CN111349237A - Polyfluoro functional polybenzazole electrode material applied to supercapacitor and preparation method thereof - Google Patents
Polyfluoro functional polybenzazole electrode material applied to supercapacitor and preparation method thereof Download PDFInfo
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- CN111349237A CN111349237A CN202010159634.7A CN202010159634A CN111349237A CN 111349237 A CN111349237 A CN 111349237A CN 202010159634 A CN202010159634 A CN 202010159634A CN 111349237 A CN111349237 A CN 111349237A
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0622—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0627—Polycondensates containing six-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- H01G11/48—Conductive polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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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 a polyfluoro functional polybenzazole electrode material applied to a super capacitor and a preparation method thereof, belonging to the technical field of electrode materials of super capacitors, wherein the precursor structure of the polybenzazole electrode material is substituted at 4, 5, 6 or 7 positions of indole molecules, the number of the substituted positions is 1, 2, 3 and 4 respectively, and R is R1Is trifluoromethyl or trifluoroethyl, the R2Is fluorine atom, trifluoromethyl or trifluoroethyl. The polyfluoro functional polybenzazole film electrode of the super capacitor adopts polyfluoro functional polybenzazole filmThe film is used as a supercapacitor electrode, and the synergistic effect of polyfluorinated modification and a special indole condensed ring structure is fully utilized, so that the film has a higher specific capacitance value and good charge-discharge cycle stability, and has a good application prospect when being used as a supercapacitor electrode material.
Description
Technical Field
The invention relates to the technical field of electrode materials of supercapacitors, in particular to a polyfluorinated functional polybenzazole electrode material applied to a supercapacitor and a preparation method thereof.
Background
With the rapid consumption of fossil fuels and the increasing deterioration of environmental pollution caused by the consumption of large amounts of fossil fuels, there is an increasing demand for the effective utilization of energy and the search for renewable and clean energy sources that can replace fossil fuels. Energy storage is an intermediate step in achieving versatile, clean and efficient use of energy and has attracted extensive attention and increased research interest worldwide. Compared with the traditional capacitor, the super capacitor is an electrochemical energy storage device with great development prospect, and has the characteristics of high energy density, good power density, fast charge and discharge, long cycle life and the like, so that the super capacitor has attracted extensive attention in academic and industrial fields in the past decades.
As an extremely important electrode material of a super capacitor, the preparation process of the conductive polymer is simpler, the cost is lower, and the comprehensive performance is more excellent, including higher conductivity and electrochemical activity, so that the conductive polymer becomes one of the most promising electrode materials of the super capacitor. Compared with typical conducting polymers polyaniline, polypyrrole and polythiophene, polybenzazole belonging to a condensed ring family bears the structural characteristics of polyparaphenylene and polypyrrole, so that the polybenzazole has the advantages of good thermal stability, electrochemical reversibility and the like, and is receiving more and more attention. However, the specific capacitance of pure polybenzazole prepared by direct electropolymerization only reaches 103F g-1, and the capacitance retention rate after 5000 circles is only 68%, which greatly limits the application of the polybenzazole in the field of supercapacitors. Based on this problem, structural modification is an important way to modify polymers.
Fluorine atoms have a high electronegativity and a minimum atomic radius (excluding H), and fluorine-containing groups are regarded as a special group for improving polymer properties. The existence of fluorine atoms can often form stronger hydrogen bonding action in molecules and among molecules, the introduction of a plurality of fluorine atoms can further strengthen the interaction force among molecules, and the introduction of a plurality of fluorine atoms can not cause excessive steric hindrance among molecules, so that the polymer has better thermal stability, oxidation stability and structural stability. The introduction of a plurality of fluorine atoms reduces the surface energy of the polymer, thereby greatly improving the morphological structure of the polymer, providing more active sites for pseudocapacitance reaction, and having positive influence on the improvement of the capacitance performance of the conductive polymer. However, after multi-fluorination of aniline, thiophene or pyrrole with a single-ring structure, the electrochemical activity of the corresponding polymer is obviously reduced, and indole has a special condensed-ring structure, so that the invention utilizes the multi-fluorination to regulate and control the capacitive performance of polybenzazole, and provides valuable reference for developing novel high-performance conductive polymer electrode materials.
