CN1117028C - Process for preparing activated carbon to make electrode of super capacitor - Google Patents
Process for preparing activated carbon to make electrode of super capacitor Download PDFInfo
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- CN1117028C CN1117028C CN 00118967 CN00118967A CN1117028C CN 1117028 C CN1117028 C CN 1117028C CN 00118967 CN00118967 CN 00118967 CN 00118967 A CN00118967 A CN 00118967A CN 1117028 C CN1117028 C CN 1117028C
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- super capacitor
- activated carbon
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- coking
- active carbon
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Abstract
The present invention discloses a method for preparing activated carbon to make an electrode of a super capacitor. The method uses phenol-formaldehyde resin as raw materials, and coking, carbonization, activation, washing, drying, etc. are carried out to the phenol-formaldehyde resin to obtain the needed activated carbon. The technical key points of the present invention lie in the temperature of coking, carbonization and activation and an activating agent adopted. The specific surface area of the activated carbon prepared by the present invention reaches more than 2000m<2>/g, and the specific weight reaches more than 0.72 g/cm<3>; the weight ratio capacitance of the electrode of the super capacitor made of the activated carbon reaches more than 250 F/g, and the volume ratio capacitance reaches more than 174 F/cm<3>.
Description
The invention relates to a kind of special purpose process of active carbon of preparation.The gac that utilizes this method to produce can be used for making the electrode of ultracapacitor.
Ultracapacitor had both had the high-specific-power and the high cyclicity characteristics of ordinary capacitor, had the energy storage characteristics of battery again, and therefore, it can satisfy the service requirements of high-specific-power, can satisfy the service requirements than high-energy-density again.Because it has high temperature resistant, semipermanent charge-discharge performance and non-maintaining advantage than battery, has been widely used in IC unicircuit, super large-scale integration and computer storage backup battery, and the standby power supply of other high loadinies.Particularly the ultracapacitor of high-energy-density can be independently or with secondary cell (as the lithium ion battery) combination of high-energy-density power-supply system as electromobile, prospect will be widely used.
The energy storage of ultracapacitor is based on the electrical double layer that the electrode charging forms down.Therefore require the material of electrode should have very high specific surface area and suitable big density.The specific surface area of gac BET commonly used is less than 1000m
2/ g is used to make the electrode of electrical condenser, the about 60F/g of its gravimetric capacitance, and volumetric capacitance only is 40F/cm
2, can not satisfy the electrode of super capacitor performance requriements far away.
Purpose of the present invention is to provide a kind of method for preparation of active carbon of making electrode of super capacitor.The prepared gac of Using such method is made the electrode of electrical condenser, and gravimetric capacitance can reach more than the 250F/g, and volumetric capacitance can reach 174F/cm
3More than.
For achieving the above object, the present invention is realized by following technical proposals.With the resin is raw material, mainly passes through coking, carbonization, activation treatment and comprises the gac that aftertreatments such as washing, oven dry, pulverizing obtain, and it is characterized in that, the resin that is adopted is a resol, carry out coking and handled 3～5 hours under 150～300 ℃, carbonizing matter carries out charing under 400～700 ℃ handles, and obtains carbon material, with carbonic acid gas, or water vapor, or potassium hydroxide solution, or liquor zinci chloridi, or sodium hydroxide solution is promoting agent, carries out activation treatment at 450～900 ℃.
Above-mentioned best coking is treated to 180～220 ℃ of temperature.
Above-mentioned best charing treatment temp is 500～600 ℃.
Above-mentioned optimal activation treatment temp is 600～700 ℃.
Above-mentioned optimal activation treatment agent is a sodium hydroxide solution.
Below the present invention is described in detail.
It is raw material that the present invention adopts resol, and with being that raw material is produced gac and compared with coal or rice husk, its comprehensive physical property of the gac that is obtained is higher.The gac of the low slightly rice husk of specific surface area wherein, and proportion, volumetric capacitance, gravimetric capacitance all are higher than other gacs.Therefore the selected resol of the present invention is starting material, has established one step of key that the present invention has three property.In technological process of the present invention, wherein activating treatment temperature is one of gordian technique.Activation treatment improves activation temperature and can increase specific surface area, but its proportion will descend, and therefore controls an optimal activation treatment temp, can guarantee that gac has higher comprehensive physical property, and optimal activation treatment temp of the present invention is 600～700 ℃.
