CN112201486A - Preparation method of poly (3, 4-ethylenedioxythiophene)/graphite felt flexible electrode material - Google Patents
Preparation method of poly (3, 4-ethylenedioxythiophene)/graphite felt flexible electrode material Download PDFInfo
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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
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Abstract
The invention discloses a preparation method of a poly (3, 4-ethylenedioxythiophene)/graphite felt flexible electrode material, and belongs to the technical field of preparation of electrode materials for supercapacitors. The electrode material is prepared by polymerizing 3, 4-ethylenedioxythiophene serving as a monomer, sodium dodecyl sulfate serving as a surfactant, orange II serving as a dopant and ammonium persulfate serving as an oxidant on a graphite felt by a chemical oxidation method. The electrode material prepared by the invention has higher specific capacitance and excellent cycle stability, is mainly used for manufacturing flexible electrodes of supercapacitors, and has obvious economic value and social benefit.
Description
Technical Field
The invention belongs to the technical field of preparation of electrode materials for a super capacitor, and particularly relates to a preparation method of a poly (3, 4-ethylenedioxythiophene)/graphite felt flexible electrode material.
Background
The conductive polymer flexible electrode material has the performance advantages of good flexibility, high charging and discharging speed, environmental friendliness, high safety, low cost and the like, and has an important application value in the field of wearable electronic equipment. Among a plurality of conductive polymer flexible electrode materials, the poly 3, 4-ethylenedioxythiophene flexible electrode material has the advantages of high conductivity, good high-temperature stability, low oxidation potential, electrochemical stability and the like, and is an ideal flexible electrode material for the super capacitor. However, the poly 3, 4-ethylenedioxythiophene has strong rigidity of conjugated molecular chains and poor mechanical property; the monomer has low solubility in water and is easy to agglomerate during polymerization; the commercial application of the poly 3, 4-ethylenedioxythiophene flexible electrode material is limited due to the defects of high relative molecular mass, low theoretical specific capacitance and the like. Chinese patent CN110797210A discloses a preparation method of a poly 3, 4-ethylenedioxythiophene flexible electrode material, which is prepared by immersing pretreated cotton threads into 3, 4-ethylenedioxythiophene, then immersing into a hydrochloric acid aqueous solution of ammonium persulfate, and carrying out chemical oxidation. The test result shows that the specific capacitance of the electrode material is 255F/g under the current density of 0.2A/g, and the specific capacitance retention rate after 2000 cycles is 92%. Compared with the cotton fiber flexible matrix with low conductivity, no high temperature resistance and no acid and alkali resistance, the graphite felt not only has the characteristics of high temperature resistance, corrosion resistance, no melting, large void ratio (90 percent), good conductivity, elasticity and the like, but also can be folded and cut at will. The graphite felt is used as a substrate of the flexible electrode material, and the conductive polymer is polymerized on the graphite felt, so that the conductivity, specific capacitance and circulation stability of the conductive polymer flexible electrode material can be improved, and the conductive polymer flexible electrode material has excellent mechanical properties.
Disclosure of Invention
Aiming at the problems of low conductivity, high temperature resistance, poor acid and alkali resistance and the like of a cotton thread matrix of the conventional poly 3, 4-ethylenedioxythiophene flexible electrode material, the invention provides a preparation method of a poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material. The electrode material prepared by the invention has higher specific capacitance and excellent cycle stability, is mainly used for manufacturing flexible electrodes of supercapacitors, and has obvious economic value and social benefit.
In order to achieve the purpose, the invention adopts the following technical scheme:
the poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material is prepared by polymerizing 3, 4-ethylenedioxythiophene serving as a monomer, sodium dodecyl sulfate serving as a surfactant, orange II serving as a dopant and ammonium persulfate serving as an oxidant on a graphite felt by a chemical oxidation method.
The preparation method of the poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material specifically comprises the following steps:
(1) adding 1.5-2.5 g of sodium dodecyl sulfate into 50-100 mL of deionized water, magnetically stirring at room temperature for 10-20 min, adding 0.2-0.3 g of 3, 4-ethylenedioxythiophene, magnetically stirring at room temperature for 30-60 min, finally adding 0.2-0.35 g of orange II, and magnetically stirring at room temperature for 20-40 min to obtain a mixed solution of the orange II and the 3, 4-ethylenedioxythiophene.
