CN111768978A - Preparation method of graphene and polyaniline composite fiber electrode material - Google Patents
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- H—ELECTRICITY
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- 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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- 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
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- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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
- H01G11/40—Fibres
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- 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
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- 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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- 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
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Abstract
The invention discloses a preparation method of a graphene and polyaniline composite fiber electrode material. The method comprises the following steps: (1) washing polyaniline with deionized water, and air drying to obtain product A; (2) adding the product A into an organic solvent, performing ultrasonic dispersion, and magnetically stirring to obtain a product B; (3) adding graphene oxide into the product B, performing ultrasonic dispersion at the temperature of-3-5 ℃, and then dropwise adding deionized water under the condition of magnetic stirring to obtain graphene oxide and polyaniline composite gel, namely a product C; (4) and preparing the product C into a fibrous electrode material, and carrying out chemical reduction or thermal reduction and vacuum drying to obtain the fibrous electrode material. The method solves the problems that polyaniline is easy to agglomerate and graphene sheets are easy to compactly stack in the process of compounding polyaniline and graphene, greatly improves the electrochemical performance of the electrode material, and has the advantages of simple and easy operation, low cost and easy large-scale preparation.
Description
Technical Field
The invention relates to a preparation method of a composite electrode material, in particular to a preparation method of a graphene and polyaniline composite fiber electrode material.
Background
With the gradual decrease of fossil fuels, people are urgently required to find new energy sources capable of replacing the fossil fuels. In the process of utilizing new energy, energy storage and conversion become very important, and energy storage devices such as super capacitors and batteries have been widely researched by scientists. For an energy storage device, the storage of ions by an electrode material and the influence of conductivity on the performance of the energy storage device are large, graphene becomes one of the most potential materials of the energy storage material due to the huge specific surface area and high conductivity of graphene, but the theoretical specific capacitance of graphene is low (550F g)-1) And the strong pi-pi interaction between the sheets makes the sheets easy to be seriously stacked, reduces the contact area of electrolyte ions and the surface of the graphene, reduces the capacitance of a double electric layer, and limits the exertion of the theoretical specific capacitance of the graphene. Polyaniline is a conductive polymer with unique electrochemical activity, strong chemical stability, low cost and simple preparation method, and the theoretical specific capacitance value of the polyaniline is as high as 1284Fg-1And the synthesis condition is easy to control, and the microstructure is adjustable, so the polyaniline is widely concerned, however, the polyaniline is easy to agglomerate in the electrochemical charge and discharge process, so that the electrochemical performance is reduced. Therefore, researchers often compound graphene and polyaniline to integrate the excellent physicochemical properties of graphene and polyaniline, and meanwhile, the graphene material is used as a support framework of polyaniline to prevent the polyaniline from agglomerating, and the polyaniline is used as a barrier between graphene sheets to avoid dense stacking of the graphene sheets. In recent years, research on graphene and polyaniline electrode materials involves various preparation methods, which can be broadly summarized as electrochemical polymerization, interfacial polymerization, in-situ composite, physical mixing, and the like. However, in these methods, polyaniline is generally retained on the surface of the graphene sheet layer, and it is difficult to uniformly disperse polyaniline in the graphene-based material, and thus it is difficult to sufficiently exhibit the excellent properties of polyaniline and graphene. In the invention, the method of the cosolvent is adopted, so that the graphene and the polyaniline can be uniformly compounded,finally, the graphene and polyaniline composite fiber electrode material with excellent electrochemical performance is obtained.
Disclosure of Invention
The invention aims to provide a preparation method of a graphene and polyaniline composite fiber electrode material. The method solves the problems that polyaniline is easy to agglomerate and graphene sheets are easy to compactly stack in the process of compounding polyaniline and graphene, greatly improves the electrochemical performance of the electrode material, and has the characteristics of simple and easy operation, low cost and easy large-scale preparation.
