CN103723722A - Preparation method of graphene-modified activated carbon for supercapacitor - Google Patents
Preparation method of graphene-modified activated carbon for supercapacitor Download PDFInfo
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- CN103723722A CN103723722A CN201310590070.2A CN201310590070A CN103723722A CN 103723722 A CN103723722 A CN 103723722A CN 201310590070 A CN201310590070 A CN 201310590070A CN 103723722 A CN103723722 A CN 103723722A
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Abstract
The invention discloses a preparation method of graphene-modified activated carbon for a supercapacitor and belongs to the technical field of electrode material preparation. The method comprises the steps of taking petroleum coke activated carbon as a raw material, removing impurities, matching graphene with specific parameters, performing high-temperature activation and removing organic solvents to obtain the graphene-modified activated carbon for the supercapacitor. The activated carbon prepared with the method is 1600-2020 m<2> in specific surface area and 0.3008 g/ml in tap density and has various specific parameters of the activated carbon for the supercapacitor. The supercapacitor made of the activated carbon is above 320 F/g in mass specific capacitance and 198 F/cm<2> in volume specific capacitance.
Description
Technical field
The invention belongs to electrode materials preparing technical field, be specifically related to a kind of preparation method of Graphene modification activated carbon for super capacitors, the present invention relates to a kind of preparation method of Graphene modification activated carbon for super capacitors, it is in organic solvent, to carry out high-temperature activation by adding Graphene after gac decon, then removes organic solvent and obtain Graphene modification super capacitor gac.
Background technology
Ultracapacitor is a kind of model electrochemical energy storage device.Because it is according to electrochemical principle design, produced, the electrochemical capacitor that is therefore otherwise known as, general reference has the electrical condenser of superpower and high-energy-density.Ultracapacitor have discharge and recharge fast, long service life, power density high, safeguard the advantages such as simple and convenient, economic environmental protection, have more and more important, purposes more and more widely.
Carbon material, particularly sp
2the carbon material of hydridization, because the specific surface area of special laminate structure, super large forms the electrode materials into important energy storage device.Carbon material is widely used in lithium cell as decolorizing carbon, gac, graphite etc.
Graphene has higher specific surface area and high specific conductivity because of it, therefore when as capacitor material, have the character more excellent than traditional porous carbon materials, but Graphene volumetric capacitance is little, cannot be applied to the electricity devices such as jumbo ultracapacitor.Although the volumetric capacitance that can improve Graphene with activated carbon modified Graphene is to 119.7F/cm
2, but the activation temperature of its modifying process is higher, and Graphene is expensive, simultaneously owing to not preparing in a large number the technology of Graphene at present, and can not suitability for industrialized production so prepare electrode for super capacitor material with Graphene.
Gac is that ultracapacitor is used maximum electrode materialss, has the advantages such as specific surface area is high, electrochemical stability good, abundant raw material.But gac electroconductibility is poor, pore size distribution is unreasonable, the microvoid structure of gac has been contributed main specific surface area, and the migration resistance of ion in micropore is larger, and in addition, the ultracapacitor heat dispersion that traditional gac is made is undesirable.Therefore, no matter how its raw material sources change, how preparation technology to improve, and the specific surface area of traditional gac has reached peak value, the very large breakthrough of cannot having reentried of the capacitor performance of traditional Activated Carbon Production.
Therefore, how to overcome the deficiencies in the prior art and become the difficult problem that electrode materials preparing technical field is needed solution badly.
Summary of the invention
The object of the invention is, in order to solve the deficiencies in the prior art, provides a kind of preparation method of graphene oxide modification activated carbon for super capacitors, and gac specific surface area prepared by the method reaches 1600 m
2~ 2020m
2, tap density reaches 0.3008g/ml, the ultracapacitor of making of it, and more than quality reaches 320F/g than electric capacity, volumetric capacitance reaches 198F/cm
2.
The technical solution used in the present invention is as follows:
A kind of preparation method of Graphene modification activated carbon for super capacitors adds Graphene dispersion in organic solvent by gac raw material after washing, supersound process, be heated to after 60 ℃ ~ 100 ℃, constant temperature is stirred to and mixes fully, then obtains Graphene modification activated carbon for super capacitors through filtration and centrifugal treating; Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:1 ~ 1:80, and Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene and organic solvent is 1 ‰ ~ 5%;
Described organic solvent is one or more the composition in dimethyl carbonate, the first and second base carbonic ethers, NSC 11801, propylene carbonate and gamma-butyrolactone, and its concrete ratio is not done requirement.Select organic solvent, compare with deionized water, the difference of its wetting property causes Graphene-gac packaging assembly different, thereby makes volumetric capacitance and the quality of the Graphene gac mixture that obtains higher than electric capacity.
