CN107190367A - The preparation method of nitrogen sulphur codope porous carbon fiber - Google Patents
The preparation method of nitrogen sulphur codope porous carbon fiber Download PDFInfo
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- CN107190367A CN107190367A CN201710545876.8A CN201710545876A CN107190367A CN 107190367 A CN107190367 A CN 107190367A CN 201710545876 A CN201710545876 A CN 201710545876A CN 107190367 A CN107190367 A CN 107190367A
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- carbon fiber
- porous carbon
- nitrogen sulphur
- sulphur codope
- nitrogen
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- PFRUBEOIWWEFOL-UHFFFAOYSA-N [N].[S] Chemical compound [N].[S] PFRUBEOIWWEFOL-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 35
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 35
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000003213 activating effect Effects 0.000 claims abstract description 12
- 238000001994 activation Methods 0.000 claims abstract description 12
- 229920000742 Cotton Polymers 0.000 claims abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000835 fiber Substances 0.000 claims abstract description 6
- 238000003763 carbonization Methods 0.000 claims abstract description 5
- 230000004913 activation Effects 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 20
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 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
- 239000003795 chemical substances by application Substances 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 11
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 4
- 238000004821 distillation Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 10
- 239000005864 Sulphur Substances 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- 239000003575 carbonaceous material Substances 0.000 description 9
- 230000014759 maintenance of location Effects 0.000 description 8
- 239000003990 capacitor Substances 0.000 description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000011736 potassium bicarbonate Substances 0.000 description 5
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 5
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229920000767 polyaniline Polymers 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- -1 Amino phenols Chemical class 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- DWNBOPVKNPVNQG-LURJTMIESA-N (2s)-4-hydroxy-2-(propylamino)butanoic acid Chemical class CCCN[C@H](C(O)=O)CCO DWNBOPVKNPVNQG-LURJTMIESA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 241000219071 Malvaceae Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000010583 slow cooling Methods 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
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
- 230000010148 water-pollination Effects 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 OR LIGHT-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 OR LIGHT-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 OR LIGHT-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 OR LIGHT-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
Abstract
The invention discloses a kind of preparation method using cotton as carbon source processing machinery ultracapacitor nitrogen sulphur codope porous carbon fiber of good performance.Specifically related to one kind is using cotton as raw material, by carbonization, the introducing of nitrogen sulphur, 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 sulfur compound 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 nitrogen sulphur codope porous carbon fiber.
Description
Technical field
The present invention relates to a kind of preparation method of nitrogen sulphur codope porous carbon fiber, and in particular to one kind is first by cotton carbon
Change prepares carbon fiber, then it is mixed with nitrogen, sulphur source, activating reagent, and high-temperature process prepares ultracapacitor nitrogen sulphur codope
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 widely used in surpassing due to many merits such as chemical property is stable, specific surface area is big, hole is flourishing, aperture is adjustable
Level capacitor electrode material.At present, the porous carbon materials applied to ultracapacitor have many kinds, such as spherical carbon, graininess carbon,
Fibrous carbon etc..Wherein, porous carbon fiber light weight, tensile strength and excellent heat stability, its surface distributed abundant hole
Gap 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 is widely studied.Achievement in research shows simultaneously, and hetero atom (N, B, P, S, F, Ni, Co etc.) doping is having for row
The path of the lifting carbon material chemical property of effect.For example, in capacitor electrode material field, the doping of nitrogen element sulphur can lead to
The electronic receipt or supply characteristics of influence carbon material are crossed, the formation of electric double layer is influenceed.In addition, the doping of nitrogen can also strengthen
The electric conductivity of carbon material, promotes the fast transferring of ion, fake capacitance is introduced, so as to improve carbon material in electrode of super capacitor material
Performance on material.Therefore preparing the porous carbon materials of nitrogen sulphur codope has important researching value.