The technical scheme of the invention is as follows: a preparation method of a graphene and polyaniline composite fiber electrode material comprises the following steps:
(1) washing polyaniline with deionized water, and air drying to obtain product A;
(2) adding the product A into an organic solvent, performing ultrasonic dispersion, and magnetically stirring to obtain a product B;
(3) adding graphene oxide into the product B, performing ultrasonic dispersion at the temperature of-3-5 ℃, and then dropwise adding deionized water under the condition of magnetic stirring to obtain graphene oxide and polyaniline composite gel, namely a product C;
(4) and preparing the product C into a fibrous electrode material, namely a product D, and carrying out chemical reduction or thermal reduction and vacuum drying to obtain the electrode material.
In the preparation method of the graphene and polyaniline composite fiber electrode material, in the step (1), polyaniline is prepared by a rapid polymerization method.
In the preparation method of the graphene and polyaniline composite fiber electrode material, in the step (2), 0.006-0.03 g A product is added into 10mL of organic solvent according to the proportion; the organic solvent is N, N-dimethylformamide or N-methylpyrrolidone.
In the preparation method of the graphene and polyaniline composite fiber electrode material, in the step (2), ultrasonic dispersion is performed for 20-60 min, and magnetic stirring is performed for 20-40 min.
In the preparation method of the graphene and polyaniline composite fiber electrode material, in the step (3), the mass ratio of graphene oxide, polyaniline and deionized water in the product C is 20-100: 1: 1000 to 3000.
In the preparation method of the graphene and polyaniline composite fiber electrode material, in the step (3), ultrasonic dispersion is performed for 1-2 hours at the temperature of-3-5 ℃.
In the preparation method of the graphene and polyaniline composite fiber electrode material, in the step (4), the electrode material is fibrous.
In the preparation method of the graphene and polyaniline composite fiber electrode material, in the step (4), the chemical reduction is hydroiodic acid reduction and hydrazine hydrate reduction; the hydriodic acid reduction is to add hydriodic acid into the product D, reduce for 0.4 to 0.6 hours at the temperature of 15 to 25 ℃ and reduce for 1.3 to 1.7 hours at the temperature of 70 to 90 ℃; the hydrazine hydrate reduction is carried out for 22-26 hours under hydrazine hydrate steam; the thermal reduction is carried out for 5-7 hours at 140-160 ℃.
In the preparation method of the graphene and polyaniline composite fiber electrode material, in the step (4), the vacuum drying temperature is 50-70 ℃, and the drying time is 22-26 h.
In the preparation method of the graphene and polyaniline composite fiber electrode material, gel formed by polyvinyl alcohol and sulfuric acid is used as electrolyte to assemble the supercapacitor.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts the organic solvent to disperse the prepared polyaniline, and in the process of magnetic stirring, under the action of shearing force and hydrogen bonds of the organic solvent and the polyaniline, the fibrous polyaniline generates a process of nucleation and growth to form the nano needle-shaped polyaniline.
2. Specifically, the method comprises the steps of firstly obtaining fibrous polyaniline by adopting a rapid polymerization method, dispersing the obtained polyaniline in an organic solvent to enable the polyaniline and the organic solvent to generate hydrogen bond interaction, then compounding the polyaniline and graphene oxide to form a graphene oxide and polyaniline composite, obtaining the graphene oxide and polyaniline fibers by a wet spinning technology, reducing the graphene oxide and polyaniline composite fibers to obtain graphene and polyaniline composite fibers, and finally removing the organic solvent under the high-temperature vacuum condition to obtain the graphene and polyaniline composite fiber electrode with good dispersion.
Experiments prove that:
the graphene and polyaniline composite fiber electrode prepared by the method has excellent electrochemical performance. The applicant constructs a fiber type super capacitor based on the graphene and polyaniline composite fiber electrode prepared according to the embodiment, and performs performance test on the device. Table 1 shows the comparison of the electrochemical properties of the graphene and polyaniline composite fiber electrode of the present invention and other fiber electrode materials, and the results show that the electrochemical properties of the composite fiber electrode obtained by the present invention are at a higher level.
