CN1830769A - Preparation method of high superficial area porous carbon material - Google Patents
Preparation method of high superficial area porous carbon material Download PDFInfo
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- CN1830769A CN1830769A CNA2006100461075A CN200610046107A CN1830769A CN 1830769 A CN1830769 A CN 1830769A CN A2006100461075 A CNA2006100461075 A CN A2006100461075A CN 200610046107 A CN200610046107 A CN 200610046107A CN 1830769 A CN1830769 A CN 1830769A
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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
- Y02E60/10—Energy storage using batteries
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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
Abstract
A porous carbon with high specific surface area used as the electrode of super capacitor and lithium battery is prepared through proportionally dissolving resorcin, formaldehyde, and potassium (or sodium) hydroxide as catalyst in water, laying aside at 80-95 deg.C for 1-3 days to obtaining water-phase gel, drying, carbonifying at 650-900 deg.C for 30-180 min, water washing and drying.
Description
Technical field
The present invention relates to the electrode materials preparation field of relevant ultracapacitor, fuel cell, lithium cell and electro-adsorption device, the polycondensation that also belongs to aldehyde and phenol simultaneously prepares the technical field of high superficial area porous carbon material.
Background technology
Charcoal-aero gel is a kind of novel, porous, amorphous nano raw material of wood-charcoal material, compare with traditional absorbent charcoal material, charcoal-aero gel has good conductivity, specific surface area is big, the variable density scope is wide, pore size distribution concentrates on characteristics such as mesopore scope, is preparation high power density, high-energy-density ultracapacitor ideal electrode materials.But the key factor that limits the charcoal-aero gel commercial applications at present is that charcoal-aero gel complicated process of preparation, synthesis cycle are long.The raw material and the technology of existing preparation charcoal-aero gel mainly comprise:
1. Resorcinol is a raw material.US 4 997 804 (RW Pekala) is a raw material with Resorcinol and formaldehyde, and 90 ℃ of polymerase 17 skies form gel aqueous phase under the yellow soda ash katalysis, and gel aqueous phase is through acetone solvent replacement process, supercritical CO
2Drying can obtain organic aerogel, and further 1050 ℃ of charings obtain charcoal-aero gel under argon shield.The specific surface area of gained charcoal-aero gel is 400 ~ 1100m
2/ g.But this prepared cycle is long, and the supercritical drying drying process is comparatively complicated.
2. phenol is raw material.US 5 744 510 (RW Pekala) can obtain organic aerogel with phenol and furfural in pure phase-polymerization, and charing obtains charcoal-aero gel, density 0.2 ~ 1.0g/cm
3, specific surface area 350 ~ 1000m
2/ g.This technology is saved the solvent exchange process before the supercritical drying.
3. Phloroglucinol monomethyl ether is a raw material.With the Phloroglucinol monomethyl ether is that the polymerization under the two-step catalysis condition of raw material and formaldehyde can obtain the low density organic aerogel, and density only is 0.013g/cm after the charing
3(KJ Barral, et.al., J.Non-Cryst.Solids, 1998,225:46).But still comprise CO in this technological process
2Supercritical drying.
4. mixture cresol is a raw material.It is raw material that ZL03133416.4 (Li Wencui etc.) substitutes the part Resorcinol with mixture cresol, obtains hydrogel with oxymethylene polymerization under the alkaline catalysts effect; Hydrogel is through acetone displacement, supercritical CO
2Obtain organic aerogel after the drying; Organic aerogel obtains high-specific surface area and the charcoal-aero gel that is rich in mesopore through charing.This technology has superiority on cost of material, but does not solve the long problem of synthesis cycle.
5. Freeze Drying Technique.Adopt Freeze Drying Technique to replace supercritical drying can obtain the middle high resorcinol formaldehyde charcoal-aero gel of porosity, but charcoal-aero gel specific surface area that lyophilize obtains and pore volume are less than sample (H Tamon, et.a1., the Carbon of supercritical drying, 1999,37:2049; Drying Technology, 2001,19 (2): 313).
