CN1760226A - Method for preparing composite conductive high molecular electrode material in use for super capacitor - Google Patents
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Abstract
An electrically conductive composite high-molecular electrode material used for super capacitor is prepared through using pyrrole monomer to form polypyrrole on working electrode. It features the synergestic effect between polypyrrole and the polymer of phenylamine, vinyldioxy thiophene and p-phenylene, resulting in high specific capacitance (200 F/g) and wide potential window (0-1.2 V for aqueous solution and 0-3 V for organic solvent).
Description
Technical field
The present invention relates to a kind of electronic material preparation method, particularly a kind of preparation method of composite conductive high molecular electrode material in use for super capacitor.
Technical background
Ultracapacitor mainly is divided into electrostatic double layer type ultracapacitor and oxidation-reduction type ultracapacitor.Mainly by the long-pending decision of electrode material surface, its theoretical electrical capacity is directly proportional with the specific surface area of electrode materials the specific capacitance of electrostatic double layer type ultracapacitor.At present mainly be to come increasing specific surface area by the method that adopts gac or carbon nanotube to do electrode materials, its specific storage is about 50F/g～150F/g.The electrode materials of common oxidation-reduction type ultracapacitor is generally metal oxide (as RuO
2), its capacity derives from electroactive substance and at electrode surface or inside redox reaction fast takes place, and therefore has higher Faraday pseudo-capacitance in theory, but general cycle performance is relatively poor.Up to the present, the actual capacitance value of report is well below theoretical value.Conducting polymer composite then is another kind of novel oxidation-reduction type electrode material for super capacitor, and its theoretical specific capacity is higher, and (polyaniline: 750F/g), but cycle performance is relatively poor for polyethylene dioxythiophene: 210F/g, polypyrrole: 620F/g.In order to improve its cycle performance, existing researcher adopts gac or carbon nanotube modification conducting polymer composite, but this method can reduce its specific storage.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of preparation method who improves the composite conductive high molecular electrode material in use for super capacitor of specific storage when improving cycle performance is provided.
For achieving the above object, the preparation method that the present invention adopts is: the 1) preparation of A solution: at first adding halogenide, perchlorate or sulfonate in water or organic solvent, to make the concentration of halogenide, perchlorate or sulfonate be the electrolyte solution of 0.1～1mol/l, the pH of adding and the corresponding acid of ionogen or alkali adjusting electrolyte solution is 3～10 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.1～1mol/l;
3) insert stainless (steel) wire or nickel screen then in B solution and make work electrode and stainless steel tank or graphite cake and carry out electrochemical polymerization as counter electrode, the polymerization current density is 3～20mA/cm
2, polymerization time is 1～60 minute; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 60～80 ℃ of oven dry;
4) preparation of C solution: in A solution, add aniline, ethene dioxythiophene or penylene is made aniline, ethene dioxythiophene or is 0.1～1mol/l to the concentration of penylene, obtain C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 0.2～20mA/cm
2, polymerization time is 5～60 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 60～80 ℃ of oven dry.
The said organic solvent of the present invention is methyl alcohol, propylene carbonate or acetonitrile; Halogenide is lithium chloride, sodium-chlor, Repone K or etamon chloride; Perchlorate is lithium perchlorate, sodium perchlorate, potassium perchlorate or perchloric acid tetraethyl ammonium; Sulfonate is Sodium dodecylbenzene sulfonate, p-methyl benzenesulfonic acid sodium, 1-naphthalene sulfonic aicd sodium or 2-sodium naphthalene sulfonate; Acid is hydrochloric acid, perchloric acid, Witco 1298 Soft Acid, p-methyl benzenesulfonic acid, 1-naphthalene sulfonic aicd or 2-naphthene sulfonic acid; Alkali is sodium hydroxide, lithium hydroxide, potassium hydroxide or tetraethyl ammonium hydroxide.
The present invention has adopted pyrrole monomer to form polypyrrole on working electrode, has high specific volume, in addition polypyrrole (PPy) and aniline, ethene dioxythiophene, to the synergistic effect of the formed polymkeric substance of penylene, the combined electrode that makes this invention prepare has the bulking value above 200F/g, and have aniline, ethene dioxythiophene, to the distinctive wide electrochemical window of the formed polymkeric substance of penylene: 0～1.2V (at the aqueous solution) or 0～3V (at organic solvent), and when high power discharge, still have higher specific storage and cyclical stability preferably.