Table 1 comparison of electrochemical performance of fibrous supercapacitors based on graphene and polyaniline composite fibers of the present invention with other graphene and polyaniline composite fibrous supercapacitors
FIG. 1 is a diagram of graphene and polyaniline composite fibers prepared by the method of the present invention woven on an existing fabric, and it can be seen from FIG. 1 that the fibers obtained by the method of the present invention have good flexibility and mechanical strength capable of meeting the requirements of textile process on mechanical strength of the fibers; FIG. 2 is a scanning electron microscope image of the graphene and polyaniline composite fiber prepared by the present invention, and it can be clearly seen from FIG. 1 that the diameter of the fiber is 100 microns; fig. 3 is a scanning electron microscope image of the graphene and polyaniline composite fiber prepared by the present invention, and it can be seen from fig. 3 that acicular polyaniline is uniformly loaded on the graphene sheet layer; FIG. 4 shows a super capacitor based on graphene and polyaniline composite fiber electrodes prepared by the methodAt a sweep rate of 2mVs-2The Cyclic Voltammetry (CV) curve of time, from fig. 4, can be seen the characteristic redox peak corresponding to polyaniline, further illustrating the successful loading of polyaniline in the electrode material.
In conclusion, the method solves the problems that polyaniline is easy to agglomerate and graphene sheets are easy to compactly stack in the process of compounding polyaniline and graphene, greatly improves the electrochemical performance of the electrode material, and has the advantages of simple and easy operation, low cost and easy large-scale preparation.
Drawings
FIG. 1 is a diagram of graphene and polyaniline composite fibers prepared by the present invention woven on a conventional fabric;
FIG. 2 is a scanning electron microscope image of the graphene and polyaniline composite fiber prepared by the present invention;
FIG. 3 is a scanning electron microscope image of the graphene and polyaniline composite fiber prepared by the present invention;
FIG. 4 shows the sweep rate of a supercapacitor based on the graphene and polyaniline composite fiber electrode prepared by the method of the invention is 2mV s-2Cyclic Voltammetry (CV) profile over time.
Detailed Description
The invention is further illustrated by the following figures and examples, which are not to be construed as limiting the invention.
Example 1: a preparation method of a graphene and polyaniline composite fiber electrode material comprises the following steps:
(1) washing polyaniline with deionized water, and air drying to obtain product A; the polyaniline is prepared by a rapid polymerization method;
(2) adding 0.006g A product into 10mL of organic solvent; the organic solvent is N, N-dimethylformamide, ultrasonic dispersion is carried out for 20min, and magnetic stirring is carried out for 20 min;
(3) adding 0.6g of graphene oxide into the product B, performing ultrasonic dispersion at 5 ℃ for 2 hours, and then dropwise adding 10mL of deionized water under the condition of magnetic stirring to obtain graphene oxide and polyaniline composite gel, namely a product C;
(4) and preparing the product C into fibers by a wet spinning technology, reducing the fibers by hydroiodic acid, and drying the fibers at 50 ℃ for 26 hours in vacuum to obtain a fiber electrode material, wherein the electrode material uses gel consisting of 1M polyvinyl alcohol (PVA) and sulfuric acid as an electrolyte to construct a fiber type supercapacitor.
Example 2: a preparation method of a graphene and polyaniline composite electrode material comprises the following steps:
(1) washing polyaniline with deionized water, and air drying to obtain product A; the polyaniline is prepared by a rapid polymerization method;
(2) adding 0.012g A product into 10mL organic solvent; the organic solvent is N, N-dimethylformamide, ultrasonic dispersion is carried out for 30min, and magnetic stirring is carried out for 40 min;
(3) adding 0.6g of graphene oxide into the product B, performing ultrasonic dispersion at 5 ℃ for 1h, and then dropwise adding 10mL of deionized water under the condition of magnetic stirring to obtain graphene oxide and polyaniline composite gel, namely a product C;
(4) and preparing the product C into fibers by a wet spinning technology, reducing the fibers by hydroiodic acid, and drying the fibers for 24 hours at 60 ℃ in vacuum to obtain an electrode material, wherein the electrode material uses gel consisting of 1M polyvinyl alcohol and sulfuric acid as an electrolyte to construct a fiber type supercapacitor.
