CN108928819A - A kind of method that oxidizing reduction preparation is graphitized classifying porous carbon material - Google Patents
A kind of method that oxidizing reduction preparation is graphitized classifying porous carbon material Download PDFInfo
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- CN108928819A CN108928819A CN201710386120.3A CN201710386120A CN108928819A CN 108928819 A CN108928819 A CN 108928819A CN 201710386120 A CN201710386120 A CN 201710386120A CN 108928819 A CN108928819 A CN 108928819A
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- porous carbon
- oxidant
- permanganate
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- carbon material
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000001590 oxidative effect Effects 0.000 title claims abstract description 26
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 24
- 230000009467 reduction Effects 0.000 title claims abstract description 4
- 238000002360 preparation method Methods 0.000 title claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000012298 atmosphere Substances 0.000 claims abstract description 37
- 229910001868 water Inorganic materials 0.000 claims abstract description 30
- 239000007800 oxidant agent Substances 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 230000003647 oxidation Effects 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000005087 graphitization Methods 0.000 claims abstract description 7
- 230000001360 synchronised effect Effects 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 64
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 48
- 238000001035 drying Methods 0.000 claims description 42
- 229910052799 carbon Inorganic materials 0.000 claims description 41
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 238000001994 activation Methods 0.000 claims description 34
- 240000008289 Quercus suber Species 0.000 claims description 23
- 235000016977 Quercus suber Nutrition 0.000 claims description 23
- 239000012286 potassium permanganate Substances 0.000 claims description 19
- 206010013786 Dry skin Diseases 0.000 claims description 18
- 239000007799 cork Substances 0.000 claims description 18
- 238000001704 evaporation Methods 0.000 claims description 18
- 230000008020 evaporation Effects 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 240000007594 Oryza sativa Species 0.000 claims description 12
- 235000007164 Oryza sativa Nutrition 0.000 claims description 12
- 235000009566 rice Nutrition 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 150000002500 ions Chemical class 0.000 claims description 10
- 238000003763 carbonization Methods 0.000 claims description 9
- 239000010902 straw Substances 0.000 claims description 9
- 240000006240 Linum usitatissimum Species 0.000 claims description 8
- 235000004431 Linum usitatissimum Nutrition 0.000 claims description 8
- 240000008042 Zea mays Species 0.000 claims description 8
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 8
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 8
- 235000005822 corn Nutrition 0.000 claims description 8
- 239000010903 husk Substances 0.000 claims description 8
- 239000002699 waste material Substances 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 7
- 244000299507 Gossypium hirsutum Species 0.000 claims description 7
- 244000046052 Phaseolus vulgaris Species 0.000 claims description 7
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims description 7
- 239000003792 electrolyte Substances 0.000 claims description 7
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 7
- 241000609240 Ambelania acida Species 0.000 claims description 6
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 6
- 244000105624 Arachis hypogaea Species 0.000 claims description 6
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 6
- 235000018262 Arachis monticola Nutrition 0.000 claims description 6
- 240000007049 Juglans regia Species 0.000 claims description 6
- 235000009496 Juglans regia Nutrition 0.000 claims description 6
- 235000003956 Luffa Nutrition 0.000 claims description 6
- 244000050983 Luffa operculata Species 0.000 claims description 6
- 235000008331 Pinus X rigitaeda Nutrition 0.000 claims description 6
- 241000018646 Pinus brutia Species 0.000 claims description 6
- 235000011613 Pinus brutia Nutrition 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 240000000111 Saccharum officinarum Species 0.000 claims description 6
- 235000007201 Saccharum officinarum Nutrition 0.000 claims description 6
- -1 acerdol Chemical compound 0.000 claims description 6
- 239000010905 bagasse Substances 0.000 claims description 6
- 235000020232 peanut Nutrition 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 235000020234 walnut Nutrition 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052788 barium Inorganic materials 0.000 claims description 5
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052793 cadmium Inorganic materials 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000011777 magnesium Substances 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 229910052701 rubidium Inorganic materials 0.000 claims description 5
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 5
- 239000010907 stover Substances 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- JYLNVJYYQQXNEK-UHFFFAOYSA-N 3-amino-2-(4-chlorophenyl)-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(CN)C1=CC=C(Cl)C=C1 JYLNVJYYQQXNEK-UHFFFAOYSA-N 0.000 claims description 4
- KLARSDUHONHPRF-UHFFFAOYSA-N [Li].[Mn] Chemical compound [Li].[Mn] KLARSDUHONHPRF-UHFFFAOYSA-N 0.000 claims description 4
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 claims description 2
- 244000198134 Agave sisalana Species 0.000 claims description 2
- 240000000560 Citrus x paradisi Species 0.000 claims description 2
- 244000060011 Cocos nucifera Species 0.000 claims description 2
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 2
- 229920000742 Cotton Polymers 0.000 claims description 2
- 244000068988 Glycine max Species 0.000 claims description 2
- 235000010469 Glycine max Nutrition 0.000 claims description 2
- 239000007832 Na2SO4 Substances 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 2
- 241001506047 Tremella Species 0.000 claims description 2
- 235000021307 Triticum Nutrition 0.000 claims description 2
- 244000098338 Triticum aestivum Species 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims 1
- 241000233866 Fungi Species 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims 1
- 210000005056 cell body Anatomy 0.000 claims 1
- 229910052804 chromium Inorganic materials 0.000 claims 1
- 239000011651 chromium Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000007772 electrode material Substances 0.000 abstract description 5
- 239000003990 capacitor Substances 0.000 abstract description 3
