CN107190366A - The preparation method of ultracapacitor N doping porous carbon fiber - Google Patents
The preparation method of ultracapacitor N doping porous carbon fiber Download PDFInfo
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- CN107190366A CN107190366A CN201710545539.9A CN201710545539A CN107190366A CN 107190366 A CN107190366 A CN 107190366A CN 201710545539 A CN201710545539 A CN 201710545539A CN 107190366 A CN107190366 A CN 107190366A
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- carbon fiber
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- doping porous
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 47
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 47
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 230000003213 activating effect Effects 0.000 claims abstract description 13
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 13
- 229920000742 Cotton Polymers 0.000 claims abstract description 11
- 238000001994 activation Methods 0.000 claims abstract description 11
- 239000000835 fiber Substances 0.000 claims abstract description 8
- 238000003763 carbonization Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229920000877 Melamine resin Polymers 0.000 claims description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000012190 activator Substances 0.000 claims description 2
- 210000002700 urine Anatomy 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 230000004913 activation Effects 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 abstract 1
- 230000014759 maintenance of location Effects 0.000 description 8
- 239000011736 potassium bicarbonate Substances 0.000 description 8
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 8
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 8
- 239000004202 carbamide Substances 0.000 description 7
- 230000008859 change Effects 0.000 description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 7
- 229920002239 polyacrylonitrile Polymers 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 5
- 150000001412 amines Chemical class 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000009987 spinning Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000004640 Melamine resin Substances 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- -1 dimethyl methyl Chemical group 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000010041 electrostatic spinning Methods 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 125000004355 nitrogen functional group Chemical group 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical group 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- XKJCHHZQLQNZHY-UHFFFAOYSA-N phthalimide Chemical compound C1=CC=C2C(=O)NC(=O)C2=C1 XKJCHHZQLQNZHY-UHFFFAOYSA-N 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/14—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with organic compounds, e.g. macromolecular compounds
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/40—Fibres
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of new method using cotton as carbon source processing machinery ultracapacitor N doping porous carbon fiber of good performance.Specifically related to one kind is using cotton as raw material, by carbonization, the introducing of nitrogen source, with reference to the new method of chemical activation method processing machinery ultracapacitor porous carbon fiber of good performance.The present invention includes comprising the following steps that:It is fiber first by cotton high temperature cabonization, carbon fiber is mixed with activating reagent, nitrogen source by certain mass ratio, dried after adding appropriate distillation water retting certain time thereto again, then activation process certain time in tube furnace, solid is washed, dried, and obtains ultracapacitor N doping porous carbon fiber.
Description
Technical field
The present invention relates to a kind of preparation method of ultracapacitor with N doping porous carbon fiber, and in particular to one kind is first
Cotton carbonization is prepared into carbon fiber, then it is mixed with nitrogen source, activating reagent, high-temperature activation prepares ultracapacitor N doping
The new method of porous carbon fiber.
Background technology
Ultracapacitor due to charge-discharge velocity is fast, high energy force density and power density, excellent cyclical stability
And high stability and as researchers extensive concern energy storage device.According to the different super capacitors of energy storage mechanism
Device can be divided into two kinds of capacitors of electric double layer and fake capacitance, and electrode material is to determine one of key factor of performance of the supercapacitor.
Porous carbon is due to big specific surface area, stable chemical property, big pore volume, connection and homogeneous duct, adjustable
Many advantages, such as aperture and as with application prospect electrode material for super capacitor.At present, applied to ultracapacitor
Porous carbon materials have many kinds, such as spherical carbon, graininess carbon, fibrous carbon etc..Wherein, porous carbon fiber light weight, stretching is strong
Degree and excellent heat stability, its surface distributed abundant pore structure, it is possible to increase its contact area with electrolyte, shortens
Ion transmission path.Energy storage efficiency is improved, these properties promote porous carbon fiber and are widely studied.