(2) Immersing a graphite felt sample strip into the mixed solution prepared in the step (1), adding 15-25 mL of ammonium persulfate hydrochloric acid solution into the mixed solution, and magnetically stirring at room temperature for 4-24 hours; taking out the graphite felt sample strip, soaking the graphite felt sample strip in methanol for 5-10 h, then soaking the graphite felt sample strip in 1 mol/L ammonia water for 24-48 h, finally soaking the graphite felt sample strip in 1 mol/L hydrochloric acid for 1-3 h, alternately washing the graphite felt sample strip with methanol and deionized water until filtrate is colorless, and performing vacuum drying at 60 ℃ for 24 h to prepare the orange II doped poly 3, 4-ethylenedioxythiophene/graphite felt composite material, namely the poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material.
In the hydrochloric acid solution of the ammonium persulfate in the step (2), the concentration of the ammonium persulfate is 0.3 mol/L, and the concentration of the hydrochloric acid is 1 mol/L.
The invention has the following remarkable advantages:
(1) the sodium dodecyl sulfate can be used as a surfactant to improve the solubility of the 3, 4-ethylenedioxythiophene in water, so that the sodium dodecyl sulfate is beneficial to improving the polymerization speed of the poly-3, 4-ethylenedioxythiophene on the graphite felt. Meanwhile, the sodium dodecyl sulfate is also beneficial to the poly (3, 4-ethylenedioxythiophene) on the surface of the graphite felt fiber to present a loose porous structure, and the contact area of the active substance and the electrolyte is increased, so that the specific capacitance of the electrode material is improved.
(2) The orange II serving as a dopant has a large pi-conjugated molecular structure, can improve the pi-conjugated degree of a poly (3, 4-ethylenedioxythiophene) molecular chain, can contribute to partial pseudocapacitance, and achieves the purpose of improving the specific capacitance of an electrode material. Meanwhile, the orange II molecules with larger molecular size can also play a role of a pore-foaming agent, and are beneficial to the poly (3, 4-ethylenedioxythiophene) on the surface of the graphite felt fiber to present a loose porous structure.
(3) The graphite felt fiber is used as a supporting material, so that the cycling stability of the electrode material can be improved. A large amount of pi conjugated electrons on the graphite felt fiber can promote the electron transmission of the orange II doped poly 3, 4-ethylenedioxythiophene, and the specific capacitance of the electrode material is improved. In addition, the graphite felt is used as a substrate material of the electrode, and can also endow the electrode material with excellent mechanical properties.
(4) The poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material prepared by the invention has higher specific capacitance and excellent cycling stability, when the charging and discharging current densities are 1A/g, 2A/g, 4A/g and 8A/g respectively, the specific capacitances are 385F/g, 279F/g, 246F/g and 208F/g respectively, after 2000 cycles, the specific capacitance reaches 99.2%, and the poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material is mainly used for manufacturing flexible electrodes of supercapacitors and has obvious economic value and social benefit.
Drawings
FIG. 1 is an infrared absorption spectrum of the orange II doped poly (3, 4-ethylenedioxythiophene)/graphite felt composite material prepared in example 1;
FIG. 2 is a scanning electron micrograph of the orange II doped poly (3, 4-ethylenedioxythiophene)/graphite felt composite material prepared in example 1;
FIG. 3 is a scanning electron micrograph of the poly (3, 4-ethylenedioxythiophene)/graphite felt composite prepared in comparative example 1;
FIG. 4 is a scanning electron micrograph of orange II doped poly (3, 4-ethylenedioxythiophene) prepared in comparative example 2;
FIG. 5 is a scanning electron micrograph of poly-3, 4-ethylenedioxythiophene prepared in comparative example 3.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
(1) Adding 2 g of sodium dodecyl sulfate into 80 mL of deionized water, magnetically stirring at room temperature for 15 min, adding 0.25 g of 3, 4-ethylenedioxythiophene, magnetically stirring at room temperature for 45 min, finally adding 0.3 g of orange II, and magnetically stirring at room temperature for 30 min to obtain a mixed solution of the orange II and the 3, 4-ethylenedioxythiophene.