With embodiment the present invention is further specified again below.From of the influence of example one visible different activation temperatures to the gac physical property; Adopt different starting material, the difference of the gac physical property of producing from example two is visible: when as seen example three carries out activation treatment with different activating treatment agents, the difference of the physical property of gac.
Example one:
With 180 ℃ of resol heating, be incubated 4 hours earlier, coking is handled.Pyrogenic resin 400～700 ℃ of heating charing in 1 hour processing down, obtains carbon material through pulverizing.With carbon material and sodium hydroxide activator mix, nitrogen protection, thermal treatment temp is divided into 450 ℃, 500 ℃, 550 ℃, 600 ℃, 700 ℃, 800 ℃, 900 ℃, and heat-up rate is 20 ℃/h, is incubated 30 minutes, obtains the different activities charcoal.These gac reusable heat water washings, oven dry and pulverizing obtain gac.The physical property of these gacs is as shown in table 1.With this gac is that material preparation becomes electrical condenser, is electrolytic solution with 30%KOH, and the charge and discharge voltage range is at 0.05～1.0 volt, and the charge and discharge electric current is 30mA/cm
2
The physical property of the absorbent charcoal material for preparing under the different activation temperatures of table 1 relatively
| Sequence number | Pyrolysis temperature ℃ | BET specific surface area m 2/g | Proportion g/cm 3 | Volumetric capacitance F/cm 3 | Gravimetric capacitance F/g |
| 1 | 450 | 420 | 0.76 | 55.3 | 72.8 |
| 2 | 500 | 633 | 0.74 | 67.7 | 91.5 |
| 3 | 550 | 955 | 0.72 | 85.0 | 118.0 |
| 4 | 600 | 1532 | 0.69 | 174.4 | 252.7 |
| 5 | 700 | 2045 | 0.61 | 172.7 | 283.1 |
| 6 | 800 | 2515 | 0.53 | 161.9 | 305.5 |
| 7 | 900 | 3127 | 0.45 | 144.9 | 322.0 |
Example two:
With coal, rice husk and resin respectively by example one same method preoxidation or coking.Through pulverizing,, obtain carbon material separately again by example one carbonizing treatment method.By example together quadrat method with carbon material and sodium hydroxide activator mix, under nitrogen protection, 550 ℃ of insulations, thermal treatment in 30 minutes obtains gac.These gac reusable heat water washings, oven dry and pulverizing, the gac that obtains being suitable for.The physical property of these gacs is as shown in table 2.The electric capacity of absorbent charcoal material records by the measuring method of example one.
The physical property of the absorbent charcoal material of table 2 different material preparation relatively
| Raw material | BET specific surface area m 2/g | Proportion g/cm 3 | Volumetric capacitance F/cm 3 | Gravimetric capacitance F/g |
| Coal | 854 | 0.69 | 65.8 | 95.4 |
| Rice husk | 1016 | 0.35 | 36.4 | 103.9 |
| Resin | 955 | 0.72 | 85.0 | 118.0 |
Example three:
Resin is handled by example one method coking, pulverizing, charing, obtained carbon material.Carbon material adopts different activators: water vapor, carbonic acid gas, sodium hydroxide and potassium hydroxide, under nitrogen protection, 600 ℃ of insulations thermal treatment in 30 minutes obtains gac.These gacs are pressed together quadrat method of example, the washing of reusable heat water, oven dry and pulverizing, the gac that obtains being suitable for.The physical property of these gacs is as shown in table 3.The electric capacity of absorbent charcoal material records by example one same measuring method.
The physical property of the absorbent charcoal material that the different Treatment with activating agent of table 3 are prepared relatively
| Activator | BET specific surface area m 2/g | Proportion g/cm 3 | Volumetric capacitance F/cm 3 | Gravimetric capacitance F/g |
| Water vapor | 1033 | 0.53 | 60.1 | 113.4 |
| Carbonic acid gas | 801 | 0.62 | 59.3 | 95.6 |
| Sodium hydroxide | 1532 | 0.69 | 174.4 | 252.7 |
| The hydrogen potassium hydride KH | 1320 | 0.51 | 92.2 | 180.7 |
The gac specific surface area that the present invention produced can reach 2000m
2More than/the g, proportion can reach 0.72g/cm
3More than.Gac with above-mentioned characteristic is made electrode of super capacitor, and its gravimetric capacitance reaches more than the 250F/g, and volumetric capacitance reaches 174F/cm
3More than.