6. constant pressure and dry technology.US 5 420 168 (Mayer et.al.) is a raw material with Resorcinol and formaldehyde, by improving the reactant total content is 50%, while control catalyst concentration, the mol ratio that is phenol content and catalyzer is 200, can obtain wet gel through sol-gel process, this kind wet gel can be realized low pressure (about 0.1-1.0atm) drying through solvent exchange.Drying temperature is 20 ~ 50 ℃, depends on air velocity and drying temperature time of drying.
Summary of the invention
The purpose of this invention is to provide that a kind of preparation cycle is short, technological process is simple and the preparation method of lower-cost high superficial area porous carbon material.
Technical solution of the present invention is, a kind of preparation method of high superficial area porous carbon material, amount by changing Resorcinol and formaldehyde in the polymerization system and catalyst concentration are controlled specific surface area and the pore size distribution with modulation raw material of wood-charcoal material, promptly Resorcinol according to a certain ratio, formaldehyde and catalyzer are configured to solution, and the concentration of used formaldehyde solution is 37-40%.Wherein, Resorcinol and the formaldehyde mass percent in the aqueous solution is 10-50wt%, and the mol ratio of Resorcinol and formaldehyde is 1: 1-1: 3, and the mass ratio of catalyzer and Resorcinol is 0.5-4, catalyst system therefor is sodium hydroxide or potassium hydroxide.With the solution container of packing into, the sealing back is placed 12-72h down in 80-95 ℃, obtains gel aqueous phase, and gel aqueous phase obtains xerogel through 50-150 ℃ of normal pressure or after drying under reduced pressure 1-4 days; Xerogel is raised to 650-900 ℃ by room temperature under protection of inert gas, and temperature rise rate 1-10 ℃/min, and constant temperature 30-180min, obtain carbonization product.Described rare gas element is any in nitrogen, argon, the helium.Carbonization product is 6-7 through being washed to washings pH value; Washing back product to constant weight, obtains having the porous carbon material of high-specific surface area at 50-150 ℃ of normal pressure or drying under reduced pressure.
Realize that ultimate principle of the present invention is, the polymerization under the basic catalyst condition of Resorcinol and formaldehyde obtains having the gel aqueous phase of three-dimensional net structure, drying is after high temperature carbonization, and basic catalyst plays activation in carbonization process, finally obtain the porous carbon material of high-specific surface area.
Effect of the present invention and benefit be, the amount of reaction-ure mixture and ratio and catalyzer can prepare the raw material of wood-charcoal material with different specific surface areas in the polymerization system by changing.This method has that preparation cycle is short, technological process is simple and lower-cost characteristics.Gained raw material of wood-charcoal material is applicable to the electrode materials of making high power density, high-energy-density electrode material for super capacitor and fuel cell and lithium cell.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1: take by weighing 5.6g Resorcinol, 8.3g 37% formaldehyde solution, 15g deionized water and 11.2g potassium hydroxide respectively and be positioned over wiring solution-forming in the beaker of 50ml, in the sealed vessel of packing into.Be placed in 90 ℃ of baking ovens and placed 1 day, obtain gel aqueous phase.Place 120 ℃ of baking ovens to carry out constant pressure and dry 3 days gel aqueous phase, subsequently it is carried out charing.In the carbonization process with high-purity N
2Be protection gas, temperature rise rate is 3 ℃/min, and whole temperature is 700 ℃, constant temperature time 60min, and cooling back sample obtains the porous carbon material product after washing, drying.N
2The BET specific surface area of absorption test is 1583cm
2/ g, mean pore size 3.2nm, pore volume 0.668cm
3/ g.
Embodiment 2: change the potassium hydroxide amount among the embodiment 1 into 5.6g, other condition obtains porous carbon material with embodiment 1.N
2The BET specific surface area of absorption test is 522m
2/ g, mean pore size 4.4nm, pore volume 0.304cm
3/ g.
