CN1872674A - Method for preparing active mesopore carbon with high specific surface area in use for electrochemical capacitor - Google Patents
Method for preparing active mesopore carbon with high specific surface area in use for electrochemical capacitor Download PDFInfo
- Publication number
- CN1872674A CN1872674A CNA2006100193211A CN200610019321A CN1872674A CN 1872674 A CN1872674 A CN 1872674A CN A2006100193211 A CNA2006100193211 A CN A2006100193211A CN 200610019321 A CN200610019321 A CN 200610019321A CN 1872674 A CN1872674 A CN 1872674A
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- China
- Prior art keywords
- specific surface
- surface area
- high specific
- activation
- petroleum coke
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000003990 capacitor Substances 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 title description 2
- 230000004913 activation Effects 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000002006 petroleum coke Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims abstract 2
- 238000002791 soaking Methods 0.000 claims abstract 2
- 238000005406 washing Methods 0.000 claims abstract 2
- 230000007935 neutral effect Effects 0.000 abstract 1
- 239000000571 coke Substances 0.000 description 12
- 239000011148 porous material Substances 0.000 description 9
- 238000009413 insulation Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000012047 saturated solution Substances 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000012190 activator Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007420 reactivation Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- 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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- Carbon And Carbon Compounds (AREA)
Abstract
一种电化学电容器用高比表面积中孔活性炭的制备方法，它是以石油焦为原料，其特征是制备工艺步骤为：先将石油焦研磨到80～150目，然后按照质量比为KOH∶石油焦＝4～6的比例将二者混合，放入活化炉中并先于400～ 500℃保温1～2h进行预处理，再升温到750～850℃进行活化，活化1.5～2.5h后，冷却、研磨、用去离子水浸泡并水洗至中性、干燥得到高比表面积中孔活性炭。A method for preparing mesoporous activated carbon with a high specific surface area for electrochemical capacitors, which uses petroleum coke as a raw material, and is characterized in that the preparation process steps are as follows: firstly grind the petroleum coke to 80-150 mesh, and then KOH according to the mass ratio: Petroleum coke = 4~6, mix the two, put them into the activation furnace and first heat at 400~500°C for 1~2h for pretreatment, then raise the temperature to 750~850°C for activation, after activation for 1.5~2.5h, Cooling, grinding, soaking with deionized water and washing until neutral, drying to obtain high specific surface area mesoporous activated carbon.
Description
Technical field
The present invention relates to a kind of preparation method of high specific surface area in use for electrochemical capacitor mesopore activated carbon.
Background technology
Electrochemical capacitor enjoys the concern of countries in the world government and enterprise with enormous and latent market owing to being with a wide range of applications.The various gacs that are used for electrochemical capacitor at present mainly are the high specific surface micro-pore charcoals, and not only the specific surface area utilization ratio was low when such gac was used as electrochemical capacitor electrode material, and power characteristic is poor.Improve the mesopore content of gac, not only help improving the specific surface area utilization ratio of gac, thereby improve its specific volume, and help improving its power characteristic.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high specific surface area in use for electrochemical capacitor mesopore activated carbon, it is to be the process of active carbon as electrochemical capacitor electrode material that feedstock production has high-specific surface area and high mesopore content simultaneously with the refinery coke.
The present invention is achieved like this, it is to be raw material with the refinery coke, it is characterized in that step of preparation process is: earlier refinery coke is ground to 80～150 orders, be KOH according to mass ratio then: the ratio of refinery coke=4～6 is mixed the two, put into activation furnace and carry out pre-treatment prior to 400～500 ℃ of insulation 1～2h, being warmed up to 750～850 ℃ again activates, behind activation 1.5～2.5h, cooling, grind, with deionized water soak and be washed to neutrality, it is dry that just can to obtain specific surface area be 1500～2000m
2/ g, mesopore volume are 0.4～0.8mL/g, and mesopore content is 50～70% high-specific surface area mesopore activated carbon.