Patent CN105931855A discloses a kind of conjunction of ultracapacitor nitrogen sulphur codope carbon-polyaniline composite material
Into method.It is related to aqua-solution method and synthesizes poly- (aniline-instigate fen) composite, high temperature pyrolytic cracking (HTP) synthetic nitrogen sulphur codope carbon materials
Material, chemical oxidization method synthetic nitrogen sulphur codope carbon-polyaniline composite material and the research for being used for ultracapacitor, including following step
Suddenly：Prepare poly- (aniline one instigates fen) composite, prepare nitrogen sulphur codope carbon material, to prepare nitrogen sulphur codope carbon-polyaniline multiple
Condensation material electrode.The beneficial effects of the invention are as follows：Composite possesses more preferable electric conductivity, smaller electrode resistance, preferably
Capacitive property, and show more preferable cyclical stability.Patent CN105776178A discloses one kind and utilizes DCL/Direct coal liquefaction weight
Nitrogen sulphur codope porous charcoal of organic point of preparation of matter and its preparation method and application.This method comprises the following steps：(1) it is coal is straight
Liquefaction heavy organics grind into powder is connect, by obtaining the product of hydrophily first through base, shuttle acidifying or sulfonation；(2) by
The mixture reaction of one product and formaldehyde and sulphur arteries and veins obtains nitrogenous, sulphur the second product；(3) by the second product with it is a certain proportion of
Magnesium source mechanical mixture, is then positioned in retort and carbonizes, obtain magnesia and the porous carbon mixture of nitrogen sulphur codope；Through pickling
Remove magnesia and obtain nitrogen sulphur codope porous charcoal.Nitrogen sulphur codope porous charcoal prepared by the present invention has excellent electrochemistry
Can, it is a kind of high performance electrode material for super capacitor.Patent CN105084358A discloses a kind of for ultracapacitor
Nitrogen sulphur codope activated carbon preparation method.Nitrogen sulphur codope activated carbon is mainly matched somebody with somebody by following compositions by its ratio of weight and number
Than being produced through charing and activating process；Described composition is：Big hair Sterculiaceae fruit is powdery 1-2 parts after charing；
1-4 parts of alkali activator；The preparation method comprises the following steps that (1) is carbonized：1. soak：2. hydro-thermal process：3. drainage is centrifuged；
4. dry；5. grind；(2) activate：1. stage heating and insulation are used：2. slow cooling；3. hydrochloric acid solution soaks：4. water
Wash；5. dry；Ultracapacitor nitrogen sulphur codope activated carbon is become after drying.Patent CN106492749A discloses one kind
The preparation method of nitrogen, sulphur codope micropore-mesopore carbosphere.The present invention relates to a kind of nitrogen, sulphur codope micropore-mesopore carbosphere
Preparation method.Amino phenols, formalin, the skin propylhomoserins of L- half, surfactant, Ludox, second alcohol and water are pressed into certain mass
Than mixing.Water and ethanol are mixed at 20-35 DEG C and sequentially add remaining raw material wherein, 24h is after 100 DEG C of hydro-thermals for reaction
24h is handled, in nitrogen atmosphere, 600-900 DEG C of charing is raised to from room temperature with 2-10 DEG C/min heating rate, removed with NaOH
Silica, obtains nitrogen, the mesoporous carbosphere of sulphur codope.
Above patent raw material is generally organic compound, and building-up process is relative complex, the carbon material of the nitrogen sulphur codope of preparation
And Non-fibrous, therefore prepare by raw material of reproducible biomass the porous carbon fiber of nitrogen sulphur codope there is important research
Meaning.Cotton is a kind of natural biomass resource with fibre structure, remains to keep fibre structure after carbonization, has simultaneously
Good mechanical performance.Therefore, using cotton as raw material, prepared by way of carbonization, activation, nitrogen sulphur codope with Gao Bibiao
Area, 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, sulphur, with reference to chemical activation system
Standby host tool ultracapacitor of good performance nitrogen sulphur codope porous carbon fiber.This route raw material wide material sources, synthetic method
Simplicity, the hole development degree and nitrogen sulfur doping amount of porous carbon fiber are controlled by adjusting the addition of activating reagent and nitrogen sulphur,
Final processing machinery ultracapacitor of good performance nitrogen sulphur codope porous carbon fiber.
The content of the invention
It is total to it is an object of the present invention to provide one kind by carbon source processing machinery ultracapacitor nitrogen sulphur of good performance of cotton
The new method of doping porous carbon fiber.