Disclosure of Invention
Aiming at the technical problems, the invention provides a polyfluorinated functional polybenzazole electrode material applied to a supercapacitor and a preparation method thereof, which make full use of the synergistic effect of polyfluorinated modification and special condensed ring structure of indole, so that the polyfluorinated functional polybenzazole electrode material has higher specific capacitance value and good charge-discharge cycle stability, and has good application prospect as a supercapacitor electrode material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a precursor structure of the polybenzazole electrode material is substituted on 4, 5, 6 or 7 sites of indole molecules, the number of substitution is 1, 2, 3 and 4 respectively, and the molecular structure is shown as the following formula:
wherein said R1Is trifluoromethyl or trifluoroethyl, the R2Is fluorine atom, trifluoromethyl or trifluoroethyl.
The invention also discloses a preparation method of the polyfluoro functional polybenzazole electrode material applied to the super capacitor, which comprises the following steps:
(1) electrochemical solution formulation
Dissolving a polymer precursor in an organic solvent under the nitrogen atmosphere, and adding a supporting electrolyte into the organic solvent to obtain an electrochemical solution;
(2) electrodeposition of polyfluoro-functionalized polybenzazole films
And (2) placing the prepared electrochemical solution into an electrochemical reaction device, wherein the electrochemical reaction device adopts a three-electrode system (a working electrode, a reference electrode and a counter electrode), introducing nitrogen into the solution to remove dissolved oxygen in the solution, and electrodepositing the polyfluoro functional polybenzazole film on the working electrode by adopting a potentiostatic method or a continuous cyclic voltammetry method.
Preferably, the organic solvent is any one of acetonitrile and dichloromethane, and the supporting electrolyte is any one of tetrabutylammonium perchlorate, tetrabutylammonium hexafluorophosphate and tetrabutylammonium tetrafluoroborate.
Preferably, the concentration of the precursor in the electrochemical solution is 0.05-0.08mol/L, and the solubility of the supporting electrolyte is 0.1 mol/L.
Preferably, the potentiostatic polymerization potential is 1.40-1.55V, and the polymerization electric quantity is controlled within the range of 28-30mC/cm2In the meantime.
The beneficial effects of the invention are as follows: according to the polyfluoro functional polybenzazole film electrode of the supercapacitor, the polyfluoro functional polybenzazole film is used as the supercapacitor electrode, and the synergistic effect of polyfluoro modification and a special indole condensed ring structure is fully utilized, so that the polyfluoro functional polybenzazole film electrode has a high specific capacitance value and good charge-discharge cycle stability, and has a good application prospect when being used as a supercapacitor electrode material.
Drawings
FIG. 1 is a graph of the electrode surface topography of poly (6-trifluoromethylindole) in example 1;
FIG. 2 is a graph showing the charge-discharge curves (A) and specific capacitances (B) of poly (6-trifluoromethylindole) in example 1 at different current densities in a 1mol/L sulfuric acid solution;
FIG. 3 is a graph showing the charge and discharge stability of poly (6-trifluoromethylindole) in example 1 in a 1mol/L sulfuric acid solution.
Detailed Description
To facilitate understanding of those skilled in the art, the present invention will be further described with reference to specific examples.
Example 1:
a preparation method of a polyfluoro functional polybenzazole electrode material applied to a super capacitor comprises the following steps:
(1) electrochemical solution formulation
Dissolving a precursor 6-trifluoromethyl indole in dichloromethane in a nitrogen atmosphere, and adding a supporting electrolyte tetrabutylammonium tetrafluoroborate into the dichloromethane to obtain an electrochemical solution, wherein the concentration of the precursor is 0.08mol/L, and the solubility of the supporting electrolyte is 0.1 mol/L;
(2) electrodeposition of polyfluoro-functionalized polybenzazole films
Placing the prepared electrochemical solution into an electrochemical reaction device, wherein the electrochemical reaction device adopts a three-electrode system (a platinum wire with the diameter of 1mm is used as a working electrode, a platinum wire with the diameter of 1mm is used as a counter electrode and Ag/AgCl with the diameter of 1mm is used as a reference electrode), introducing nitrogen into the solution for 30min to remove dissolved oxygen in the solution, adopting a potentiostatic method, the potentiostatic method has a polymerization potential of 1.40V, and controlling the polymerization electric quantity range to be 28-30mC/cm2Meanwhile, a (6-trifluoromethyl indole) film is deposited on the working electrode.