Further preferably described gac raw material is refinery coke gac.
Further preferably described gac raw material granularity is 800 ~ 12000 orders.
Further preferably described graphene film footpath is 100nm ~ 500 μ m.
Further preferably the time of described supersound process is 0.5h ~ 10h.
Further preferably under described heated constant temperature condition, churning time is 0.5h ~ 10h.
Further preferably the mode of described removal organic solvent is centrifugation.
compared with prior art, its beneficial effect is in the present invention:the present invention, by introducing Graphene, has formed the network configuration that Graphene and gac form, and first makes the specific surface area of gac be fully used, and utilization ratio is up to 99%; Next has increased substantially the electroconductibility of gac, has fundamentally changed the large problem of ion migration resistance; Again, the heat conductivility of Graphene excellence makes the heat dispersion of device improve 55%.The present invention uses a small amount of Graphene, avoids using high activation temperature can make the Properties of Activated Carbon obtaining significantly improve, and Integrated using cost is low, and added value is high, can be applicable to suitability for industrialized production.Select organic solvent to make dispersion liquid, the gac of modification is than capacitance data, current best higher by 60.1% than the world.
Accompanying drawing explanation
Fig. 1 is the Electronic Speculum figure of the Graphene modification activated carbon for super capacitors of the embodiment of the present invention 8 preparations.
Specific embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
The present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
A kind of preparation method of Graphene modification activated carbon for super capacitors adds Graphene dispersion in organic solvent by 800 object refinery coke gacs after washing, supersound process 0.5h, be heated to after 60 ℃, constant temperature stirs 0.5h, through centrifugation, remove organic solvent again, obtain the present embodiment Graphene modification activated carbon for super capacitors; Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:1, and Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene and dimethyl carbonate is 1 ‰, and graphene film footpath is 100nm.
Embodiment 2
A kind of preparation method of Graphene modification activated carbon for super capacitors adds Graphene dispersion in organic solvent by 12000 object refinery coke gacs after washing, supersound process 10h, be heated to after 100 ℃, constant temperature stirs 10h to mixing fully, through centrifugation, remove organic solvent again, obtain the present embodiment Graphene modification activated carbon for super capacitors; Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:80, and Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene and the first and second base carbonic ethers is 5%, and graphene film footpath is 500 μ m.
Embodiment 3
A kind of preparation method of Graphene modification activated carbon for super capacitors adds Graphene dispersion in organic solvent by 1000 object refinery coke gacs after washing, supersound process 2h, be heated to after 70 ℃, constant temperature stirs 4h to mixing fully, through centrifugation, remove organic solvent again, obtain the present embodiment Graphene modification activated carbon for super capacitors; Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:20, and Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene and NSC 11801 is 9 ‰, and graphene film footpath is 100 μ m.
Embodiment 4
A kind of preparation method of Graphene modification activated carbon for super capacitors adds Graphene dispersion in organic solvent by 1000 object refinery coke gacs after washing, supersound process 4h, be heated to after 80 ℃, constant temperature stirs 5h to mixing fully, through centrifugation, remove organic solvent again, obtain the present embodiment Graphene modification activated carbon for super capacitors; Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:30, and Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene and propylene carbonate is 1%, and graphene film footpath is 100 μ m.
Embodiment 5
A kind of preparation method of Graphene modification activated carbon for super capacitors adds Graphene dispersion in organic solvent by 1000 object refinery coke gacs after washing, supersound process 7h, be heated to after 90 ℃, constant temperature stirs 8h to mixing fully, through centrifugation, remove organic solvent again, obtain the present embodiment Graphene modification activated carbon for super capacitors; Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:78, and Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene and gamma-butyrolactone is 2%, and graphene film footpath is 100 μ m.
Embodiment 6
A kind of preparation method of Graphene modification activated carbon for super capacitors adds Graphene dispersion in organic solvent by 1000 object refinery coke gacs after washing, supersound process 9h, be heated to after 75 ℃, constant temperature stirs 6h to mixing fully, through centrifugation, remove organic solvent again, obtain the present embodiment Graphene modification activated carbon for super capacitors; Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:40, Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene, dimethyl carbonate and the first and second base carbonic ethers and organic solvent is 2:34:66, and graphene film footpath is 100 μ m.