At present, preparing the presoma of carbon fiber mainly has pitch, polyacrylonitrile, phenolic resin etc., and it is all from coal and stone
Extracted in oil, belong to non-renewable resources.It is fine that patent CN106521717A discloses a kind of high specific surface area porous carbon
The preparation method of dimension, step is as follows:By the spinning solution of polyacrylonitrile, pore creating material (silica) and the dimethyl methyl phthalein amine of N, N mono-
Be carbonized after electrostatic spinning, high-ratio surface porous carbon fiber is obtained after thermokalite is washed, dried.Patent CN103806129A is public
A kind of N doping porous carbon fiber material and preparation method and application is opened, its step is as follows:(1) nitrogen source and carbon source are dissolved
Yu Shuizhong, through staticly settling, being filtrated to get the predecessor that the nitrogen source is combined with the carbon source;The nitrogen source is melamine
And/or cyanuric acid;The carbon source is organic acid and/or organic amine;(2) predecessor is placed in tube furnace and be calcined
Porous carbon fiber is obtained, it has the chemical property that high specific surface area is become reconciled.Patent CN103225135A discloses one kind
Porous carbon fiber and preparation method thereof.Its step is as follows:Will be (polyacrylonitrile, poly- by pore creating material (calcium carbonate), high molecular polymer
Phthalimide, pitch, polyvinyl alcohol, polyethylene adjoin at least one of pyrrolidone and phenolic resin) and organic solvent (N, N mono- or two
Methyl first phthalein amine, N monomethyls adjoin at least one of pyrrolidone and dimethyl alum) composition spinning solution carry out spinning after be carbonized
Pickling, obtains the porous carbon fiber.Patent CN105671692A discloses the Nitrogen-rich porous carbon fibre that a kind of melamine resin is modified
Tie up the preparation method of electrode material.It is with melamine and formaldehyde synthesis melamine resin;Polyacrylonitrile is dissolved in N, N mono- or two
In methyl first phthalein amine, add melamine resin and be configured to spinning solution;MF/PAN composite fiber precursors are made by electrostatic spinning;Will
MF/PAN composite fibres, which are pre-oxidized, are carbonized etc., is thermally treated resulting in rich nitrogen carbon fiber;Electrode of super capacitor is made in NCNF,
With preferable performance.
Above patent prepares porous carbon fiber by presoma of non-renewable resources, and its cost is higher, is unfavorable for holding
Supervention exhibition.Therefore porous carbon fiber is prepared by raw material of reproducible biomass has important Research Significance.Cotton is a kind of
The natural biomass resource with fibre structure, remains to keep fibre structure, while having good mechanical performance after carbonization.
Therefore, using cotton as raw material, prepared by way of carbonization, activation, N doping with high-specific surface area, containing certain nitrogen function
Group, the electrode material for super capacitor of good mechanical properties have certain researching value.
This patent is that, using cotton as raw material, it is fiber to be carbonized, then by the introducing of nitrogen source, is prepared with reference to chemical activation
The ultracapacitor of satisfactory mechanical property N doping porous carbon fiber.This route raw material wide material sources, simple synthetic method, lead to
The hole development degree and the doping of nitrogen functional group of activating reagent and the addition control porous carbon fiber of nitrogen source are overregulated, most
Whole processing machinery ultracapacitor of good performance N doping porous carbon fiber.
The content of the invention
It is an object of the present invention to provide one kind using cotton as carbon source processing machinery ultracapacitor N doping of good performance
The new method of porous carbon fiber.
The present invention is fiber first by cotton high temperature cabonization, by carbon fiber and activating reagent, nitrogen source in mass ratio 1: 3: 2~
1: 6: 5 (g/g/g) mix, add thereto appropriate distilled water be well mixed, by after impregnation mixture 14h in 110 DEG C of baking ovens
Dry 6h, by mixture in 700~1000 DEG C of tube furnaces 0.5~2h of activation process, solid washing, dry, obtained nitrogen mixes
Miscellaneous porous carbon fiber carries out electrochemical property test.
It is a feature of the present invention that:The activator is the mixture or saleratus and hydrogen of saleratus and potassium hydroxide
The mixture of sodium oxide molybdena.
It is a feature of the present invention that:The nitrogen source is urea or melamine.
Embodiment
Embodiment 1:Cotton is carbonized 1h in tube furnace at 800 DEG C first, by obtained carbon fiber and activating reagent
(KHCO3: KOH mass ratio be 1: 2), urea in mass ratio 1: 4: 2 (g/g/g) mixing, add thereto appropriate distilled water mix
Close uniform, 6h will be dried after impregnation mixture 14h in 110 DEG C of baking ovens, by mixture in 800 DEG C of tube furnaces activation process
1h, solid washing, dry, obtained N doping porous carbon fiber progress electrochemical property test, with 6mol/L potassium hydroxide
For electrolyte, specific capacity is measured for 306F/g, and 5000 capability retentions of circulation are 96% or so.
Embodiment 2:Change carbon fiber and activating reagent (KHCO3: KOH mass ratio is 1: 2), the mass ratio 1: 5 of urea:
2 (g/g/g), other conditions be the same as Example 1, the specific capacitance of obtained N doping porous carbon fiber is 334F/g, is circulated 5000 times
Capability retention is 97% or so.
Embodiment 3:Change carbon fiber and activating reagent (KHCO3: KOH mass ratio is 1: 2), the mass ratio 1: 6 of urea:
3 (g/g/g), other conditions be the same as Example 1, the specific capacitance of obtained N doping porous carbon fiber is 313F/g, is circulated 5000 times
Capability retention is 97% or so.