Example 3: a preparation method of a graphene and polyaniline composite fiber electrode material comprises the following steps:
(1) washing polyaniline with deionized water, and air drying to obtain product A; the polyaniline is prepared by a rapid polymerization method;
(2) adding 0.03g A product into 10mL of organic solvent; the organic solvent is N, N-dimethylformamide, ultrasonic dispersion is carried out for 30min, and magnetic stirring is carried out for 40 min;
(3) adding 0.6g of graphene oxide into the product B, performing ultrasonic dispersion for 2 hours at the temperature of-3 ℃, and then dropwise adding 10mL of deionized water under the condition of magnetic stirring to obtain graphene oxide and polyaniline composite gel, namely a product C;
(4) and preparing the product C into fibers by a wet spinning technology, reducing the fibers by hydroiodic acid, and drying the fibers at 70 ℃ for 22 hours in vacuum to obtain an electrode material, wherein the electrode material uses gel consisting of 1M polyvinyl alcohol and sulfuric acid as an electrolyte to construct a fiber type supercapacitor.
Example 4: a preparation method of a graphene and polyaniline composite electrode material comprises the following steps:
(1) washing polyaniline with deionized water, and air drying to obtain product A; the polyaniline is prepared by a rapid polymerization method;
(2) adding 0.012g A product into 10mL organic solvent; the organic solvent is N, N-dimethyl pyrrolidone, ultrasonic dispersion is carried out for 40min, and magnetic stirring is carried out for 30 min;
(3) adding 0.6g of graphene oxide into the product B, performing ultrasonic dispersion at 0 ℃ for 1h, and then dropwise adding 10mL of deionized water under the condition of magnetic stirring to obtain graphene oxide and polyaniline composite gel, namely a product C;
(4) and preparing the product C into fibers by a wet spinning technology, reducing the fibers by hydroiodic acid, and drying the fibers for 24 hours at 60 ℃ in vacuum to obtain an electrode material, wherein the electrode material uses gel consisting of 1M polyvinyl alcohol and sulfuric acid as an electrolyte to construct a fiber type supercapacitor.
Example 5: a preparation method of a graphene and polyaniline composite fiber electrode material comprises the following steps:
(1) washing polyaniline with deionized water, and air drying to obtain product A; the polyaniline is prepared by a rapid polymerization method;
(2) adding 0.018g A product into 10mL of organic solvent; the organic solvent is N, N-dimethylformamide, ultrasonic dispersion is carried out for 50min, and magnetic stirring is carried out for 30 min;
(3) adding 0.6g of graphene oxide into the product B, performing ultrasonic dispersion for 1h at the temperature of-3 ℃, and then dropwise adding 20mL of deionized water under the condition of magnetic stirring to obtain graphene oxide and polyaniline composite gel, namely a product C;
(4) and preparing the product C into fibers by a wet spinning technology, reducing the fibers by hydrazine hydrate, drying the fibers for 26 hours in a vacuum drying oven at the temperature of 60 ℃ to obtain an electrode material, and constructing the fiber type supercapacitor by using gel consisting of 1M polyvinyl alcohol and sulfuric acid as an electrolyte for the electrode material.
Example 6: a preparation method of a graphene and polyaniline composite fiber electrode material comprises the following steps:
(1) washing polyaniline with deionized water, and air drying to obtain product A; the polyaniline is prepared by a rapid polymerization method;
(2) adding 0.018g A product into 10mL of organic solvent; the organic solvent is N, N-dimethylformamide, ultrasonic dispersion is carried out for 60min, and magnetic stirring is carried out for 40 min;
(3) adding 0.6g of graphene oxide into the product B, performing ultrasonic dispersion at 3 ℃ for 1h, and then dropwise adding 20mL of deionized water under the condition of magnetic stirring to obtain graphene oxide and polyaniline composite gel, namely a product C;
(4) and preparing the product C into fibers by a wet spinning technology, carrying out thermal reduction on the fibers, reducing the fibers in a hydrothermal kettle for 6 hours at the temperature of 150 ℃, drying the fibers in a vacuum drying oven for 24 hours at the temperature of 60 ℃ to obtain an electrode material, and constructing the fiber type supercapacitor by using the gel consisting of 1M of polyvinyl alcohol and sulfuric acid as an electrolyte for the electrode material.