Embodiment 3: change the potassium hydroxide amount among the embodiment 1 into 22.4g, other condition obtains high superficial area porous carbon material with embodiment 1.N
2The BET specific surface area of absorption test is 2760m
2/ g, mean pore size 2.5nm, pore volume 1.347cm
3/ g.
Embodiment 4: change the whole temperature of the charing among the embodiment 1 into 900 ℃, other condition obtains high superficial area porous carbon material with embodiment 1.N
2The BET specific surface area of absorption test is 2041cm
2/ g, mean pore size 3.1nm, pore volume 1.027cm
3/ g.
Embodiment 5: change the whole temperature of the charing among the embodiment 1 into 650 ℃, other condition obtains high superficial area porous carbon material with embodiment 1.N
2The BET specific surface area of absorption test is 1531cm
2/ g, mean pore size 3.3nm, pore volume 0.651cm
3/ g.
Embodiment 6: the sample that obtains among the embodiment 1 was fully ground 300 mesh sieves, took by weighing raw material of wood-charcoal material 1.70g, acetylene black 0.20g and tetrafluoroethylene 0.10g by weight 85: 10: 5, mix the back and fully stir into paste with alcohol dampening, make the thick thin slice of 0.15-0.3 μ m on tabletting machine, determining 6 areas is 1cm
2Disk, under 10MPa, be pressed in and make pole piece on the nickel foam, itself and battery diaphragm are assembled into 3 sandwich type electrical condensers, be electrolytic solution with the 30%KOH aqueous solution, after in electrolytic solution, fully soaking, at 1mA/cm
2Test under the continuous current, the quality that obtains is 294F/g than electric capacity.
Claims (6)
1. the preparation method of a high superficial area porous carbon material, it is characterized in that, with the Resorcinol is raw material, in the presence of basic catalyst, get gel aqueous phase with oxymethylene polymerization, the gel aqueous phase drying, charing obtains high superficial area porous carbon material, preparation technology is: with Resorcinol, formaldehyde and basic catalyst and water mixing wiring solution-forming, pack in the container and sealing, under 80-95 ℃ of condition, place 12-72h, obtain gel aqueous phase, wherein, Resorcinol and the formaldehyde mass percent in solution is 10-50%, the mol ratio of Resorcinol and formaldehyde is 1: 1-1: 3, and the mass ratio of catalyzer and Resorcinol is 0.5-4; Gel aqueous phase was obtained xerogel at 50-150 ℃ of dry 1-4 days; With the xerogel charing that under protection of inert gas, heats up, be raised to 650-900 ℃ by room temperature, temperature rise rate 1-10 ℃/min, constant temperature 30-180min is 6-7 through being washed to washings pH value, obtains high superficial area porous carbon material 50-150 ℃ of drying.
2. the preparation method of a kind of high superficial area porous carbon material according to claim 1 is characterized in that, described basic catalyst is sodium hydroxide or potassium hydroxide.
3. the preparation method of a kind of high superficial area porous carbon material according to claim 1 is characterized in that, described rare gas element is nitrogen, argon or helium.
4. the preparation method of a kind of high superficial area porous carbon material according to claim 1 is characterized in that, the concentration of used formaldehyde solution is 37-40%.
5. the preparation method of a kind of high superficial area porous carbon material according to claim 1 is characterized in that, described gel aqueous phase makes xerogel through 50-150 ℃ of constant pressure and dry or drying under reduced pressure.
6. the preparation method of a kind of high superficial area porous carbon material according to claim 1 is characterized in that, described carbonization product is 6-7 through being washed to washings pH value; Washing back product is at 50-150 ℃ of normal pressure or drying under reduced pressure.
