CN107316750B - A kind of graphene-based electrode material for super capacitor of high conductivity and preparation method thereof - Google Patents
A kind of graphene-based electrode material for super capacitor of high conductivity and preparation method thereof Download PDFInfo
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- CN107316750B CN107316750B CN201710686087.6A CN201710686087A CN107316750B CN 107316750 B CN107316750 B CN 107316750B CN 201710686087 A CN201710686087 A CN 201710686087A CN 107316750 B CN107316750 B CN 107316750B
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- 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 kind of graphene-based electrode material for super capacitor of high conductivity and preparation methods, are prepared by following raw material in parts by weight: 3 ~ 5 parts of active carbon, 1 ~ 3 point of titania nanotube, 2 ~ 5 parts of graphene, 4 ~ 6 parts of diisostearoyl ethylene titanate, 40 ~ 50 parts of ethyl acetate, 0.2 ~ 0.6 part of polyacrylonitrile, 10 ~ 15 parts of dimethylformamide.Electrode for super capacitor material produced by the present invention has good chemical stability and conductivity, specific capacitance and energy density are higher simultaneously, active carbon and titania nanotube and graphene after processing has good dispersibility and adhesiveness, make full use of the porous structure of graphene, improve the utilization of specific surface area, the conductivity for sufficiently improving active carbon and graphene, improves the surface wettability of graphene, is a kind of good electrode material of comprehensive performance.
Description
Technical field
The present invention relates to electrochemical material preparation field more particularly to a kind of graphene-based supercapacitors of high conductivity
Electrode material and preparation method thereof.
Background technique
Supercapacitor is a kind of energy storaging product of great market competitiveness, and quick charge, heavy-current discharge may be implemented,
And with 100,000 times or more charge lifetimes, occupy epochmaking status in some needs in short-term application of high-multiplying power discharge.
Electrode is the core component of supercapacitor, and electrode material directly influences the performance of supercapacitor, mesh
Preceding common electrode material is active carbon.
With the development of nano material, the two-dimensional graphene material with lamellar structure causes electrochemical material field
Extensive concern.It is a variety of the study found that it is compound with electrode material, the performance of supercapacitor can be promoted.But due to graphite
The two-dimensional nano lamella structure of alkene makes it easily reunite together, and the performance advantage of graphene is difficult to be given full play of.Cause
This, often shows lower conductivity and surface wettability by the capacitor electrode material that graphene is main material, to a certain degree
On limit application of the graphene in electrode material for super capacitor.
Summary of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of high conductivity and good capacitive graphene-based super electricity
Container electrode material and preparation method thereof.
Solve the technical solution that above-mentioned technical problem uses are as follows: a kind of graphene-based electrode of super capacitor of high conductivity
Material is prepared by following raw material in parts by weight: 3 ~ 5 parts of active carbon, 1 ~ 3 point of titania nanotube, graphene 2 ~ 5
Part, 4 ~ 6 parts of diisostearoyl ethylene titanate, 40 ~ 50 parts of ethyl acetate, 0.2 ~ 0.6 part of polyacrylonitrile, dimethylformamide
10 ~ 15 parts.
Preferably, a kind of graphene-based electrode material for super capacitor of high conductivity, by following parts by weight
Several raw materials are prepared: 4 parts of active carbon, titania nanotube 2 divide, 3 parts of graphene, diisostearoyl ethylene titanate
5 parts, 45 parts of ethyl acetate, 0.4 part of polyacrylonitrile, 12 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of high conductivity, including following step
It is rapid:
(1) active carbon and titania nanotube are mixed and is placed in the acid solution of 10 ~ 15 times of amounts, sonic oscillation 10 ~
8 ~ 10h of insulated and stirred after being warming up to 60 ~ 70 DEG C after 20min, obtains mixed liquor, and the deionized water of 2 ~ 3 times of mixing liquid measures of addition is simultaneously quiet
8 ~ 10h is set, is washed with deionized after filtering to neutrality, mixture one is dried to obtain；
(2) the resulting mixture one of step (1) is placed in the mixing of diisostearoyl ethylene titanate and ethyl acetate
In solution, 6 ~ 8h is stood after stirring 1 ~ 2h, filters and dries solids, grinds 1 ~ 2h, 200 meshes is crossed, obtains mixture two；
(3) it will be uniformly mixed under polyacrylonitrile and dimethylformamide room temperature, be then heated to 50 ~ 60 DEG C and graphite is added
Alkene 30 ~ 60min of ultrasound, then 1 ~ 2h of insulated and stirred, filtering are dried at 110 ~ 120 DEG C to constant weight after removing solvent, obtain modification
Graphene；
(4) the strong resulting mixture two of step (2) and step (3) resulting modified graphene are placed in mortar, and grinding 2 ~
4h is subsequently poured into mold, is heated to 120 ~ 130 DEG C, mold is placed on electric tablet machine, in 10MPa pressure to uniform
30 ~ 40min of lower hot pressing after cooling and demolding, is polished smooth the electrode obtained material with sand paper.