Performing performance characterization on the obtained poly (6-trifluoromethylindole) film, wherein fig. 1 is an electrode surface topography of poly (6-trifluoromethylindole), and as shown in fig. 1, the surface of the conductive polymer electrode material is a three-dimensional flower-like structure with a plurality of cavities; FIG. 2 is a graph of charge-discharge curves (A) and specific capacitances (B) of poly (6-trifluoromethylindole) in 1mol/L sulfuric acid solution at different current densities, and as shown in FIG. 2, the electrode material shows typical pseudo-capacitance behavior, and the capacitance value at a current density of 10A g-1 is 296F g-1When the current density increased to 60A g-1Specific capacitance value of 175F g-1(ii) a FIG. 3 is a graph showing the charge-discharge stability of poly (6-trifluoromethylindole) in 1mol/L sulfuric acid solution, and as shown in FIG. 3, the stability of the material reaches 91% under the condition of 5000 charge-discharge cycles.
Example 2
A preparation method of a polyfluoro functional polybenzazole electrode material applied to a super capacitor comprises the following steps:
(1) electrochemical solution formulation
Dissolving a precursor 5, 6-difluoroindole in acetonitrile under the atmosphere of nitrogen, and adding tetrabutylammonium perchlorate serving as a supporting electrolyte into the acetonitrile to obtain an electrochemical solution, wherein the concentration of the precursor is 0.05mol/L, and the solubility of the supporting electrolyte is 0.1 mol/L;
(2) electrodeposition of polyfluoro-functionalized polybenzazole films
Placing the prepared electrochemical solution into an electrochemical reaction device, wherein the electrochemical reaction device adopts a three-electrode system (a platinum disk with the diameter of 3mm is used as a working electrode, a platinum wire with the diameter of 1mm is used as a counter electrode and Ag/AgCl with the diameter of 1mm is used as a reference electrode), introducing nitrogen into the solution for 30min to remove dissolved oxygen in the solution, adopting a potentiostatic method, the potentiostatic method has the polymerization potential of 1.40V, and controlling the polymerization electric quantity range to be 28-30mC/cm2Meanwhile, a (5, 6-difluoroindole) film is deposited on the working electrode.
The conductive polymer electrode material was determined to have a current density of 18A g-1Lower capacitance value of 291F g-1When the current density increased to 77A g-1Specific capacitance value of 220F g-1The stability of the material after 5000 circles reaches 82%.
Example 3
A preparation method of a polyfluoro functional polybenzazole electrode material applied to a super capacitor comprises the following steps:
(1) electrochemical solution formulation
Dissolving a precursor 5, 6, 7-tris (trifluoromethyl) indole in dichloromethane in a nitrogen atmosphere, and adding tetrabutylammonium hexafluorophosphate serving as a supporting electrolyte into the dichloromethane to obtain an electrochemical solution, wherein the concentration of the precursor is 0.05mol/L, and the solubility of the supporting electrolyte is 0.1 mol/L;
(2) electrodeposition of polyfluoro-functionalized polybenzazole films
Placing the prepared electrochemical solution into an electrochemical reaction device, wherein the electrochemical reaction device adopts a three-electrode system (the area is 1 × 2 cm)2The ITO conductive glass is used as a working electrode, and the area is 1.5 × 3cm2The platinum sheet is used as a counter electrode and Ag/AgCl with the diameter of 1mm is used as a reference electrode), nitrogen is introduced into the solution for 30min to remove dissolved oxygen in the solution, a potentiostatic method is adopted, the polymerization potential of the potentiostatic method is 1.50V, and the polymerization electric quantity is controlled within the range of 28-30mC/cm2Meanwhile, a (5, 6, 7-tris (trifluoromethyl) indole) film is electrodeposited on the working electrode.