Description of drawings
Fig. 1 is the microscopic appearance figure of " goat's horn shape " pyrrole monomer;
Fig. 2 is that wherein X-coordinate is a cycle index according to the capacity cycle characteristics figure of the electrode materials of preparation method's preparation of the present invention, and ordinate zou is a specific storage.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
Embodiment 1:1) preparation of A solution: at first adding lithium chloride in water, to make the concentration of lithium chloride be the electrolyte solution of 0.1mol/l, and adding hydrochloric acid again in electrolyte solution, to regulate the pH of electrolyte solution be 3, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.1mol/l;
3) insert in B solution then that stainless (steel) wire is made the work electrode and stainless steel tank is done electrode is carried out electrochemical polymerization, the polymerization current density is 20mA/cm
2, polymerization time is 1 minute; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 60 ℃ of oven dry;
4) preparation of C solution: adding aniline in A solution, to make the concentration of aniline be 0.3mol/l, obtains C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 0.2mA/cm
2, polymerization time is 50 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 60 ℃ of oven dry.
Embodiment 2:1) preparation of A solution: at first adding sodium-chlor in methanol solution, to make the concentration of sodium-chlor be the electrolyte solution of 0.6mol/l, the pH of the corresponding hydrochloric acid adjusting of adding and ionogen electrolyte solution is 4 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.9mol/l;
3) insert in B solution then that nickel screen is made the work electrode and graphite cake carries out electrochemical polymerization as counter electrode, the polymerization current density is 15mA/cm
2, polymerization time is 20 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 75 ℃ of oven dry;
4) preparation of C solution: adding ethene dioxythiophene in A solution, to make the concentration of ethene dioxythiophene be 0.1mol/l, obtains C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 15mA/cm
2, polymerization time is 28 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 76 ℃ of oven dry.
Embodiment 3:1) preparation of A solution: at first adding Repone K in carbonic allyl ester solution, to make the concentration of Repone K be the electrolyte solution of 0.3mol/l, the pH of the corresponding hydrochloric acid adjusting of adding and ionogen electrolyte solution is 5 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 1mol/l;
3) insert in B solution then that stainless (steel) wire is made the work electrode and graphite cake carries out electrochemical polymerization as counter electrode, the polymerization current density is 10mA/cm
2, polymerization time is 15 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 80 ℃ of oven dry;
4) preparation of C solution: add in A solution that penylene is made the concentration to penylene is 0.6mol/l, obtain C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 10mA/cm
2, polymerization time is 30 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 72 ℃ of oven dry.
Embodiment 4:1) preparation of A solution: at first adding etamon chloride in acetonitrile solution, to make the concentration of etamon chloride be the electrolyte solution of 0.8mol/l, the pH of the corresponding hydrochloric acid adjusting of adding and ionogen electrolyte solution is 6 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.8mol/l;
3) insert in B solution then that nickel screen is made the work electrode and stainless steel tank is done electrode is carried out electrochemical polymerization, the polymerization current density is 3mA/cm
2, polymerization time is 28 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 65 ℃ of oven dry;
4) preparation of C solution: adding aniline in A solution, to make the concentration of aniline be 0.8mol/l, obtains C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 8mA/cm
2, polymerization time is 45 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 65 ℃ of oven dry.
Embodiment 5:1) preparation of A solution: at first adding lithium perchlorate in water, to make the concentration of lithium perchlorate be the electrolyte solution of 0.2mol/l, the pH of the corresponding lithium hydroxide adjusting of adding and ionogen electrolyte solution is 8 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.2mol/l;
3) insert in B solution then that stainless (steel) wire is made the work electrode and stainless steel tank is done electrode is carried out electrochemical polymerization, the polymerization current density is 9mA/cm
2, polymerization time is 36 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 63 ℃ of oven dry;
4) preparation of C solution: adding ethene dioxythiophene in A solution, to make the concentration of ethene dioxythiophene be 1mol/l, obtains C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 0.6mA/cm
2, polymerization time is 50 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 80 ℃ of oven dry.
Embodiment 6:1) preparation of A solution: at first adding sodium perchlorate in methanol solution, to make sodium perchlorate concentration be the electrolyte solution of 0.9mol/l, the pH of the corresponding sodium hydroxide adjusting of adding and ionogen electrolyte solution is 9 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.5mol/l;
3) insert in B solution then that nickel screen is made the work electrode and stainless steel tank is done electrode is carried out electrochemical polymerization, the polymerization current density is 12mA/cm
2, polymerization time is 45 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 76 ℃ of oven dry;
4) preparation of C solution: add in A solution that penylene is made the concentration to penylene is 0.2mol/l, obtain C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 20mA/cm
2, polymerization time is 36 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 78 ℃ of oven dry.