Further, acid solution as described in step (1) is the concentrated sulfuric acid and concentrated nitric acid mixed liquor, the concentrated sulfuric acid and concentrated nitric acid
Volume ratio is 2:1.
Compared with prior art, what the present invention had has the beneficial effect that
Electrode for super capacitor material produced by the present invention has good chemical stability and conductivity, while than electricity
Hold and energy density be higher, active carbon and titania nanotube and graphene after processing have good dispersibility and
Adhesiveness makes full use of the porous structure of graphene, improves the utilization of specific surface area, sufficiently improves active carbon and graphene
Conductivity improves the surface wettability of graphene, is a kind of good electrode material of comprehensive performance.
Specific embodiment
The present invention is described further combined with specific embodiments below.Following embodiment is only described the present invention
The explanation of property, this does not limit the scope of protection of the present invention.
Moreover, raw material used in the present invention is unless otherwise required conventional commercial product；Likewise, being made
Method is conventional production method unless otherwise required.
Embodiment 1: a kind of graphene-based electrode material for super capacitor of high conductivity, by the raw material of following parts by weight
Be prepared: 4 parts of active carbon, titania nanotube 2 divide, 3 parts of graphene, 5 parts of diisostearoyl ethylene titanate, acetic acid
45 parts of ethyl ester, 0.4 part of polyacrylonitrile, 12 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of high conductivity, including following step
It is rapid:
(1) active carbon and titania nanotube are mixed and is placed in the acid solution of 12 times of amounts, after sonic oscillation 15min
Insulated and stirred 9h, obtains mixed liquor after being warming up to 65 DEG C, and the deionized water of 2 times of mixing liquid measures is added and stands 9h, spends after filtering
Ion water washing is dried to obtain mixture one to neutrality；
(2) the resulting mixture one of step (1) is placed in the mixing of diisostearoyl ethylene titanate and ethyl acetate
In solution, 7h is stood after stirring 1h, filters and dries solids, grinds 2h, 200 meshes is crossed, obtains mixture two；
(3) it will be uniformly mixed under polyacrylonitrile and dimethylformamide room temperature, be then heated to 55 DEG C and graphene is added
Ultrasonic 45min, then insulated and stirred 2h, filtering are dried at 115 DEG C to constant weight after removing solvent, obtain modified graphene；
(4) the strong resulting mixture two of step (2) and step (3) resulting modified graphene are placed in mortar, grind 3h
To uniform, it is subsequently poured into mold, is heated to 125 DEG C, mold is placed on electric tablet machine, the hot pressing under 10MPa pressure
35min after cooling and demolding, is polished smooth the electrode obtained material with sand paper.
Further, acid solution as described in step (1) is the concentrated sulfuric acid and concentrated nitric acid mixed liquor, the concentrated sulfuric acid and concentrated nitric acid
Volume ratio is 2:1.