Claims (5)
1. method for preparation of active carbon of making electrode of super capacitor, it is to be raw material with the resin, pass through coking, carbonization, activation treatment and comprise the gac that washing, oven dry, pulverizing aftertreatment obtain, it is characterized in that, the resin that is adopted is a resol, carrying out coking under 150～300 ℃ handled 3～5 hours, carbonizing matter carries out charing at 400～700 ℃ to be handled, obtain carbon material, with carbonic acid gas, or water vapour, or potassium hydroxide solution, or liquor zinci chloridi, or sodium hydroxide solution is promoting agent, carries out activation treatment at 450～900 ℃.
2. by the method for preparation of active carbon of the said making electrode of super capacitor of claim 1, it is characterized in that the coking treatment temp is 180～220 ℃.
3. by the method for preparation of active carbon of the said making electrode of super capacitor of claim 1, it is characterized in that the charing treatment temp is 500～600 ℃.
4. by the method for preparation of active carbon of the said making electrode of super capacitor of claim 1, it is characterized in that activating treatment temperature is 600～700 ℃.
5. by the method for preparation of active carbon of the said making electrode of super capacitor of claim 1, it is characterized in that activating treatment agent is a sodium hydroxide solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00118967 CN1117028C (en) | 2000-09-05 | 2000-09-05 | Process for preparing activated carbon to make electrode of super capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00118967 CN1117028C (en) | 2000-09-05 | 2000-09-05 | Process for preparing activated carbon to make electrode of super capacitor |
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| CN1291587A CN1291587A (en) | 2001-04-18 |
| CN1117028C true CN1117028C (en) | 2003-08-06 |
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| CN 00118967 Expired - Fee Related CN1117028C (en) | 2000-09-05 | 2000-09-05 | Process for preparing activated carbon to make electrode of super capacitor |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1307669C (en) * | 2001-11-02 | 2007-03-28 | 中国科学院上海冶金研究所 | Manufacture of high-voltage electrochemical capacitor |
| CN1319087C (en) * | 2002-08-19 | 2007-05-30 | 中国科学院山西煤炭化学研究所 | Method for increasing specific capacitance of active carbon electrode by carrying transition metal |
| CN100417590C (en) * | 2003-07-18 | 2008-09-10 | 中国科学院山西煤炭化学研究所 | Method for preparing spherical active cardon with base of resin |
| CN100348481C (en) * | 2005-10-05 | 2007-11-14 | 西南交通大学 | Production of active carbon material for capacitor electrode with double electric layers |
| US8524632B2 (en) * | 2010-01-22 | 2013-09-03 | Corning Incorporated | High-capacitance and low-oxygen porous carbon for EDLCs |
| CN101844765B (en) * | 2010-06-02 | 2012-01-11 | 天津大学 | Active carbon for preparing carbon electrode of super capacitor and preparation method thereof |
| CN102101668B (en) * | 2010-12-11 | 2012-05-23 | 河南理工大学 | Method for preparing activated carbon of high-specific capacitance super capacitor |
| CN103215056B (en) * | 2013-04-25 | 2015-03-04 | 太原理工大学 | Method for improving semicoke pore structure |
| CN103409853A (en) * | 2013-08-22 | 2013-11-27 | 吉林大学 | Method for preparing active carbon fiber material with energy storage characteristic from polyacrylonitrile-based pre-oxidized fiber and application of active carbon fiber material |
| CN104609419B (en) * | 2015-02-13 | 2016-10-05 | 洛阳月星新能源科技有限公司 | A kind of absorbent charcoal material, preparation method and ultracapacitor |
| CN107500291B (en) * | 2017-07-10 | 2019-10-18 | 吉林大学 | A kind of preparation method of lignin-base phenolic resin capacitance carbon |
| CN111217368B (en) * | 2020-02-17 | 2023-10-03 | 中钢集团鞍山热能研究院有限公司 | Production process and device of hard carbon anode material |
| TWI750722B (en) * | 2020-07-06 | 2021-12-21 | 巨鑫化學股份有限公司 | Manufacturing method of spherical phenol formaldehyde carbon |
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