Embodiment 7
A kind of preparation method of Graphene modification activated carbon for super capacitors adds Graphene dispersion in organic solvent by 1000 object refinery coke gacs after washing, supersound process 3h, be heated to after 60 ℃ ~ 100 ℃, constant temperature stirs 5h to mixing fully, through centrifugation, remove organic solvent again, obtain the present embodiment Graphene modification activated carbon for super capacitors; Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:45, Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene, the first and second base carbonic ethers, NSC 11801 and propylene carbonate is 2:25:40:35, and graphene film footpath is 100 μ m.
Embodiment 8
A kind of preparation method of Graphene modification activated carbon for super capacitors adds Graphene dispersion in organic solvent by 1000 object refinery coke gacs after washing, supersound process 7h, be heated to after 88 ℃, constant temperature stirs 4h to mixing fully, through centrifugation, remove organic solvent again, obtain the present embodiment Graphene modification activated carbon for super capacitors; Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:35, Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene, dimethyl carbonate, the first and second base carbonic ethers, NSC 11801, propylene carbonate and gamma-butyrolactone is 2:25:25:25:25:25, and graphene film footpath is 100 μ m;
The Electronic Speculum figure of the Graphene modified activated carbon that is applicable to ultracapacitor that the present embodiment makes as shown in Figure 1.In figure, can find out the form that Graphene and gac are compound.
Embodiment 9
A kind of preparation method of Graphene modification activated carbon for super capacitors adds Graphene dispersion in organic solvent by 1000 object refinery coke gacs after washing, supersound process 7h, be heated to after 66 ℃, constant temperature stirs 7h to mixing fully, through centrifugation, remove organic solvent again, obtain the present embodiment Graphene modification activated carbon for super capacitors; Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:75, Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene, dimethyl carbonate, the first and second base carbonic ethers, propylene carbonate and gamma-butyrolactone is 1:25:25:25:25, and graphene film footpath is 100 μ m.
Comparative example
Take 1000 object refinery coke gac 1.43g, after washing, adding 50g mass ratio is 1:1:1:1:1 dimethyl carbonate, the first and second base carbonic ethers, NSC 11801, propylene carbonate and gamma-butyrolactone mixed organic solvents, supersound process 7h, be heated to after 88 ℃, constant temperature stirs 4h to mixing fully, then obtains gac through centrifugation removal organic solvent.
The embodiment of the present invention 1 ~ 9 and comparative example's processing parameter and products thereof performance detection data is as shown in table 1.
Table 1 embodiment of the present invention 1 ~ 9 and comparative example's processing parameter and products thereof performance detection data
| ? | Graphene | Graphene dispersion in organic solvent | Refinery coke gac | Quality compares electric capacity | Volumetric capacitance |
| Embodiment 1 | 0.5g | 500.0g | 500.0g | 199.1F/cm 2 | 321.1F/g |
| Embodiment 2 | 1.0g | 20.0g | 0.25g | 198.2F/cm 2 | 320.6F/g |
| Embodiment 3 | 0.9g | 100.0g | 5.0g | 198.5F/cm 2 | 321.2F/g |
| Embodiment 4 | 1.0g | 100.0g | 3.3g | 198.9F/cm 2 | 324.0F/g |
| Embodiment 5 | 1.0g | 50.0g | 0.64g | 198.3F/cm 2 | 321.3F/g |
| Embodiment 6 | 1.0g | 50.0g | 1.25g | 198.2F/cm 2 | 321.5F/g |
| Embodiment 7 | 1.0g | 50.0g | 1.11g | 198.3F/cm 2 | 320.4F/g |
| Embodiment 8 | 1.0g | 50.0g | 1.43g | 199.8F/cm 2 | 326.1F/g |
| Embodiment 9 | 1.0g | 100.0g | 1.33g | 198.7F/cm 2 | 322.8F/g |
| Comparative example | 0g | 100.0g | 1.43g | 118.4F/cm 2 | 198.1F/g |
From above-described embodiment, can find out, the activated carbon for super capacitors after Graphene modification, volumetric capacitance and quality have significantly and promote than electric capacity.
Content and the composition of the Graphene modification activated carbon for super capacitors of embodiment 8 preparations are detected, it is as shown in table 2 that it detects data simultaneously.