Embodiment 2: a kind of graphene-based electrode material for super capacitor of high conductivity, by the raw material of following parts by weight
Be prepared: 3 parts of active carbon, titania nanotube 1 divide, 2 parts of graphene, 4 parts of diisostearoyl ethylene titanate, acetic acid
40 parts of ethyl ester, 0. part of polyacrylonitrile, 10 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of high conductivity, including following step
It is rapid:
(1) active carbon and titania nanotube are mixed and is placed in the acid solution of 10 times of amounts, after sonic oscillation 10min
Insulated and stirred 8h, obtains mixed liquor after being warming up to 60 DEG C, and the deionized water of 2 times of mixing liquid measures is added and stands 8h, spends after filtering
Ion water washing is dried to obtain mixture one to neutrality；
(2) the resulting mixture one of step (1) is placed in the mixing of diisostearoyl ethylene titanate and ethyl acetate
In solution, 6h is stood after stirring 1h, filters and dries solids, grinds 1h, 200 meshes is crossed, obtains mixture two；
(3) it will be uniformly mixed under polyacrylonitrile and dimethylformamide room temperature, be then heated to 50 DEG C and graphene is added
Ultrasonic 30min, then insulated and stirred 1h, filtering are dried at 110 DEG C to constant weight after removing solvent, obtain modified graphene；
(4) the strong resulting mixture two of step (2) and step (3) resulting modified graphene are placed in mortar, grind 2h
To uniform, it is subsequently poured into mold, is heated to 120 DEG C, mold is placed on electric tablet machine, the hot pressing under 10MPa pressure
30min after cooling and demolding, is polished smooth the electrode obtained material with sand paper.
Further, acid solution as described in step (1) is the concentrated sulfuric acid and concentrated nitric acid mixed liquor, the concentrated sulfuric acid and concentrated nitric acid
Volume ratio is 2:1.
Embodiment 3: a kind of graphene-based electrode material for super capacitor of high conductivity, by the raw material of following parts by weight
Be prepared: activity 5 parts, titania nanotube 3 divide, 5 parts of graphene, 6 parts of diisostearoyl ethylene titanate, acetic acid second
50 parts of ester, 0.6 part of polyacrylonitrile, 15 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of high conductivity, including following step
It is rapid:
(1) active carbon and titania nanotube are mixed and is placed in the acid solution of 15 times of amounts, after sonic oscillation 20min
Insulated and stirred 10h, obtains mixed liquor after being warming up to 70 DEG C, and the deionized water of 3 times of mixing liquid measures is added and stands 10h, uses after filtering
Deionized water is washed to neutrality, and mixture one is dried to obtain；
(2) the resulting mixture one of step (1) is placed in the mixing of diisostearoyl ethylene titanate and ethyl acetate
In solution, 8h is stood after stirring 2h, filters and dries solids, grinds 2h, 200 meshes is crossed, obtains mixture two；
(3) it will be uniformly mixed under polyacrylonitrile and dimethylformamide room temperature, be then heated to 60 DEG C and graphene is added
Ultrasonic 60min, then insulated and stirred 2h, filtering are dried at 120 DEG C to constant weight after removing solvent, obtain modified graphene；
(4) the strong resulting mixture two of step (2) and step (3) resulting modified graphene are placed in mortar, grind 4h
To uniform, it is subsequently poured into mold, is heated to 130 DEG C, mold is placed on electric tablet machine, the hot pressing under 10MPa pressure
40min after cooling and demolding, is polished smooth the electrode obtained material with sand paper.
Further, acid solution as described in step (1) is the concentrated sulfuric acid and concentrated nitric acid mixed liquor, the concentrated sulfuric acid and concentrated nitric acid
Volume ratio is 2:1.
Embodiment 4: a kind of graphene-based electrode material for super capacitor of high conductivity, by the raw material of following parts by weight
Be prepared: 3 parts of active carbon, titania nanotube 3 divide, 2 parts of graphene, 6 parts of diisostearoyl ethylene titanate, acetic acid
40 parts of ethyl ester, 0.6 part of polyacrylonitrile, 10 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of high conductivity, phase specific steps are same
Embodiment 1.
Embodiment 5: a kind of graphene-based electrode material for super capacitor of high conductivity, by the raw material of following parts by weight
Be prepared: 4 parts of active carbon, titania nanotube 1 divide, 5 parts of graphene, 5 parts of diisostearoyl ethylene titanate, poly- third
0.5 part of alkene nitrile, 13 parts of dimethylformamide.
A kind of preparation method of the graphene-based electrode material for super capacitor of high conductivity, phase specific steps are same
Embodiment 1.
Have higher conductivity, energy density and power close using supercapacitor made from electrode material of the invention
Degree, while chemical stability is good, has more superior performance.
Should it is again noted that above-described embodiment content is only the preferred embodiment of the present invention, be not to be regarded as
For limiting practical range of the invention.It is all according to equivalent change made by the present patent application range or improvement, should still belong to
Within protection scope of the present invention.