Embodiment 7:1) preparation of A solution: at first adding potassium perchlorate in carbonic allyl ester solution, to make potassium perchlorate concentration be the electrolyte solution of 1mol/l, the pH of the corresponding potassium hydroxide adjusting of adding and ionogen electrolyte solution is 10 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.7mol/l;
3) insert in B solution then that nickel screen is made the work electrode and graphite cake carries out electrochemical polymerization as counter electrode, the polymerization current density is 7mA/cm
2, polymerization time is 52 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 72 ℃ of oven dry;
4) preparation of C solution: adding aniline in A solution, to make the concentration of aniline be 0.9mol/l, obtains C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 13mA/cm
2, polymerization time is 52 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 63 ℃ of oven dry.
Embodiment 8:1) preparation of A solution: at first adding the perchloric acid tetraethyl ammonium in acetonitrile solution, to make the concentration of perchloric acid tetraethyl ammonium be the electrolyte solution of 0.5mol/l, the pH of the corresponding tetraethyl ammonium hydroxide adjusting of adding and ionogen electrolyte solution is 9 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.4mol/l;
3) insert in B solution then that nickel screen is made the work electrode and stainless steel tank is done electrode is carried out electrochemical polymerization, the polymerization current density is 5mA/cm
2, polymerization time is 60 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 70 ℃ of oven dry;
4) preparation of C solution: adding ethene dioxythiophene in A solution, to make the concentration of ethene dioxythiophene be 0.5mol/l, obtains C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 4mA/cm
2, polymerization time is 20 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 70 ℃ of oven dry.
Embodiment 9:1) preparation of A solution: at first adding Sodium dodecylbenzene sulfonate in water, to make the concentration of Sodium dodecylbenzene sulfonate be the electrolyte solution of 0.7mol/l, the pH of the corresponding Witco 1298 Soft Acid adjusting of adding and ionogen electrolyte solution is 4 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.1mol/l;
3) insert in B solution then that nickel screen is made the work electrode and stainless steel tank is done electrode is carried out electrochemical polymerization, the polymerization current density is 13mA/cm
2, polymerization time is 20 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 63 ℃ of oven dry;
4) preparation of C solution: add in A solution that penylene is made the concentration to penylene is 0.4mol/l, obtain C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 1mA/cm
2, polymerization time is 60 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 63 ℃ of oven dry.
Embodiment 10:1) preparation of A solution: at first in methanol solution, add the electrolyte solution that concentration is 0.4mol/l that is mixed with that p-methyl benzenesulfonic acid sodium makes p-methyl benzenesulfonic acid sodium, the pH of the corresponding p-methyl benzenesulfonic acid adjusting of adding and ionogen electrolyte solution is 3 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.6mol/l;
3) insert in B solution then that nickel screen is made the work electrode and graphite cake carries out electrochemical polymerization as counter electrode, the polymerization current density is 18mA/cm
2, polymerization time is 18 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 69 ℃ of oven dry;
4) preparation of C solution: adding aniline in A solution, to make the concentration of aniline be 0.7mol/l, obtains C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 11mA/cm
2, polymerization time is 30 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 75 ℃ of oven dry.
Embodiment 11:1) preparation of A solution: at first adding 1-naphthalene sulfonic aicd sodium in carbonic allyl ester solution, to make the concentration of 1-naphthalene sulfonic aicd sodium be the electrolyte solution of 0.1mol/l, the pH of the corresponding 1-naphthalene sulfonic aicd adjusting of adding and ionogen electrolyte solution is 4 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.3mol/l;
3) insert in B solution then that stainless (steel) wire is made the work electrode and graphite cake carries out electrochemical polymerization as counter electrode, the polymerization current density is 16mA/cm
2, polymerization time is 30 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 78 ℃ of oven dry;
4) preparation of C solution: adding ethene dioxythiophene in A solution, to make the concentration of ethene dioxythiophene be 0.1mol/l, obtains C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 5mA/cm
2, polymerization time is 18 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 69 ℃ of oven dry.
Embodiment 12:1) preparation of A solution: at first adding the 2-sodium naphthalene sulfonate in acetonitrile solution, to make the concentration of 2-sodium naphthalene sulfonate be the electrolyte solution of 1mol/l, the pH of the corresponding 2-naphthene sulfonic acid adjusting of adding and ionogen electrolyte solution is 4 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 1mol/l;
3) insert in B solution then that nickel screen is made the work electrode and stainless steel tank is done electrode is carried out electrochemical polymerization, the polymerization current density is 20mA/cm
2, polymerization time is 40 minutes; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 80 ℃ of oven dry;
4) preparation of C solution: add in A solution that penylene is made the concentration to penylene is 1mol/l, obtain C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 17mA/cm
2, polymerization time is 5 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 80 ℃ of oven dry.
