solvent and concentrated hydrochloric acid into a reaction beaker, and controlling the mass fraction of the hydrochloric acid in the total solution to be 20%.
(2) The solution is placed in an ultrasonic disperser to be ultrasonically dispersed uniformly, the ultrasonic disperser comprises a water bath tank, ultrasonic emitters are fixedly connected with two sides of the water bath tank, a heat conducting plate is arranged below the water bath tank, a heating plate is arranged below the heat conducting plate, the upper part of the heat conducting plate is fixedly connected with a base, a rotating shaft is movably connected above the base, a limiting plate is fixedly connected with the rotating shaft, a reaction beaker is arranged between the limiting plates, adding sodium nitrite into an ice-water bath system, stirring and reacting for 1.5h, slowly dropwise adding dispersion liquid of the carbon nano tube uniformly dispersed by ultrasonic, wherein the mass ratio of the p-aminodiphenylamine to the sodium nitrite to the carbon nano tube is 660:320:100, the reaction is continued for 3 hours, then the reaction is stirred at room temperature for 12 hours, heating to 70 ℃, stirring for reaction for 12h, filtering to remove the solvent, deionized water and ethanol for washing, and obtaining the diphenylamine-based carbon nanotube.
(3) Adding diphenylamine-based carbon nanotubes and deionized water into a reaction beaker, performing ultrasonic treatment until the mixture is uniformly dispersed, adding concentrated hydrochloric acid and aniline, controlling the concentration of hydrochloric acid in the total solution to be 3%, dropwise adding an ammonium persulfate solution in an ice-water bath system, reacting for 4 hours, reacting for 12 hours at room temperature, filtering to remove a solvent, and washing with deionized water and ethanol to obtain the polyaniline grafted carbon nanotubes.
(4) Mixing the electrode material of the polyaniline grafted carbon nano tube with an ethanol solvent, uniformly dispersing by ultrasonic, coating the slurry on the surface of a glassy carbon electrode, and drying to obtain the electrode material of the polyaniline grafted carbon nano tube.
A polyaniline grafted carbon nanotube electrode material is used as a working electrode, a platinum sheet is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, 1mol/L sulfuric acid solution is used as electrolyte, a three-electrode system is adopted, cyclic voltammetry and electrochemical energy storage tests are carried out at a CHI760D electrochemical workstation, and the national standard of the tests is GB/T34870.1-2017.
Figure BDA0002786277000000081

Claims (4)

1. An electrode material of polyaniline grafted carbon nanotubes, which is characterized in that: the preparation method of the polyaniline grafted carbon nanotube electrode material comprises the following steps:
(1) adding p-aminodiphenylamine, an ethanol solvent and concentrated hydrochloric acid into a reaction beaker, and controlling the mass fraction of hydrochloric acid in the total solution to be 10-20%;
(2) putting the solution into an ultrasonic disperser, performing ultrasonic treatment until the solution is uniformly dispersed, adding sodium nitrite into an ice-water bath system, stirring and reacting for 1-2h, slowly dropwise adding the dispersion liquid of the carbon nano tube uniformly dispersed by ultrasonic treatment, continuing to react for 2-5h, stirring and reacting for 10-20h at room temperature, heating to 70-80 ℃, and stirring and reacting for 10-20h to obtain a diphenylamine-based carbon nano tube;
(3) adding diphenylamine-based carbon nanotubes and deionized water into a reaction beaker, performing ultrasonic treatment until the mixture is uniformly dispersed, adding concentrated hydrochloric acid and aniline, controlling the concentration of hydrochloric acid in the total solution to be 2-3%, dropwise adding an ammonium persulfate solution into an ice-water bath system, reacting for 4-8h, and then reacting for 8-12h at room temperature to obtain polyaniline grafted carbon nanotubes;
(4) mixing the electrode material of the polyaniline grafted carbon nano tube with an ethanol solvent, uniformly dispersing by ultrasonic, coating the slurry on the surface of a glassy carbon electrode, and drying to obtain the electrode material of the polyaniline grafted carbon nano tube.
2. The polyaniline-grafted carbon nanotube electrode material of claim 1, wherein: the mass ratio of the p-aminodiphenylamine to the sodium nitrite to the carbon nano tube is 500-620:220-280: 100.
3. The polyaniline-grafted carbon nanotube electrode material of claim 1, wherein: the ultrasonic disperser comprises a water bath, ultrasonic emitters are fixedly connected to two sides of the water bath, a heat-conducting plate is arranged below the water bath, a heating plate is arranged below the heat-conducting plate, the upper part of the heat-conducting plate is fixedly connected with a base, a rotating shaft is movably connected to the upper part of the base, a limiting plate is fixedly connected with the rotating shaft, and a reaction beaker is arranged between the limiting plates.
4. The polyaniline-grafted carbon nanotube electrode material of claim 1, wherein: the mass ratio of the diphenylamine-based carbon nanotubes to the aniline to the ammonium persulfate in the step (3) is 5-20:100: 225-240.
CN202011299051.0A 2020-11-18 2020-11-18 Preparation method and application of electrode material of polyaniline grafted carbon nanotube Withdrawn CN112509822A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116606505A (en) * 2023-05-08 2023-08-18 南通鹿波汽车零部件有限公司 Carbon nano tube modified thermoplastic vulcanized rubber and synthesis process thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116606505A (en) * 2023-05-08 2023-08-18 南通鹿波汽车零部件有限公司 Carbon nano tube modified thermoplastic vulcanized rubber and synthesis process thereof
CN116606505B (en) * 2023-05-08 2024-01-16 南通鹿波汽车零部件有限公司 Carbon nano tube modified thermoplastic vulcanized rubber and synthesis process thereof

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Application publication date: 20210316