Claims (3)
1. a kind of graphene-based electrode material for super capacitor of high conductivity, it is characterised in that: by the original of following parts by weight
Material is prepared: 3 ~ 5 parts of active carbon, 1 ~ 3 part of titania nanotube, 2 ~ 5 parts of graphene, diisostearoyl ethylene titanate
4 ~ 6 parts, 40 ~ 50 parts of ethyl acetate, 0.2 ~ 0.6 part of polyacrylonitrile, 10 ~ 15 parts of dimethylformamide；
A kind of preparation method of the graphene-based electrode material for super capacitor of high conductivity comprising following steps:
(1) active carbon and titania nanotube are mixed and is placed in the acid solution of 10 ~ 15 times of amounts, 10 ~ 20min of sonic oscillation
After be warming up to 60 ~ 70 DEG C after 8 ~ 10h of insulated and stirred, obtain mixed liquor, the deionized waters of 2 ~ 3 times of mixing liquid measures are added and stand 8 ~
10h is washed with deionized after filtering to neutrality, is dried to obtain mixture one；
(2) the resulting mixture one of step (1) is placed in the mixed solution of diisostearoyl ethylene titanate and ethyl acetate
In, 6 ~ 8h is stood after stirring 1 ~ 2h, filters and dries solids, grinds 1 ~ 2h, 200 meshes is crossed, obtains mixture two；
(3) it will be uniformly mixed under polyacrylonitrile and dimethylformamide room temperature, and be then heated to 50 ~ 60 DEG C and that graphene is added is super
30 ~ 60min of sound, then 1 ~ 2h of insulated and stirred, filtering are dried at 110 ~ 120 DEG C to constant weight after removing solvent, obtain modified graphite
Alkene；
(4) the resulting mixture two of step (2) and step (3) resulting modified graphene are placed in mortar, 2 ~ 4h of grinding is extremely
Uniformly, it is subsequently poured into mold, is heated to 120 ~ 130 DEG C, mold is placed on electric tablet machine, it is hot under 10MPa pressure
Press 30 ~ 40min, after cooling and demolding, polished smooth the electrode obtained material with sand paper.
2. a kind of graphene-based electrode material for super capacitor of high conductivity according to claim 1, it is characterised in that:
It is prepared by following raw material in parts by weight: 4 parts of active carbon, 2 parts of titania nanotube, 3 parts of graphene, two isostearoyls
5 parts of base metatitanic acid second diester, 45 parts of ethyl acetate, 0.4 part of polyacrylonitrile, 12 parts of dimethylformamide.
3. a kind of graphene-based electrode material for super capacitor of high conductivity according to claim 1, it is characterised in that:
Acid solution as described in step (1) is the concentrated sulfuric acid and concentrated nitric acid mixed liquor, and the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 2:1.
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| CN114743800B (en) * | 2022-04-25 | 2023-07-21 | 武夷学院 | Preparation method of polyacrylic acid/graphene-based flexible electrode material |
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| CN106252089A (en) * | 2016-08-03 | 2016-12-21 | 代长华 | A kind of electrode material for super capacitor and preparation method thereof |
| CN106486290A (en) * | 2016-11-08 | 2017-03-08 | 铜陵市启动电子制造有限责任公司 | A kind of titanium manganese blending modification shitosan polypyrrole charcoal combination electrode material |
| CN106683897A (en) * | 2016-12-10 | 2017-05-17 | 宁国市大荣电器有限公司 | Modified graphene supercapacitor electrode material |
| CN106783212A (en) * | 2016-11-22 | 2017-05-31 | 张家港智电芳华蓄电研究所有限公司 | A kind of preparation method of porous carbon electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106252089A (en) * | 2016-08-03 | 2016-12-21 | 代长华 | A kind of electrode material for super capacitor and preparation method thereof |
| CN106486290A (en) * | 2016-11-08 | 2017-03-08 | 铜陵市启动电子制造有限责任公司 | A kind of titanium manganese blending modification shitosan polypyrrole charcoal combination electrode material |
| CN106783212A (en) * | 2016-11-22 | 2017-05-31 | 张家港智电芳华蓄电研究所有限公司 | A kind of preparation method of porous carbon electrode |
| CN106683897A (en) * | 2016-12-10 | 2017-05-17 | 宁国市大荣电器有限公司 | Modified graphene supercapacitor electrode material |
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