CN102874807A - Active carbon material and application of same serving as double-electric layer capacitor electrode material - Google Patents
Active carbon material and application of same serving as double-electric layer capacitor electrode material Download PDFInfo
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- CN102874807A CN102874807A CN2012103466767A CN201210346676A CN102874807A CN 102874807 A CN102874807 A CN 102874807A CN 2012103466767 A CN2012103466767 A CN 2012103466767A CN 201210346676 A CN201210346676 A CN 201210346676A CN 102874807 A CN102874807 A CN 102874807A
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- absorbent charcoal
- phosphoric acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
The invention discloses an active carbon material and application of the active carbon material serving as a double-electric layer capacitor electrode material. The active carbon material is prepared by a moso bamboo serving as a carbon source through a phosphoric acid-carbon dioxide physio-chemical activation method. The preparation method specifically comprises the following steps of: (1) getting moso bamboo sheets, adding same to a phosphoric acid solution to be fully dipped, then taking out the bamboo sheets to be dried; (2) transforming the phosphoric acid sheets obtained in step (1) into a tubular furnace, heating to reach 400 to 800 DEG C under N2 protection atmosphere, then switching into CO2 (Carbon Dioxide) atmosphere to activate for 1 to 4 hours at a constant temperature, and finally switching to the N2 protection atmosphere to be cooled to reach a room temperature; and (3) crushing and sieving the produced obtained in step (2), and washing through deionized water until the pH (Potential Of Hydrogen) of filtrate is more than 6; and then drying to obtain a active carbon material. The active carbon material prepared by the preparation method has aperture ranged from 2 to 5nm, and is capable of improving capacity of a capacitor while being used as a double-electric layer capacitor electrode material, and has an excellent performance of charging and discharging.
Description
(1) technical field
The present invention relates to a kind of absorbent charcoal material and as the application of electrode material for electric double layer capacitor.
(2) background technology
Double layer capacitor (Electrochemical Double Layer Capacitor, be called for short EDLC) be a kind of novel energy-storing device between traditional capacitor and battery, have specific power tall and big in 1kW/kg, even reach tens kilowatts every kilogram), the rapid advantages such as (less than 3min) of life-span long (more than 100,000 times), use temperature wide (40 ℃～70 ℃) and charging.These characteristics of double layer capacitor are with a wide range of applications it.
The electrode materials of double layer capacitor mainly is various high-specific surface area carbon materials, such as gac, carbon nanotube and charcoal-aero gel etc.The electrode materials that gac is cheap owing to it, abundant raw material, electrochemical stability high become tool industrialization prospect.But the commercial gac that is used at present double layer capacitor mainly is the Microporous Carbon of various high-specific surface areas.Double layer capacitor specific volume based on this Microporous Carbon is low.
(3) summary of the invention
First purpose of the present invention provides a kind of medium and small mesoporous activated carbon material, and its aperture is at 2-5nm, and it can improve condenser capacity when being used as electrode material for electric double layer capacitor and charge-discharge performance is good.
Second purpose of the present invention is as electrode material for electric double layer capacitor, to improve condenser capacity and to obtain good charge-discharge performance with described absorbent charcoal material.
The below does technical scheme of the present invention and specifies.
A kind of absorbent charcoal material, it is take mao bamboon as carbon source, adopts phosphoric acid-carbonic acid gas physical chemistry activation method to prepare, its preparation method specifically comprises the steps:
(1) gets bamboo plate, add phosphoric acid solution and fully soak, take out bamboo plate dry;
(2) bamboo plate with step (1) gained places tube furnace, at N
2Be warming up to 400-800 ℃ under the atmosphere protection, then switch to CO
2Atmosphere constant temperature activation 1-4h switches back N after finishing
2Protection is cooled to room temperature;
(3) step (2) products obtained therefrom is pulverized, and be washed till filtrate pH value greater than 6 with deionized water, drying obtains absorbent charcoal material.
In the described step (1), phosphoric acid is immersed in the mao bamboon it as chemical activating agent by immersion, and the adding of phosphoric acid can change the pyrolytic process of mao bamboon, is easy to reaming.The massfraction of described phosphoric acid solution is preferably 40 ~ 85%, and more preferably 60 ~ 85%; The mass ratio that feeds intake of phosphoric acid quality and bamboo plate is 2 ~ 4:1.For phosphoric acid fully is immersed in the mao bamboon, can first mao bamboon be cut into the little bamboo chip (for example little bamboo chip of the wide 0.5cm of long 1cm) of certain size, and in the immersion process, can stir in right amount and make it to mix.Usually, soak at room temperature that (25 ~ 30 ℃) carry out, soak time is at 1 ~ 9 day, preferred 5 ~ 9 days.