The present invention is fiber first by 700~950 DEG C of carbonizations of cotton, by carbon fiber and activating reagent, thiocarbamide in mass ratio 1
: 2: 2~1: 7: 6 (g/g/g) mixing, add thereto appropriate distilled water be well mixed, by after impregnation mixture 12h at 105 DEG C
Drying 5h in baking oven, by mixture, 0.5~3h of activation process, solid washing, drying in 700~1000 DEG C of tube furnaces, are obtained
Nitrogen sulphur codope porous carbon fiber carry 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.
Embodiment
Embodiment 1：Cotton is carbonized 1h in tube furnace at 850 DEG C first, by obtained carbon fiber and activating reagent
(KHCO3: KOH mass ratio be 1: 2), thiocarbamide in mass ratio 1: 5: 4 (g/g/g) mixing, add thereto appropriate distilled water mix
Close uniform, 5h will be dried after impregnation mixture 14h in 105 DEG C of baking ovens, by mixture in 800 DEG C of tube furnaces activation process
1.5h, solid washing, dry, obtained nitrogen sulphur codope porous carbon fiber progress electrochemical property test, with 6mol/L hydrogen
Potassium oxide is electrolyte, measures specific capacity for 338F/g, and 5000 capability retentions of circulation are 98% or so.
Embodiment 2：Change carbon fiber and activating reagent (KHCO3: KOH mass ratio is 1: 2), the mass ratio 1: 4 of thiocarbamide:
5 (g/g/g), other conditions be the same as Example 1, the specific capacitance of obtained nitrogen sulphur codope porous carbon fiber is 315F/g, circulation
5000 capability retentions are 97% or so.
Embodiment 3：Change carbon fiber and activating reagent (KHCO3: KOH mass ratio is 1: 2), the mass ratio 1: 6 of thiocarbamide:
3 (g/g/g), other conditions be the same as Example 1, the specific capacitance of obtained nitrogen sulphur codope porous carbon fiber is 323F/g, circulation
5000 capability retentions are 97% or so.
Embodiment 4：It is 2h to change the activation process time in 800 DEG C of tube furnaces of mixture, and other conditions be the same as Example 1 is obtained
The specific capacitance of the nitrogen sulphur codope porous carbon fiber arrived is 309F/g, and 5000 capability retentions of circulation are 97% or so.
Embodiment 5：It is 1h to change the activation process time in 800 DEG C of tube furnaces of mixture, and other conditions be the same as Example 1 is obtained
The specific capacitance of the nitrogen sulphur codope porous carbon fiber arrived is 318F/g, and 5000 capability retentions of circulation are 96% or so.
Embodiment 6：It is 900 DEG C to change mixture activating treatment temperature in tube furnace, and soak time is 1h, other conditions
Be the same as Example 1, the specific capacitance of obtained nitrogen sulphur codope 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 1: 5 of thiocarbamide NaOH mass ratio is 1:
: 4 (g/g/g), by mixture in 800 DEG C of tube furnaces activation process 2h, other conditions be the same as Example 1, obtained nitrogen sulphur is co-doped with
The specific capacitance of miscellaneous 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: 3), the mass ratio 1: 6 of thiocarbamide NaOH mass ratio is 1:
: 3 (g/g/g), by mixture in 850 DEG C of tube furnaces activation process 1.5h, other conditions be the same as Example 1, obtained nitrogen sulphur be total to
The specific capacitance of doping porous carbon fiber is 328F/g, and 5000 capability retentions of circulation are 97% or so.
Claims (2)
1. a kind of ultracapacitor preparation method of nitrogen sulphur codope porous carbon fiber, it is comprised the following steps that：First by cotton
It is fiber to spend 700~950 DEG C of carbonizations, and carbon fiber and activating reagent, thiocarbamide in mass ratio 1: 2: 2~1: 7: 6 (g/g/g) are mixed
Close, appropriate distilled water is added thereto and is well mixed, 5h will be dried after impregnation mixture 12h in 105 DEG C of baking ovens, by mixture
0.5~3h of activation process in 700~1000 DEG C of tube furnaces, solid washing, dry, obtained nitrogen sulphur codope porous carbon fiber
Carry out electrochemical property test.