Claims (10)
1. A preparation method of a graphene and polyaniline composite fiber electrode material is characterized by comprising the following steps: the method comprises the following steps:
(1) washing polyaniline with deionized water, and air drying to obtain product A;
(2) adding the product A into an organic solvent, performing ultrasonic dispersion, and magnetically stirring to obtain a product B;
(3) adding graphene oxide into the product B, performing ultrasonic dispersion at the temperature of-3-5 ℃, and then dropwise adding deionized water under the condition of magnetic stirring to obtain graphene oxide and polyaniline composite gel, namely a product C;
(4) and preparing the product C into a fibrous electrode material, namely a product D, and carrying out chemical reduction or thermal reduction and vacuum drying to obtain the electrode material.
2. The preparation method of the graphene and polyaniline composite fiber electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (1), polyaniline is prepared by a rapid polymerization method.
3. The preparation method of the graphene and polyaniline composite fiber electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (2), 0.006-0.03 g A product is added into 10mL of organic solvent according to the proportion; the organic solvent is N, N-dimethylformamide or N-methylpyrrolidone.
4. The preparation method of the graphene and polyaniline composite fiber electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (2), ultrasonic dispersion is carried out for 20-60 min, and magnetic stirring is carried out for 20-40 min.
5. The preparation method of the graphene and polyaniline composite fiber electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (3), the mass ratio of the graphene oxide, the polyaniline and the deionized water in the product C is 20-100: 1: 1000 to 3000.
6. The preparation method of the graphene and polyaniline composite fiber electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (3), ultrasonic dispersion is carried out for 1-2 h at the temperature of-3-5 ℃.
7. The preparation method of the graphene and polyaniline composite fiber electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (4), the electrode material is fibrous.
8. The preparation method of the graphene and polyaniline composite fiber electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (4), the chemical reduction is hydroiodic acid reduction and hydrazine hydrate reduction; the hydriodic acid reduction is to add hydriodic acid into the product D, reduce for 0.4 to 0.6 hours at the temperature of 15 to 25 ℃ and reduce for 1.3 to 1.7 hours at the temperature of 70 to 90 ℃; the hydrazine hydrate reduction is carried out for 22-26 hours under hydrazine hydrate steam; the thermal reduction is carried out for 5-7 hours at 140-160 ℃.
9. The preparation method of the graphene and polyaniline composite fiber electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: in the step (4), the temperature of vacuum drying is 50-70 ℃, and the drying time is 22-26 h.
10. The preparation method of the graphene and polyaniline composite fiber electrode material as claimed in claim 1, wherein the preparation method comprises the following steps: the graphene and polyaniline composite fiber electrode material is formed by assembling a super capacitor by taking gel consisting of polyvinyl alcohol and sulfuric acid as electrolyte.
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| CN113539697A (en) * | 2021-05-28 | 2021-10-22 | 武汉工程大学 | Reduced graphene oxide/conductive polymer composite gel and preparation method thereof |
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| JP2014093412A (en) * | 2012-11-02 | 2014-05-19 | Yokohama Rubber Co Ltd:The | Polyaniline/graphene complex, and electrode material using the same |
| CN105810455A (en) * | 2016-04-21 | 2016-07-27 | 贵州大学 | Method for preparing graphene/polyaniline composite film electrode |
| CN106012086A (en) * | 2016-07-02 | 2016-10-12 | 苏州大学 | Graphene/polyaniline composite fiber and preparation method thereof |
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| JP2014093412A (en) * | 2012-11-02 | 2014-05-19 | Yokohama Rubber Co Ltd:The | Polyaniline/graphene complex, and electrode material using the same |
| CN105810455A (en) * | 2016-04-21 | 2016-07-27 | 贵州大学 | Method for preparing graphene/polyaniline composite film electrode |
| CN106012086A (en) * | 2016-07-02 | 2016-10-12 | 苏州大学 | Graphene/polyaniline composite fiber and preparation method thereof |
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| CN113539697A (en) * | 2021-05-28 | 2021-10-22 | 武汉工程大学 | Reduced graphene oxide/conductive polymer composite gel and preparation method thereof |
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