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101060037B (en) * | 2007-05-11 | 2010-05-19 | 合肥工业大学 | A manufacture method of carbon-based metal nitrides, and carbonide supercapacitance material |
| CN101948106A (en) * | 2010-09-28 | 2011-01-19 | 华东理工大学 | Preparation method of blocky porous carbon with high specific surface area |
| CN101980958A (en) * | 2008-04-02 | 2011-02-23 | 住友化学株式会社 | Carbon manufacturing method |
| CN101299397B (en) * | 2008-03-21 | 2011-08-03 | 中国科学院上海硅酸盐研究所 | Stephanoporate carbon electrode material and preparation method thereof |
| CN101613096B (en) * | 2008-06-25 | 2011-09-07 | 中国科学院大连化学物理研究所 | Method for preparing transition metal doped mesoporous carbon material |
| CN101604580B (en) * | 2009-04-03 | 2011-10-05 | 中国科学院上海硅酸盐研究所 | Method for preparing porous carbon electrode material by method decomposing monophyletic compound at one step |
| WO2012070013A1 (en) * | 2010-11-26 | 2012-05-31 | Basf Se | Process for manufacturing nitrogen-containing porous carbonaceous material |
| CN102515145A (en) * | 2011-12-27 | 2012-06-27 | 常州第六元素材料科技股份有限公司 | Preparation process for high specific surface porous carbon material |
| CN102592698A (en) * | 2010-11-23 | 2012-07-18 | 哈钦森公司 | Sulphur-modified porous carbon material, method for preparing same and uses thereof for storing and redelivering power |
| CN102976304A (en) * | 2012-11-16 | 2013-03-20 | 同济大学 | Preparation method of porous carbon nanosphere with controllable diameter |
| CN103915628A (en) * | 2013-01-06 | 2014-07-09 | 北京汉能创昱科技有限公司 | Making method of carbon composite electrode |
| CN105110313A (en) * | 2015-07-25 | 2015-12-02 | 复旦大学 | Polyimide-based composite carbon aerogel and preparation method therefor |
| CN105514438A (en) * | 2015-12-25 | 2016-04-20 | 清华大学深圳研究生院 | Sodium-ion battery electrode material, electrode and battery |
| CN106660797A (en) * | 2014-07-03 | 2017-05-10 | 东丽株式会社 | Porous carbon material and method for manufacturing porous carbon material |
| CN107473199A (en) * | 2016-06-08 | 2017-12-15 | 中国科学院金属研究所 | A kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application |
| CN108023093A (en) * | 2017-12-04 | 2018-05-11 | 奇瑞汽车股份有限公司 | A kind of preparation method of controllable tune hole carbon material and its application in lithium-sulfur cell |
| CN106688068B (en) * | 2014-07-10 | 2019-01-01 | 松下知识产权经营株式会社 | Capacitor |
| CN109384213A (en) * | 2018-11-23 | 2019-02-26 | 福建农林大学 | A kind of preparation method of phenol-urea-formaldehyde condensation copolymerization resin base N doping charcoal-aero gel |
| CN110127662A (en) * | 2019-05-26 | 2019-08-16 | 天津大学 | A method of assist charing Small molecule organic solvents to prepare porous charcoal using alkali metal |
| CN112938974A (en) * | 2021-03-23 | 2021-06-11 | 中国科学院化学研究所 | Ultrahigh-specific-surface-area porous carbon material and preparation method thereof |
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2006
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101060037B (en) * | 2007-05-11 | 2010-05-19 | 合肥工业大学 | A manufacture method of carbon-based metal nitrides, and carbonide supercapacitance material |
| CN101299397B (en) * | 2008-03-21 | 2011-08-03 | 中国科学院上海硅酸盐研究所 | Stephanoporate carbon electrode material and preparation method thereof |
| CN101980958A (en) * | 2008-04-02 | 2011-02-23 | 住友化学株式会社 | Carbon manufacturing method |
| CN101613096B (en) * | 2008-06-25 | 2011-09-07 | 中国科学院大连化学物理研究所 | Method for preparing transition metal doped mesoporous carbon material |