(2) Immersing a graphite felt sample strip into the mixed solution prepared in the step (1), adding 20 mL of ammonium persulfate hydrochloric acid solution into the mixed solution, and magnetically stirring for 14 h at room temperature; taking out the graphite felt sample strip, soaking the graphite felt sample strip in methanol for 8 hours, then soaking the graphite felt sample strip in 1 mol/L ammonia water for 36 hours, finally soaking the graphite felt sample strip in 1 mol/L hydrochloric acid for 2 hours, alternately washing the graphite felt sample strip with methanol and deionized water until the filtrate is colorless, and drying the filtrate in vacuum at 60 ℃ for 24 hours to prepare the orange II doped poly 3, 4-ethylenedioxythiophene/graphite felt composite material, namely the poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material.
In the hydrochloric acid solution of the ammonium persulfate in the step (2), the concentration of the ammonium persulfate is 0.3 mol/L, and the concentration of the hydrochloric acid is 1 mol/L.
FIG. 1 is an infrared absorption spectrum of the orange II doped poly (3, 4-ethylenedioxythiophene)/graphite felt composite prepared in example 1. As can be seen in the figure, it is located at 1139 cm-1And 974 cm-1The absorption peaks are respectively the stretching vibration absorption peaks of C-O-C and C-S on the thiophene ring of the poly 3, 4-ethylenedioxythiophene and are positioned at 1088 cm-1And 622 cm-1The absorption peak is-SO of orange II3 -The characteristic absorption peak of the yellow orange II doped poly 3, 4-ethylenedioxythiaThe thiophene/graphite felt composite was successfully prepared.
FIG. 2 is a scanning electron micrograph of the orange II doped poly (3, 4-ethylenedioxythiophene)/graphite felt composite material prepared in example 1. As can be seen from the figure, the poly 3, 4-ethylenedioxythiophene on the surface of the graphite felt fiber has a loose porous structure, and the calculation result of BET shows that the pore size is relatively uniform, which is beneficial to increasing the contact area of an active substance and an electrolyte, thereby improving the specific capacitance of an electrode material.
Example 2
(1) Adding 1.5 g of sodium dodecyl sulfate into 50 mL of deionized water, magnetically stirring at room temperature for 10 min, adding 0.2 g of 3, 4-ethylenedioxythiophene, magnetically stirring at room temperature for 30 min, finally adding 0.2 g of orange II, and magnetically stirring at room temperature for 20 min to obtain a mixed solution of the orange II and the 3, 4-ethylenedioxythiophene.
(2) Immersing a graphite felt sample strip into the mixed solution prepared in the step (1), adding 15 mL of ammonium persulfate hydrochloric acid solution into the mixed solution, and magnetically stirring for 4 hours at room temperature; taking out the graphite felt sample strip, soaking the graphite felt sample strip in methanol for 5 h, then soaking the graphite felt sample strip in 1 mol/L ammonia water for 24 h, finally soaking the graphite felt sample strip in 1 mol/L hydrochloric acid for 1 h, alternately washing the graphite felt sample strip with methanol and deionized water until the filtrate is colorless, and drying the filtrate in vacuum at 60 ℃ for 24 h to prepare the orange II doped poly 3, 4-ethylenedioxythiophene/graphite felt composite material, namely the poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material.
In the hydrochloric acid solution of the ammonium persulfate in the step (2), the concentration of the ammonium persulfate is 0.3 mol/L, and the concentration of the hydrochloric acid is 1 mol/L.
Example 3
(1) Adding 2.5 g of sodium dodecyl sulfate into 100 mL of deionized water, magnetically stirring at room temperature for 20 min, adding 0.3 g of 3, 4-ethylenedioxythiophene, magnetically stirring at room temperature for 60 min, finally adding 0.35 g of orange II, and magnetically stirring at room temperature for 40 min to obtain a mixed solution of the orange II and the 3, 4-ethylenedioxythiophene.