In the described step (2), be warming up to temperature of reaction first under nitrogen protection, temperature rise rate is preferably 5 ~ 10 ℃/min, then switch to carbon dioxide, react as physically activated dose with carbonic acid gas, temperature of reaction is at 400 ~ 800 ℃, and the reaction times is 1 ~ 4 hour; Preferably, temperature of reaction is 500 ~ 600 ℃, and the reaction times is 3-4h; Preferred, temperature of reaction is 500 ℃, and the reaction times is 3h.Usually control the flow of carbonic acid gas in the reaction process at 40 ~ 60cm
3/ min.
In the described step (3), with the unnecessary phosphoric acid of deionized water flush away, remove impurity, have and also can be washed till neutrality with deionized water again with the salt acid elution first.
The present invention also provides described absorbent charcoal material as electrode material for electric double layer capacitor.
The present invention compared with prior art, its beneficial effect is mainly reflected in:
It is carbon source that the present invention adopts cheap mao bamboon waste material, carbon dioxide is physically activated dose, and phosphoric acid is chemical activating agent, adopts physical chemistry associating activation method to prepare absorbent charcoal material, the raw materials wide material sources, be easy to get, cheap, be easy to industrializing implementation; Preparation technology is simple, without the waste water and gas discharging, thereby environmentally friendly; Double layer capacitor capacity with the absorbent charcoal material preparation is high, and charge-discharge performance is good.
(4) description of drawings
Fig. 1 is the XRD diffractogram of embodiment 1 prepared gac;
Fig. 2 is scanning electron microscope (SEM) and transmission electron microscope (TEM) photo of embodiment 1 prepared gac;
Fig. 3 is the 77K nitrogen adsorption desorption curve of embodiment 1 prepared gac;
Fig. 4 is the prepared double layer capacitor charging and discharging curve figure of embodiment 1, voltage range 0 ~ 0.8V, and charging current is 0.4A/g, measuring temperature is 25 ± 5 ℃.
(5) specific implementation method
The below is described further technical scheme of the present invention with specific embodiment, but protection scope of the present invention is not limited to this.
Embodiment 1
Mao bamboon is cut into the little bamboo chip of the wide 0.5cm of about long 1cm; phosphoric acid and bamboo plate are that to get massfraction be that 85% phosphoric acid solution mixes with bamboo plate for the ratio of 4:1 in massfraction; dry behind the room temperature dipping 7d; place again quartz boat; in tube furnace, be warming up to 500 ℃ with 5 ℃/min temperature rise rate under the nitrogen protection; pass into carbon-dioxide protecting, flow is 40cm
3/ min at 500 ℃ of constant temperature activation 3h, then switches back nitrogen atmosphere, be cooled to room temperature after the taking-up porphyrize cross 200 mesh sieves.Use deionized water wash, until filtrate pH〉6, product is put into loft drier namely obtain absorbent charcoal material in 80 ℃ of dry 12h.
Fig. 1 is the XRD diffractogram of this material, and the reference standard card is about 22 ° and 43 ° of 002 and 100 crystal faces that the diffraction peak of locating is gac at 2 θ as can be known, and the steamed bun peak that occurs among the XRD shows that gac is unbodied.
Fig. 2 (a) is the stereoscan photograph of this material, can find out that the gac duct is rounded, shows a large amount of hole that distributing, and these holes are that diffusion and capillary principal passage occur in electrode ionogen.Fig. 2 (b) is the transmission electron microscope photo of this material, can find out that gac exists many micropores and little mesopore, and mean pore size is between 2-5nm, and these micropores and little mesopore play an important role to the formation of electrostatic double layer.
Fig. 3 is this material adsorption/desorption curve under 77K nitrogen, and the thermoisopleth adsorption curve does not overlap with the desorption curve, has obvious hysteresis, has a large amount of mesopores in the interpret sample, and the aperture mainly concentrates on 2-5nm, and the result is consistent with transmission electron microscope observing.
Make as follows electrode with embodiment 1 prepared gac:
Be coated onto on the nickel foam of 20mm * 20mm after gac mixed in the ratio of 85:10:5 with acetylene black, 60wt% tetrafluoroethylene (PTFE) emulsion respectively, on powder compressing machine, with the pressure pressurize 30s of 15MPa, descend dry 12h 120 ℃ of vacuum drying ovens.Adopt polypropylene diaphragm, electrode slice, barrier film and polythene strip are assembled into electrochemical capacitor, put into and test after 30%KOH electrolytic solution soaks 6h.