Because polypyrrole has high specific volume, particularly adopt preparation method of the present invention can make the polypyrrole (as shown in Figure 1) of surface topography for " goat's horn shape ", polypyrrole (PPy) and aniline in addition, ethene dioxythiophene, synergistic effect to the formed polymkeric substance of penylene, the combined electrode that makes the present invention prepare has the bulking value above 200F/g, and has aniline, ethene dioxythiophene, to the distinctive wide electrochemical window of the formed polymkeric substance of penylene: 0～1.2V (at the aqueous solution) or 0～3V (at organic solvent), and when high power discharge, still have higher specific storage and cyclical stability preferably, as shown in Figure 2: its discharge stream density is 100mA/g.
Claims (7)
1, a kind of preparation method of composite conductive high molecular electrode material in use for super capacitor is characterized in that:
1) preparation of A solution: at first adding halogenide, perchlorate or sulfonate in water or organic solvent, to make the concentration of halogenide, perchlorate or sulfonate be the electrolyte solution of 0.1～1mol/l, the PH of adding and the corresponding acid of ionogen or alkali adjusting electrolyte solution is 3～10 in electrolyte solution again, obtains A solution;
2) preparation of B solution: in A solution, add pyrrole monomer, be mixed with the solution B that pyrrole monomer concentration is 0.1～1mol/l;
3) insert stainless (steel) wire or nickel screen then in B solution and make work electrode and stainless steel tank or graphite cake and carry out electrochemical polymerization as counter electrode, the polymerization current density is 3～20mA/cm
2, polymerization time is 1～60 minute; Form polypyrrole at working electrode surface after polymerization is finished, take out working electrode and counter electrode, washing, and 60～80 ℃ of oven dry;
4) preparation of C solution: in A solution, add aniline, ethene dioxythiophene or penylene is made aniline, ethene dioxythiophene or is 0.1～1mol/l to the concentration of penylene, obtain C solution;
5) working electrode of drying and counter electrode are inserted into carry out electrochemical polymerization in the C solution at last, the polymerization current density is 0.2～20mA/cm
2, polymerization time is 5～60 minutes, after polymerization is finished, takes out working electrode, washs, and gets final product 60～80 ℃ of oven dry.
2, the preparation method of composite conductive high molecular electrode material in use for super capacitor according to claim 1 is characterized in that: said organic solvent is methyl alcohol, propylene carbonate or acetonitrile.
3, the preparation method of composite conductive high molecular electrode material in use for super capacitor according to claim 1 is characterized in that: said halogenide is lithium chloride, sodium-chlor, Repone K or etamon chloride.
4, the preparation method of composite conductive high molecular electrode material in use for super capacitor according to claim 1 is characterized in that: said perchlorate is lithium perchlorate, sodium perchlorate, potassium perchlorate or perchloric acid tetraethyl ammonium.
5, the preparation method of composite conductive high molecular electrode material in use for super capacitor according to claim 1 is characterized in that: said sulfonate is Sodium dodecylbenzene sulfonate, p-methyl benzenesulfonic acid sodium, 1-naphthalene sulfonic aicd sodium or 2-sodium naphthalene sulfonate.
6, the preparation method of composite conductive high molecular electrode material in use for super capacitor according to claim 1 is characterized in that: said acid is hydrochloric acid, perchloric acid, Witco 1298 Soft Acid, p-methyl benzenesulfonic acid, 1-naphthalene sulfonic aicd or 2-naphthene sulfonic acid.
7, the preparation method of composite conductive high molecular electrode material in use for super capacitor according to claim 1 is characterized in that: said alkali is sodium hydroxide, lithium hydroxide, potassium hydroxide or tetraethyl ammonium hydroxide.
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| CN102779647B (en) * | 2012-07-16 | 2015-02-25 | 东华大学 | Method for preparing pyrrole/3-(4-tert-butyl benzene) thiophene copolymer for supercapacitor |
| CN103280324A (en) * | 2013-05-30 | 2013-09-04 | 奇瑞汽车股份有限公司 | Organic conducting film layer, manufacturing method of organic conducting film layer, photocathode and dye-sensitized battery |
| CN103280324B (en) * | 2013-05-30 | 2017-11-14 | 奇瑞汽车股份有限公司 | The preparation method of the organic conductive film layer of dye-sensitized cell flexible photocathode, dye-sensitized cell |
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