Embodiment 4:Change carbon fiber and activating reagent (KHCO3: 3), the mass ratio 1: 5 of urea NaOH mass ratio is 1:
: 2 (g/g/g), other conditions be the same as Example 1, the specific capacitance of obtained N doping porous carbon fiber is 320F/g, is circulated 5000 times
Capability retention is 97% or so.
Embodiment 5:Change carbon fiber and activating reagent (KHCO3: 3), the mass ratio 1: 6 of urea NaOH mass ratio is 1:
: 2 (g/g/g), other conditions be the same as Example 1, the specific capacitance of obtained N doping porous carbon fiber is 302F/g, is circulated 5000 times
Capability retention is 96% or so.
Embodiment 6:Change carbon fiber and activating reagent (KHCO3: 3), the quality of melamine NaOH mass ratio is 1:
Than 1: 5: 2 (g/g/g), by mixture in 900 DEG C of tube furnaces activation process 1h, other conditions be the same as Example 1, obtained nitrogen mixes
The specific capacitance of miscellaneous porous carbon fiber is 298F/g, and 5000 capability retentions of circulation are 97% or so.
Embodiment 7:Change carbon fiber and activating reagent (KHCO3: 3), the mass ratio of melamine KOH mass ratio is 1:
1: 5: 2 (g/g/g), by mixture in 800 DEG C of tube furnaces activation process 2h, other conditions be the same as Example 1, obtained N doping
The specific capacitance of porous carbon fiber is 315F/g, and 5000 capability retentions of circulation are 97% or so.
Embodiment 8:Change carbon fiber and activating reagent (KHCO3: KOH mass ratio is 1: 3), the mass ratio 1: 5 of urea:
3 (g/g/g), by mixture in 800 DEG C of tube furnaces activation process 1.5h, other conditions be the same as Example 1, obtained N doping is more
The specific capacitance of hole carbon fiber is 332F/g, and 5000 capability retentions of circulation are 97% or so.
Claims (3)
1. a kind of ultracapacitor preparation method of N doping porous carbon fiber, it is comprised the following steps that:It is first that cotton is high
Temperature carbonization is fiber, and carbon fiber is mixed with activating reagent, nitrogen source in mass ratio 1: 3: 2~1: 6: 5 (g/g/g), is added thereto
Enter appropriate distilled water to be well mixed, 6h will be dried after impregnation mixture 14h in 110 DEG C of baking ovens, by mixture 700~1000
0.5~2h of activation process in DEG C tube furnace, solid washing, is dried, and obtained N doping porous carbon fiber carries out chemical property
Test.
2. a kind of preparation method of N doping porous carbon fiber as claimed in claim 1, it is characterised in that:The activator is
The mixture or saleratus and the mixture of sodium hydroxide of saleratus and potassium hydroxide.
3. a kind of preparation method of N doping porous carbon fiber as claimed in claim 1, it is characterised in that:The nitrogen source is urine
Element or melamine.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108103616A (en) * | 2018-01-12 | 2018-06-01 | 北京林业大学 | A kind of preparation method of the lignin-base carbon fibre composite of N doping |
CN108455597A (en) * | 2018-05-12 | 2018-08-28 | 中国科学院新疆理化技术研究所 | A kind of method and application preparing N doping porous carbon using cotton seed hulls as raw material |
CN108726503A (en) * | 2018-09-04 | 2018-11-02 | 南京农业大学 | A kind of porous carbon materials Ammonia reforming apparatus |
CN109473686A (en) * | 2018-12-26 | 2019-03-15 | 宁波石墨烯创新中心有限公司 | It is a kind of with biomass cotton be carbon-based catalyst and its preparation method and application |
CN110517900A (en) * | 2019-09-12 | 2019-11-29 | 四川轻化工大学 | A kind of preparation method of supercapacitor N doping low temperature carbon nanofiber electrode material |
CN111517306A (en) * | 2020-04-29 | 2020-08-11 | 内蒙古民族大学 | Graphene-like/biomass carbon fiber aerogel and preparation method and application thereof |
CN113308879A (en) * | 2021-05-26 | 2021-08-27 | 河南工业大学 | By using g-C3N4Preparation method of modified carbon fiber immobilized carrier |
CN115467159A (en) * | 2022-09-06 | 2022-12-13 | 昆明云大新能源有限公司 | In-situ etching nitrogen-doped modified carbon cloth and preparation method and application thereof |
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CN103215691A (en) * | 2012-12-15 | 2013-07-24 | 王滨 | Method for preparing hollow structure carbon fibers by using cotton as raw material |
CN103332677A (en) * | 2013-07-12 | 2013-10-02 | 天津工业大学 | Method for preparing biomass carbon-based composite energy storage material by utilizing plant fiber |
CN106517197A (en) * | 2016-11-14 | 2017-03-22 | 天津工业大学 | Method for preparing nitrogen-doped porous carbon material for supercapacitor |
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