| CN101604580B (en) * | 2009-04-03 | 2011-10-05 | 中国科学院上海硅酸盐研究所 | Method for preparing porous carbon electrode material by method decomposing monophyletic compound at one step |
| CN101948106A (en) * | 2010-09-28 | 2011-01-19 | 华东理工大学 | Preparation method of blocky porous carbon with high specific surface area |
| CN101948106B (en) * | 2010-09-28 | 2013-03-27 | 华东理工大学 | Preparation method of blocky porous carbon with high specific surface area |
| CN102592698A (en) * | 2010-11-23 | 2012-07-18 | 哈钦森公司 | Sulphur-modified porous carbon material, method for preparing same and uses thereof for storing and redelivering power |
| CN102592698B (en) * | 2010-11-23 | 2016-06-01 | 哈钦森公司 | The modified Integrate porous carbon-based material of sulfur, its preparation method, and application thereof |
| WO2012070013A1 (en) * | 2010-11-26 | 2012-05-31 | Basf Se | Process for manufacturing nitrogen-containing porous carbonaceous material |
| CN102515145A (en) * | 2011-12-27 | 2012-06-27 | 常州第六元素材料科技股份有限公司 | Preparation process for high specific surface porous carbon material |
| CN102976304B (en) * | 2012-11-16 | 2014-07-16 | 同济大学 | Preparation method of porous carbon nanosphere with controllable diameter |
| CN102976304A (en) * | 2012-11-16 | 2013-03-20 | 同济大学 | Preparation method of porous carbon nanosphere with controllable diameter |
| CN103915628B (en) * | 2013-01-06 | 2017-09-12 | 北京创昱科技有限公司 | A kind of preparation method of carbon composite anode |
| CN103915628A (en) * | 2013-01-06 | 2014-07-09 | 北京汉能创昱科技有限公司 | Making method of carbon composite electrode |
| CN106660797A (en) * | 2014-07-03 | 2017-05-10 | 东丽株式会社 | Porous carbon material and method for manufacturing porous carbon material |
| CN106660797B (en) * | 2014-07-03 | 2019-07-12 | 东丽株式会社 | The manufacturing method of Porous carbon material and Porous carbon material |
| CN106688068B (en) * | 2014-07-10 | 2019-01-01 | 松下知识产权经营株式会社 | Capacitor |
| CN105110313A (en) * | 2015-07-25 | 2015-12-02 | 复旦大学 | Polyimide-based composite carbon aerogel and preparation method therefor |
| CN105514438A (en) * | 2015-12-25 | 2016-04-20 | 清华大学深圳研究生院 | Sodium-ion battery electrode material, electrode and battery |
| CN107473199A (en) * | 2016-06-08 | 2017-12-15 | 中国科学院金属研究所 | A kind of high intensity large scale bulk charcoal-aero gel and its preparation method and application |
| CN108023093A (en) * | 2017-12-04 | 2018-05-11 | 奇瑞汽车股份有限公司 | A kind of preparation method of controllable tune hole carbon material and its application in lithium-sulfur cell |
| CN109384213A (en) * | 2018-11-23 | 2019-02-26 | 福建农林大学 | A kind of preparation method of phenol-urea-formaldehyde condensation copolymerization resin base N doping charcoal-aero gel |
| CN110127662A (en) * | 2019-05-26 | 2019-08-16 | 天津大学 | A method of assist charing Small molecule organic solvents to prepare porous charcoal using alkali metal |
| CN110127662B (en) * | 2019-05-26 | 2022-02-01 | 天津大学 | Method for preparing porous carbon by using alkali metal-assisted carbonization small-molecule organic solvent |
| CN112938974A (en) * | 2021-03-23 | 2021-06-11 | 中国科学院化学研究所 | Ultrahigh-specific-surface-area porous carbon material and preparation method thereof |
| CN112938974B (en) * | 2021-03-23 | 2022-06-14 | 中国科学院化学研究所 | Ultrahigh-specific-surface-area porous carbon material and preparation method thereof |
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