2. a kind of preparation method of nitrogen sulphur codope porous carbon fiber as claimed in claim 1, it is characterised in that：The activation
Agent is the mixture or saleratus and the mixture of sodium hydroxide of saleratus and potassium hydroxide.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108373154A (en) * | 2018-04-09 | 2018-08-07 | 王干 | A kind of preparation method of self-absorption nitrogen sulfur doping type porous carbon |
| CN108660546A (en) * | 2018-05-31 | 2018-10-16 | 华南理工大学 | A kind of environment-friendly preparation method thereof of cobalt, the porous carbon composite nano-fiber of N doping |
| CN109046426A (en) * | 2018-08-15 | 2018-12-21 | 哈尔滨工业大学 | A kind of nitrogen and sulphur original position codope nickel cobalt base carbon fibre electrolysis water catalyst and preparation method thereof |
| CN109449007A (en) * | 2018-11-05 | 2019-03-08 | 安徽工业大学 | A kind of preparation method of sulphur for electrode of super capacitor, nitrogen co-doped thin nanometer carbon plate |
| CN109994319A (en) * | 2019-04-11 | 2019-07-09 | 合肥工业大学 | The biomass derived carbon material and its synthetic method of a kind of nitrogen sulphur codope and application |
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| CN112938969A (en) * | 2021-03-23 | 2021-06-11 | 复旦大学 | Method for preparing nitrogen-sulfur co-doped activated carbon by pore-forming/doping integrated activating agent and application of method |
| 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 |
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| CN108373154A (en) * | 2018-04-09 | 2018-08-07 | 王干 | A kind of preparation method of self-absorption nitrogen sulfur doping type porous carbon |
| CN108660546B (en) * | 2018-05-31 | 2021-01-19 | 华南理工大学 | Green preparation method of cobalt and nitrogen doped porous carbon composite nanofiber |
| CN108660546A (en) * | 2018-05-31 | 2018-10-16 | 华南理工大学 | A kind of environment-friendly preparation method thereof of cobalt, the porous carbon composite nano-fiber of N doping |
| CN109046426A (en) * | 2018-08-15 | 2018-12-21 | 哈尔滨工业大学 | A kind of nitrogen and sulphur original position codope nickel cobalt base carbon fibre electrolysis water catalyst and preparation method thereof |
| CN109046426B (en) * | 2018-08-15 | 2021-06-29 | 哈尔滨工业大学 | Nitrogen and sulfur in-situ co-doped nickel-cobalt-based carbon fiber electrolytic water catalyst and preparation method thereof |
| CN109449007A (en) * | 2018-11-05 | 2019-03-08 | 安徽工业大学 | A kind of preparation method of sulphur for electrode of super capacitor, nitrogen co-doped thin nanometer carbon plate |
| CN109449007B (en) * | 2018-11-05 | 2020-09-04 | 安徽工业大学 | Preparation method of sulfur and nitrogen co-doped thin nano carbon sheet for supercapacitor electrode |
| CN109994319A (en) * | 2019-04-11 | 2019-07-09 | 合肥工业大学 | The biomass derived carbon material and its synthetic method of a kind of nitrogen sulphur codope and application |
| CN111484013A (en) * | 2020-06-09 | 2020-08-04 | 安徽工业大学 | Preparation method of nitrogen-sulfur co-doped porous carbon for supercapacitor |
| CN111484013B (en) * | 2020-06-09 | 2022-09-27 | 安徽工业大学 | Preparation method of nitrogen-sulfur co-doped porous carbon for supercapacitor |
| CN112938969A (en) * | 2021-03-23 | 2021-06-11 | 复旦大学 | Method for preparing nitrogen-sulfur co-doped activated carbon by pore-forming/doping integrated activating agent and application of method |
| 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 |
| CN113493204A (en) * | 2021-07-05 | 2021-10-12 | 江西省科学院应用化学研究所 | Preparation method of nitrogen-doped nano carbon spheres with ultrahigh specific surface area |
| CN115445574A (en) * | 2022-10-11 | 2022-12-09 | 中国科学院东北地理与农业生态研究所 | Preparation method of N, S co-doped hydrothermal carbon and application thereof in removing Cr (VI) in water |
| CN115445574B (en) * | 2022-10-11 | 2024-01-16 | 中国科学院东北地理与农业生态研究所 | Preparation method of N, S co-doped hydrothermal carbon and application thereof in removing Cr (VI) in water |
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