The present invention grinds the broken method of dipping that adopts later at refinery coke to add activator KOH, the refinery coke that will be impregnated with KOH then carries out pre-treatment in 400～500 ℃, next activate, realize radially pore-creating and the laterally control of reaming by adjusting in the reactivation process, thereby can prepare the gac that has high-specific surface area and high mesopore content simultaneously activation temperature and soak time.
Advantage of the present invention is: the gac mesopore prosperity of preparation, and mesopore volume accounts for 50%～70% of total pore volume; Pore size distribution is very narrow, and the pore volume in the following hole of 10nm accounts for more than 90% of total pore volume; Mean pore size is 2～3nm, has guaranteed that gac has high-specific surface area when having high mesopore content.
When the electrochemical capacitor electrode material, such gac is owing to have high-specific surface area and high-specific surface area utilization ratio, thereby has high specific volume; Simultaneously, because such gac has high mesopore content, so have excellent power characteristic, when high current charge-discharge, the specific volume decay is very little, can demonstrate fully the high-energy-density of electrochemical capacitor and the characteristic of high power density.
Table 1 is based on the performance of the activated carbon product of preparation technology parameter of the present invention
| Title | Index |
| Iodine sorption value (mL/g) Yamamoto Methylene Blue ZF adsorptive value (mL/g) specific surface area (m 2/ g) mesopore content (%) mean pore size (nm) | 2200～2800 400～630 1500～2000 50～70 2～3 |
Embodiment
Embodiment 1
With the refinery coke fragmentation, sieving out particle diameter is 100～120 order powder.According to mass ratio is KOH: the ratio of refinery coke=5 takes by weighing 250g KOH and is configured to saturated solution, the 50g petroleum coke powder is poured in the KOH solution soaked 24h, and refinery coke is put into activation furnace together with KOH solution.At N
2Protection down is warmed up to 450 ℃ with the speed of 10 ℃/min, and insulation 1h.And then be warmed up to 800 ℃ with the speed of 10 ℃/min, insulation 2h.The gac cooling that experiment is obtained, grind, soak and be washed to neutrality, drying with deionized water.
The performance of the activated carbon product of preparation:
Iodine number mg/g:2540
Yamamoto Methylene Blue ZF mg/g:540
Specific surface area m
2/ g:1733
Mean pore size nm:2.37
Mesopore content: 60.6%
Embodiment 2
With the refinery coke fragmentation, sieving out particle diameter is 100～120 order powder.According to mass ratio is KOH: the ratio of refinery coke=6 takes by weighing 300g KOH and is configured to saturated solution, the 50g petroleum coke powder is poured in the KOH solution soaked 24h, and refinery coke is put into activation furnace together with KOH solution.At N
2Protection down is warmed up to 500 ℃ with the speed of 10 ℃/min, and insulation 1h.And then be warmed up to 750 ℃ with the speed of 10 ℃/min, insulation 1.5h.The gac cooling that experiment is obtained, grind, soak and be washed to neutrality, drying with deionized water.