Example 4
A preparation method of a polyfluoro functional polybenzazole electrode material applied to a super capacitor comprises the following steps:
(1) electrochemical solution formulation
Dissolving a precursor 4, 6, 7-tris (trifluoroethyl) indole in acetonitrile under the nitrogen atmosphere, and adding a supporting electrolyte tetrabutylammonium perchlorate into the acetonitrile to obtain an electrochemical solution, wherein the concentration of the precursor is 0.05mol/L, and the solubility of the supporting electrolyte is 0.1 mol/L;
(2) electrodeposition of polyfluoro-functionalized polybenzazole films
Placing the prepared electrochemical solution into an electrochemical reaction device, wherein the electrochemical reaction device adopts a three-electrode system (1 × 2 cm)2The ITO conductive glass is used as a working electrode, and the area is 1.5 × 3cm2The platinum sheet is used as a counter electrode and Ag/AgCl with the diameter of 1mm is used as a reference electrode), nitrogen is introduced into the solution for 30min to remove dissolved oxygen in the solution, a potentiostatic method is adopted, the polymerization potential of the potentiostatic method is 1.55V, and the polymerization electric quantity is controlled within the range of 28-30mC/cm2Meanwhile, a (4, 6, 7-tris (trifluoroethyl) indole) thin film is electrodeposited on the working electrode.
The foregoing is merely exemplary and illustrative of the present invention and various modifications, additions and substitutions may be made by those skilled in the art to the specific embodiments described without departing from the scope of the present invention as defined in the accompanying claims.
Claims (5)
1. The polyfluoro functional polybenzazole electrode material applied to the supercapacitor is characterized in that a precursor structure of the polybenzazole electrode material is substituted at 4, 5, 6 or 7 sites of indole molecules, the number of substitution is 1, 2, 3 and 4 respectively, and the molecular structure is shown as the following formula:
wherein said R1Is trifluoromethyl or trifluoroethyl, the R2Is fluorine atom, trifluoromethyl or trifluoroethyl.
2. The preparation method of the polyfluoro functionalized polybenzazole electrode material applied to the supercapacitor, which is disclosed by the claim 1, is characterized by comprising the following steps:
(1) electrochemical solution formulation
Dissolving a polymer precursor in an organic solvent under the nitrogen atmosphere, and adding a supporting electrolyte into the organic solvent to obtain an electrochemical solution;
(2) electrodeposition of polyfluoro-functionalized polybenzazole films
And (2) placing the prepared electrochemical solution into an electrochemical reaction device, wherein the electrochemical reaction device adopts a three-electrode system (a working electrode, a reference electrode and a counter electrode), introducing nitrogen into the solution to remove dissolved oxygen in the solution, and electrodepositing the polyfluoro functional polybenzazole film on the working electrode by adopting a potentiostatic method or a continuous cyclic voltammetry method.
3. The method for preparing the polyfluoro functionalized polybenzazole electrode material for the supercapacitor according to claim 2, wherein the organic solvent is any one of acetonitrile and dichloromethane, and the supporting electrolyte is any one of tetrabutylammonium perchlorate, tetrabutylammonium hexafluorophosphate and tetrabutylammonium tetrafluoroborate.
4. The method for preparing the polyfluoro functionalized polybenzazole electrode material for the supercapacitor according to claim 2, wherein the concentration of the precursor in the electrochemical solution is 0.05-0.08mol/L, and the solubility of the supporting electrolyte is 0.1 mol/L.
5. The preparation method of the polyfluoro functionalized polybenzazole electrode material applied to the supercapacitor according to claim 2, wherein the potentiostatic polymerization potential is 1.40-1.55V, and the polymerization electric quantity is controlled within a range of 28-30mC/cm2In the meantime.
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