Fig. 4 be electrical condenser at constant current 0.4A/g constant current charge-discharge of lower multicycle curve, charging and discharging curve has obvious triangular symmetrical and distributes, and shows that the reversibility of electrode reaction is fine.The voltage of electrical condenser shows that with discharging and recharging the time linear change electrode internal resistance of acceleration voltage decline is less in the constant current charge-discharge process, and the electrical condenser specific storage can reach 190F/g.
Embodiment 2
Mao bamboon is cut into the little bamboo chip of the wide 0.5cm of about long 1cm; phosphoric acid and bamboo plate are that to get massfraction be that 85% phosphoric acid solution mixes with bamboo plate for the ratio of 4:1 in massfraction; dry behind the room temperature dipping 7d; place again quartz boat; in tube furnace, be warming up to 600 ℃ with 5 ℃/min temperature rise rate under the nitrogen protection; pass into carbon-dioxide protecting, flow is 40cm
3/ min at 600 ℃ of constant temperature activation 3h, then switches back nitrogen atmosphere, be cooled to room temperature after the taking-up porphyrize cross 200 mesh sieves.Use deionized water wash, until filtrate pH〉6, product is put into loft drier namely obtain absorbent charcoal material in 80 ℃ of dry 12h.
Make electrode with prepared gac by the method for embodiment 1, be assembled into double layer capacitor, its specific storage reaches 165F/g.
Embodiment 3
Mao bamboon is cut into the little bamboo chip of the wide 0.5cm of about long 1cm; phosphoric acid and bamboo plate are that to get massfraction be that 85% phosphoric acid solution mixes with bamboo plate for the ratio of 3:1 in massfraction; dry behind the room temperature dipping 7d; place again quartz boat; in tube furnace, be warming up to 500 ℃ with 5 ℃/min temperature rise rate under the nitrogen protection; pass into carbon-dioxide protecting, flow is 40cm
3/ min at 500 ℃ of constant temperature activation 4h, then switches back nitrogen atmosphere, be cooled to room temperature after the taking-up porphyrize cross 200 mesh sieves.Use deionized water wash, until filtrate pH〉6, product is put into loft drier namely obtain absorbent charcoal material in 80 ℃ of dry 12h.
Make electrode with prepared gac by the method for embodiment 1, be assembled into double layer capacitor, its specific storage reaches 140F/g.
Claims (9)
1. an absorbent charcoal material is characterized in that it is take mao bamboon as carbon source, adopts phosphoric acid-carbonic acid gas physical chemistry activation method to prepare, and its preparation method specifically comprises the steps:
(1) gets bamboo plate, add phosphoric acid solution and fully soak, take out bamboo plate dry;
(2) bamboo plate with step (1) gained places tube furnace, at N
2Be warming up to 400-800 ℃ under the atmosphere protection, then switch to CO
2Atmosphere constant temperature activation 1-4h switches back N after finishing
2Protection is cooled to room temperature;
(3) step (2) products obtained therefrom is pulverized sieve, and be washed till filtrate pH value greater than 6 with deionized water, drying obtains absorbent charcoal material.
2. absorbent charcoal material according to claim 2, it is characterized in that: in the described step (1), the mass ratio that feeds intake of phosphoric acid and bamboo plate is 2 ~ 4:1.
3. absorbent charcoal material according to claim 1 and 2, it is characterized in that: the massfraction of described phosphoric acid solution is 40 ~ 85%.
4. absorbent charcoal material according to claim 1 and 2, it is characterized in that: the described immersion of step (1) is at room temperature carried out, and soak time is 1 ~ 9 day.
5. absorbent charcoal material according to claim 3, it is characterized in that: the described immersion of step (1) is at room temperature carried out, and soak time is 1 ~ 9 day.
6. absorbent charcoal material according to claim 1 is characterized in that: in the described step (2), bamboo plate is placed tube furnace, at N
2Be warming up to 400 ~ 800 ℃ with 5 ~ 10 ℃/min temperature rise rate under the atmosphere protection.
7. according to claim 1,5 or 6 described absorbent charcoal materials, it is characterized in that: in the described step (2), bamboo plate is placed tube furnace, at N
2Be warming up to 500 ~ 600 ℃ under the atmosphere protection, then switch to CO
2Atmosphere constant temperature activation 3-4h.
8. absorbent charcoal material according to claim 7 is characterized in that: in the described step (2), bamboo plate is placed tube furnace, at N
2Be warming up to 500 ℃ under the atmosphere protection, then switch to CO
2Atmosphere constant temperature activation 3h.