(2) Immersing a graphite felt sample strip into the mixed solution prepared in the step (1), adding 25 mL of ammonium persulfate hydrochloric acid solution into the mixed solution, and magnetically stirring for 24 hours at room temperature; taking out the graphite felt sample strip, soaking the graphite felt sample strip in methanol for 10 h, then soaking the graphite felt sample strip in 1 mol/L ammonia water for 48 h, finally soaking the graphite felt sample strip in 1 mol/L hydrochloric acid for 3 h, alternately washing the graphite felt sample strip with methanol and deionized water until the filtrate is colorless, and drying the filtrate in vacuum at 60 ℃ for 24 h to prepare the orange II doped poly 3, 4-ethylenedioxythiophene/graphite felt composite material, namely the poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material.
In the hydrochloric acid solution of the ammonium persulfate in the step (2), the concentration of the ammonium persulfate is 0.3 mol/L, and the concentration of the hydrochloric acid is 1 mol/L.
Comparative example 1
(1) Adding 2 g of sodium dodecyl sulfate into 80 mL of deionized water, magnetically stirring at room temperature for 15 min, adding 0.25 g of 3, 4-ethylenedioxythiophene, and magnetically stirring at room temperature for 45 min to obtain a 3, 4-ethylenedioxythiophene solution.
(2) Immersing a graphite felt sample strip into the solution prepared in the step (1), adding 20 mL of ammonium persulfate hydrochloric acid solution into the mixed solution, and magnetically stirring for 14 h at room temperature; taking out the graphite felt sample strip, soaking the graphite felt sample strip in methanol for 8 hours, then soaking the graphite felt sample strip in 1 mol/L ammonia water for 36 hours, finally soaking the graphite felt sample strip in 1 mol/L hydrochloric acid for 2 hours, alternately washing the graphite felt sample strip with methanol and deionized water until the filtrate is colorless, and drying the graphite felt sample strip in vacuum at 60 ℃ for 24 hours to obtain the poly (3, 4-ethylenedioxythiophene)/graphite felt composite material.
In the hydrochloric acid solution of the ammonium persulfate in the step (2), the concentration of the ammonium persulfate is 0.3 mol/L, and the concentration of the hydrochloric acid is 1 mol/L.
FIG. 3 is a scanning electron micrograph of the poly (3, 4-ethylenedioxythiophene)/graphite felt composite material prepared in comparative example 1. As can be seen from the figure, the poly 3, 4-ethylenedioxythiophene on the surface of the graphite felt fiber still has a porous structure, and the calculation result of BET shows that the pore size is not uniform enough.
Comparative example 2
(1) Adding 2 g of sodium dodecyl sulfate into 80 mL of deionized water, magnetically stirring at room temperature for 15 min, adding 0.25 g of 3, 4-ethylenedioxythiophene, magnetically stirring at room temperature for 45 min, finally adding 0.3 g of orange II, and magnetically stirring at room temperature for 30 min to obtain a mixed solution of the orange II and the 3, 4-ethylenedioxythiophene.
(2) Adding 20 mL of hydrochloric acid solution of ammonium persulfate into the mixed solution prepared in the step (1), magnetically stirring for 14 h at room temperature, and filtering; soaking the product in methanol for 8 h, then soaking in 1 mol/L ammonia water for 36 h, finally soaking in 1 mol/L hydrochloric acid for 2 h, alternately washing with methanol and deionized water until the filtrate is colorless, and vacuum drying at 60 ℃ for 24 h to obtain the orange II doped poly 3, 4-ethylenedioxythiophene.
In the hydrochloric acid solution of the ammonium persulfate in the step (2), the concentration of the ammonium persulfate is 0.3 mol/L, and the concentration of the hydrochloric acid is 1 mol/L.
FIG. 4 is a scanning electron micrograph of orange II doped poly (3, 4-ethylenedioxythiophene) prepared in comparative example 2. As can be seen from the figure, the orange II doped poly 3, 4-ethylenedioxythiophene is in a porous block structure, and the BET calculation result shows that the pore size is not uniform enough.
Comparative example 3
(1) Adding 2 g of sodium dodecyl sulfate into 80 mL of deionized water, magnetically stirring at room temperature for 15 min, adding 0.25 g of 3, 4-ethylenedioxythiophene, and magnetically stirring at room temperature for 45 min to obtain a 3, 4-ethylenedioxythiophene solution.