The detection data of the Graphene modification activated carbon for super capacitors of table 2 embodiment 8 preparations
| Interventions Requested | Assay | Unit |
| Ash content | 0.02 | % |
| Moisture | 0.12 | % |
| PH | 4.99 | ? |
| Chlorine | 10 | ppm |
| Iron | 1 | ppm |
| Plumbous | 1 | ppm |
| Iodine absorption | 1800.2 | mg/g |
| TMP | 65.05 | % |
| Functional group | 1k6: carboxyl 0.05, phenolic hydroxyl group 0.10, hydroxyl 0.35 meq/g | Meq/g |
| Tap density | 0.3008 | g/cm3 |
Claims (7)
1. the preparation method of a Graphene modification activated carbon for super capacitors, it is characterized in that gac raw material to add Graphene dispersion in organic solvent after washing, supersound process, be heated to after 60 ℃ ~ 100 ℃, constant temperature is stirred to and mixes fully, then removes organic solvent and obtain Graphene modification activated carbon for super capacitors; The specific surface area of this gac reaches 1600 m
2~ 2020m
2, tap density reaches 0.3008g/ml;
Wherein, the mass ratio of gac and Graphene dispersion in organic solvent is 1:1 ~ 1:80;
Graphene dispersion in organic solvent is the mixture that the mass ratio of Graphene and organic solvent is 1 ‰ ~ 5%;
Described organic solvent is one or more the composition in dimethyl carbonate, the first and second base carbonic ethers, NSC 11801, propylene carbonate and gamma-butyrolactone.
2. the preparation method of Graphene modification activated carbon for super capacitors according to claim 1, is characterized in that described gac raw material is refinery coke gac.
3. the preparation method of Graphene modification activated carbon for super capacitors according to claim 1, is characterized in that described gac raw material granularity is 800 ~ 12000 orders.
4. the preparation method of Graphene modification activated carbon for super capacitors according to claim 1, is characterized in that described graphene film footpath is 100nm ~ 500 μ m.
5. the preparation method of Graphene modification activated carbon for super capacitors according to claim 1, is characterized in that the time of described supersound process is 0.5h ~ 10h.
6. the preparation method of Graphene modification activated carbon for super capacitors according to claim 1, is characterized in that under described heated constant temperature condition, churning time is 0.5h ~ 10h.
7. the preparation method of Graphene modification activated carbon for super capacitors according to claim 1, is characterized in that the mode of described removal organic solvent is centrifugation.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105118682A (en) * | 2015-09-14 | 2015-12-02 | 清华大学 | Composite particles composed of active carbon and graphene hybrids, preparation method and application |
| CN105800613A (en) * | 2016-04-18 | 2016-07-27 | 方大炭素新材料科技股份有限公司 | Preparation method for activated carbon based on graphene composite modification and used for supercapacitor |
| CN105977047A (en) * | 2016-05-24 | 2016-09-28 | 宁波墨西科技有限公司 | Graphene/active-carbon composite electrode material and preparation method thereof |
| CN106006853A (en) * | 2016-06-28 | 2016-10-12 | 南京林业大学 | Preparing method for active-carbon and graphene composite electrode material for drinking-water purification |
| CN108417408A (en) * | 2018-01-17 | 2018-08-17 | 莆田市超维二维科技发展有限公司 | A kind of ultracapacitor and preparation method thereof |
| CN109665524A (en) * | 2017-10-16 | 2019-04-23 | 山东欧铂新材料有限公司 | A kind of preparation method and supercapacitor of small particle graphene composite stone oil coke matrix activated carbon |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105118682A (en) * | 2015-09-14 | 2015-12-02 | 清华大学 | Composite particles composed of active carbon and graphene hybrids, preparation method and application |
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| CN105800613A (en) * | 2016-04-18 | 2016-07-27 | 方大炭素新材料科技股份有限公司 | Preparation method for activated carbon based on graphene composite modification and used for supercapacitor |
| CN105977047A (en) * | 2016-05-24 | 2016-09-28 | 宁波墨西科技有限公司 | Graphene/active-carbon composite electrode material and preparation method thereof |
| CN106006853A (en) * | 2016-06-28 | 2016-10-12 | 南京林业大学 | Preparing method for active-carbon and graphene composite electrode material for drinking-water purification |
| CN109665524A (en) * | 2017-10-16 | 2019-04-23 | 山东欧铂新材料有限公司 | A kind of preparation method and supercapacitor of small particle graphene composite stone oil coke matrix activated carbon |
| CN108417408A (en) * | 2018-01-17 | 2018-08-17 | 莆田市超维二维科技发展有限公司 | A kind of ultracapacitor and preparation method thereof |
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