9. absorbent charcoal material according to claim 1 is as the application of electrode material for electric double layer capacitor.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103359730A (en) * | 2013-07-08 | 2013-10-23 | 陈相展 | Activated carbon white powder preparation technology |
| CN104386685A (en) * | 2014-10-22 | 2015-03-04 | 北京化工大学 | Method for preparing nitrogen-doped active carbon from nitrogen-enriched biomass raw material |
| CN105110331A (en) * | 2015-09-01 | 2015-12-02 | 侯梦斌 | Preparation method of low-resistance electrolysis-insoluble electrode |
| CN106219546A (en) * | 2016-08-09 | 2016-12-14 | 中山市天美能源科技有限公司 | A kind of bagasse active carbon and preparation method thereof |
| CN106333418A (en) * | 2016-08-27 | 2017-01-18 | 荥经县极星生物科技有限公司 | Health-care insoles with bamboo activated carbon |
| CN107275102A (en) * | 2017-08-15 | 2017-10-20 | 中国工程物理研究院激光聚变研究中心 | The preparation method of silk hair turf based super capacitor electrode material |
| CN107275101A (en) * | 2017-08-15 | 2017-10-20 | 中国工程物理研究院激光聚变研究中心 | The method that joint activation prepares bamboo charcoal based super capacitor electrode material |
| CN107954422A (en) * | 2017-11-17 | 2018-04-24 | 温州大学新材料与产业技术研究院 | The preparation and application of a kind of mesoporous biological matter carbon plate material of high-specific surface area |
| CN108226253A (en) * | 2018-01-19 | 2018-06-29 | 牡丹江师范学院 | electrochemical sensor based on biomass carbon and preparation method thereof and electro-catalysis application |
| CN110085817A (en) * | 2019-04-15 | 2019-08-02 | 深圳市高能达电池有限公司 | A kind of preparation method and applications of active bamboo/sulphur composite material |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103359730A (en) * | 2013-07-08 | 2013-10-23 | 陈相展 | Activated carbon white powder preparation technology |
| CN104386685A (en) * | 2014-10-22 | 2015-03-04 | 北京化工大学 | Method for preparing nitrogen-doped active carbon from nitrogen-enriched biomass raw material |
| CN105110331A (en) * | 2015-09-01 | 2015-12-02 | 侯梦斌 | Preparation method of low-resistance electrolysis-insoluble electrode |
| CN106219546A (en) * | 2016-08-09 | 2016-12-14 | 中山市天美能源科技有限公司 | A kind of bagasse active carbon and preparation method thereof |
| CN106219546B (en) * | 2016-08-09 | 2019-01-15 | 中山市天美能源科技有限公司 | A kind of bagasse active carbon and preparation method thereof |
| CN106333418A (en) * | 2016-08-27 | 2017-01-18 | 荥经县极星生物科技有限公司 | Health-care insoles with bamboo activated carbon |
| CN107275101A (en) * | 2017-08-15 | 2017-10-20 | 中国工程物理研究院激光聚变研究中心 | The method that joint activation prepares bamboo charcoal based super capacitor electrode material |
| CN107275101B (en) * | 2017-08-15 | 2018-08-31 | 中国工程物理研究院激光聚变研究中心 | The method that joint activation prepares bamboo charcoal based super capacitor electrode material |
| CN107275102B (en) * | 2017-08-15 | 2018-08-31 | 中国工程物理研究院激光聚变研究中心 | The preparation method of silk hair turf based super capacitor electrode material |
| CN107275102A (en) * | 2017-08-15 | 2017-10-20 | 中国工程物理研究院激光聚变研究中心 | The preparation method of silk hair turf based super capacitor electrode material |
| CN107954422A (en) * | 2017-11-17 | 2018-04-24 | 温州大学新材料与产业技术研究院 | The preparation and application of a kind of mesoporous biological matter carbon plate material of high-specific surface area |
| CN107954422B (en) * | 2017-11-17 | 2020-01-24 | 温州大学新材料与产业技术研究院 | Preparation and application of mesoporous biomass carbon sheet material with high specific surface area |
| CN108226253A (en) * | 2018-01-19 | 2018-06-29 | 牡丹江师范学院 | electrochemical sensor based on biomass carbon and preparation method thereof and electro-catalysis application |
| CN110085817A (en) * | 2019-04-15 | 2019-08-02 | 深圳市高能达电池有限公司 | A kind of preparation method and applications of active bamboo/sulphur composite material |
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Application publication date: 20130116 |