(2) Adding 20 mL of hydrochloric acid solution of ammonium persulfate into the solution prepared in the step (1), magnetically stirring for 14 h at room temperature, and filtering; soaking the product in methanol for 8 h, then soaking in 1 mol/L ammonia water for 36 h, finally soaking in 1 mol/L hydrochloric acid for 2 h, alternately washing with methanol and deionized water until the filtrate is colorless, and vacuum drying at 60 ℃ for 24 h to obtain the poly-3, 4-ethylenedioxythiophene.
In the hydrochloric acid solution of the ammonium persulfate in the step (2), the concentration of the ammonium persulfate is 0.3 mol/L, and the concentration of the hydrochloric acid is 1 mol/L.
FIG. 5 is a scanning electron micrograph of poly-3, 4-ethylenedioxythiophene prepared in comparative example 3. As can be seen from the figure, poly 3, 4-ethylenedioxythiophene has a coarse blocky structure, and BET calculation results show that the pore size is not uniform.
The method comprises the steps of taking a product wrapped by graphite paper as a working electrode, taking a platinum sheet as a counter electrode, taking a saturated calomel electrode as a reference electrode, taking 1 mol/L sulfuric acid aqueous solution as electrolyte, testing the specific capacitance of the products prepared in the examples and the comparative examples by using a constant current charging and discharging method, and testing the cyclic stability of the products prepared in the examples and the comparative examples by using a cyclic voltammetry method, wherein the voltage range is-0.2V-0.8V, the charging and discharging current densities are 1A/g, 2A/g, 4A/g and 8A/g respectively, and the scanning rate is 100 mV/s. The pore size distribution was calculated by the Barrett-Joyner-Halenda (BJH) method. The electrochemical performance test results and pore size distribution of the three groups of examples and the three groups of comparative examples are shown in table 1.
TABLE 1 test results
From the test results of the three groups of examples and the three groups of comparative examples, it can be seen that the poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material prepared by using a chemical oxidation method has higher specific capacitance and excellent cycling stability, wherein the poly 3, 4-ethylenedioxythiophene is used as a monomer, the sodium dodecyl sulfate is used as a surfactant, the orange II is used as a doping agent, and the ammonium persulfate is used as an oxidizing agent.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (2)
1. A preparation method of a poly (3, 4-ethylenedioxythiophene)/graphite felt flexible electrode material is characterized by comprising the following steps: the electrode material is formed by polymerizing 3, 4-ethylenedioxythiophene serving as a monomer, sodium dodecyl sulfate serving as a surfactant, orange II serving as a dopant and ammonium persulfate serving as an oxidant on a graphite felt by a chemical oxidation method; the preparation method comprises the following steps:
(1) adding 1.5-2.5 g of sodium dodecyl sulfate into 50-100 mL of deionized water, magnetically stirring at room temperature for 10-20 min, adding 0.2-0.3 g of 3, 4-ethylenedioxythiophene, magnetically stirring at room temperature for 30-60 min, finally adding 0.2-0.35 g of orange II, and magnetically stirring at room temperature for 20-40 min to prepare a mixed solution of the orange II and the 3, 4-ethylenedioxythiophene;
(2) immersing a graphite felt sample strip into the mixed solution prepared in the step (1), adding 15-25 mL of ammonium persulfate hydrochloric acid solution into the mixed solution, and magnetically stirring at room temperature for 4-24 hours; taking out the graphite felt sample strip, soaking the graphite felt sample strip in methanol for 5-10 h, then soaking the graphite felt sample strip in 1 mol/L ammonia water for 24-48 h, finally soaking the graphite felt sample strip in 1 mol/L hydrochloric acid for 1-3 h, alternately washing the graphite felt sample strip with methanol and deionized water until filtrate is colorless, and performing vacuum drying at 60 ℃ for 24 h to prepare the orange II doped poly 3, 4-ethylenedioxythiophene/graphite felt composite material, namely the poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material.
2. The preparation method of the poly 3, 4-ethylenedioxythiophene/graphite felt flexible electrode material according to claim 1, wherein the preparation method comprises the following steps: in the hydrochloric acid solution of the ammonium persulfate in the step (2), the concentration of the ammonium persulfate is 0.3 mol/L, and the concentration of the hydrochloric acid is 1 mol/L.
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