The performance of the activated carbon product of preparation:
Iodine number mg/g:2710
Yamamoto Methylene Blue ZF mg/g:410
Specific surface area m
2/ g:2340
Mean pore size nm:1.87
Mesopore content: 52%
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100193211A CN1872674A (en) | 2006-06-09 | 2006-06-09 | Method for preparing active mesopore carbon with high specific surface area in use for electrochemical capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006100193211A CN1872674A (en) | 2006-06-09 | 2006-06-09 | Method for preparing active mesopore carbon with high specific surface area in use for electrochemical capacitor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1872674A true CN1872674A (en) | 2006-12-06 |
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ID=37483305
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006100193211A Pending CN1872674A (en) | 2006-06-09 | 2006-06-09 | Method for preparing active mesopore carbon with high specific surface area in use for electrochemical capacitor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1872674A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101950683A (en) * | 2010-09-09 | 2011-01-19 | 江西财经大学 | Preparation method of semi-spherical active carbon electrode material of super capacitor |
| CN101964259A (en) * | 2010-10-27 | 2011-02-02 | 扬州大学 | Method for preparing super capacitor carbon electrode material by using high sulfur petroleum coke |
| CN101439857B (en) * | 2008-12-11 | 2011-03-02 | 武汉科技大学 | Mesoporous activated carbon and preparation process thereof |
| CN102101668A (en) * | 2010-12-11 | 2011-06-22 | 河南理工大学 | Method for preparing activated carbon of high-specific capacitance super capacitor |
| CN102214514A (en) * | 2011-03-21 | 2011-10-12 | 中南大学 | Production method of high-specific-capacitance activated carbon electrode material for super capacitor |
| CN102254699A (en) * | 2011-05-13 | 2011-11-23 | 湖南耐普恩电能科技有限公司 | Pretreatment technology for super capacitor electrode material and manufacturing method of electrode |
| CN102295283A (en) * | 2011-06-13 | 2011-12-28 | 福建省龙岩龙能粉煤灰综合利用有限公司 | Method for preparing activated carbon of high specific surface area through alkali activation |
| CN101423210B (en) * | 2008-10-20 | 2012-05-30 | 浙江富来森竹炭有限公司 | A kind of manufacture method of activated carbon for polar electrode using biomass material as raw material |
| CN102963876A (en) * | 2012-10-31 | 2013-03-13 | 同济大学 | Preparation method of microporous carbon material |
| CN108946722A (en) * | 2018-07-16 | 2018-12-07 | 深圳市环球绿地新材料有限公司 | The preparation method and its product and purposes of the controllable spherical activated charcoal in aperture |
| 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 |
| CN116062912A (en) * | 2022-12-21 | 2023-05-05 | 华南理工大学 | A kind of alkali-treated woody carbon self-supporting electrode material and its preparation method and application |
-
2006
- 2006-06-09 CN CNA2006100193211A patent/CN1872674A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423210B (en) * | 2008-10-20 | 2012-05-30 | 浙江富来森竹炭有限公司 | A kind of manufacture method of activated carbon for polar electrode using biomass material as raw material |
| CN101439857B (en) * | 2008-12-11 | 2011-03-02 | 武汉科技大学 | Mesoporous activated carbon and preparation process thereof |
| CN101950683B (en) * | 2010-09-09 | 2012-07-11 | 江西财经大学 | Preparation method of hemispherical activated carbon electrode material for supercapacitor |
| CN101950683A (en) * | 2010-09-09 | 2011-01-19 | 江西财经大学 | Preparation method of semi-spherical active carbon electrode material of super capacitor |
| CN101964259A (en) * | 2010-10-27 | 2011-02-02 | 扬州大学 | Method for preparing super capacitor carbon electrode material by using high sulfur petroleum coke |
| CN102101668A (en) * | 2010-12-11 | 2011-06-22 | 河南理工大学 | Method for preparing activated carbon of high-specific capacitance super capacitor |
| CN102214514A (en) * | 2011-03-21 | 2011-10-12 | 中南大学 | Production method of high-specific-capacitance activated carbon electrode material for super capacitor |
| CN102254699A (en) * | 2011-05-13 | 2011-11-23 | 湖南耐普恩电能科技有限公司 | Pretreatment technology for super capacitor electrode material and manufacturing method of electrode |
| CN102295283A (en) * | 2011-06-13 | 2011-12-28 | 福建省龙岩龙能粉煤灰综合利用有限公司 | Method for preparing activated carbon of high specific surface area through alkali activation |
| CN102963876A (en) * | 2012-10-31 | 2013-03-13 | 同济大学 | Preparation method of microporous carbon material |
| 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 |
| CN108946722A (en) * | 2018-07-16 | 2018-12-07 | 深圳市环球绿地新材料有限公司 | The preparation method and its product and purposes of the controllable spherical activated charcoal in aperture |
| CN116062912A (en) * | 2022-12-21 | 2023-05-05 | 华南理工大学 | A kind of alkali-treated woody carbon self-supporting electrode material and its preparation method and application |
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Open date: 20061206 |