- 238000005554 pickling Methods 0.000 abstract description 3
- 239000002028 Biomass Substances 0.000 abstract 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 30
- 239000007789 gas Substances 0.000 description 24
- 238000002242 deionisation method Methods 0.000 description 20
- 229910052757 nitrogen Inorganic materials 0.000 description 15
- 239000003643 water by type Substances 0.000 description 13
- 230000004913 activation Effects 0.000 description 12
- 238000010792 warming Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 8
- 239000012190 activator Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- RDVQTQJAUFDLFA-UHFFFAOYSA-N cadmium Chemical compound [Cd][Cd][Cd][Cd][Cd][Cd][Cd][Cd][Cd] RDVQTQJAUFDLFA-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- JOSWYUNQBRPBDN-UHFFFAOYSA-P ammonium dichromate Chemical compound [NH4+].[NH4+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O JOSWYUNQBRPBDN-UHFFFAOYSA-P 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000006479 redox reaction Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052754 neon Inorganic materials 0.000 description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 241000124033 Salix Species 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- XAQCJVGGJJFLPP-UHFFFAOYSA-L azane;hydroxy-(hydroxy(dioxo)chromio)oxy-dioxochromium Chemical class N.N.O[Cr](=O)(=O)O[Cr](O)(=O)=O XAQCJVGGJJFLPP-UHFFFAOYSA-L 0.000 description 1
- 244000285940 beete Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 235000011222 chang cao shi Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000009415 formwork Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- PXLIDIMHPNPGMH-UHFFFAOYSA-N sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 description 1
- KIEOKOFEPABQKJ-UHFFFAOYSA-N sodium dichromate Chemical class [Na+].[Na+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KIEOKOFEPABQKJ-UHFFFAOYSA-N 0.000 description 1
- 238000010129 solution processing Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of methods that oxidizing reduction prepares the biomass-based classifying porous carbon material of graphitization, it includes that oxidant and biomass presoma, wherein oxidant and biomass forerunner body mass ratio are about 0.5:1.0~10:1.0.It weighs quantitative oxidant and biomass presoma and carries out quality that is uniformly mixed, then pressing oxidant and water:Volume ratio 0.01:1.0~1.0:The water that 1.0 (g/ml) weigh determining volume is uniformly mixed with oxidation of precursor agent, is boiled and is evaporated, synchronous carbonization-activation under inert atmosphere protection, then through salt pickling and washing to get the classifying porous carbon material of graphitization.The invention also discloses graded porous carbons obtained by this method as electrode material for super capacitor.
Description
Technical field
It the invention belongs to porous carbon materials preparation technical field, specifically discloses using oxidant as activator, passes through oxidation
Agent solution processing carbonization presoma, through drying, synchronous carbonization and activation preparation graphitization micropore-mesoporous composite ratings porous carbon
The method of material makes full use of oxidant and the redox reaction carried out between presoma that is carbonized, and has reached the mesh for being classified pore-creating
's.
Background technique
Currently, the conventional method for preparing porous carbon is the post activation that is first carbonized, activation is its committed step, product porous carbon
With typical pore characteristics.Activation mainly has three kinds of physical activation method, chemical activation method and template techniques, physical activation method
It is with H2O and CO2Equal gases are pore-creating activator, at 700 DEG C or more, are continually fed into activated gas and carve to carbonization presoma
Erosion, which activates, is made porous carbon materials, as the patent of invention of Publication No. CN101397136A, CN104591183A is all made of physics
Activation method prepares porous carbon.Chemical activation method is with KOH, NaOH, K2CO3、Na2CO3、ZnCl2、H3PO4Equal chemical reagent are to live
Agent, by presoma and activator by setting quality proportioning, the two is uniformly mixed, handles through high-temperature activation, through pickling, washing,
Be drying to obtain micro-pore carbon material, as Publication No. CN102502628A, CN101332992A, CN102718213A,
The patent of invention of CN103408012A, CN103449433A are all made of different chemical activating agents and prepare porous carbon.Template is
Using the material with specific morphology as template, organic matter is injected into template, after high-temperature process, template is removed using ad hoc approach
Porous carbon similar with formwork structure is made.Templating species are various, wherein hard template because it can preferably control pore structure,
It is a most common class template, the invention such as Publication No. CN1724344A, CN102976305A, CN105664848A is special
Benefit prepares porous carbon materials using hard template.Common hard template has mesopore silicon oxide, zeolite etc., is prepared using hard template more
When the carbon of hole, need to remove hard template using chemical reagent such as HF, highly basic, which has certain pollution to environment.Soft template method
Be frequently with method, the surfactant and organic compound that common soft template has block copolymer, ion micelle, structure special
Object etc. removes soft template and is easier relative to hard template, in high temperature cabonization or activation process, that is, is pyrolyzed volatilization removing
, but the cost is relatively high for the method, such as the patent of invention of Publication No. CN103833003A, CN105692583A, that is, uses
Different soft templates prepare porous carbon materials.According to different preparation methods, prepared by the structure of porous carbon, physical chemistry
Property and its absorption property have very big difference, therefore study porous carbon materials new preparation technology and be with a wide range of applications.
Currently, the research for being prepared porous carbon using the redox reaction between oxidant and presoma is also rarely reported.
In general, oxidant is mostly used to make surface modifier in the preparation process of porous carbon, surface is carried out to carbon material and is modified, such as publication number
It is modified to carbon material progress surface using potassium permanganate for the patent of invention of CN103626150A, CN104959110A；Publication number
Carbon material is surface modified using potassium bichromate for the patent of invention of CN102208661A, changes material surface characteristic.Mesh
It is preceding only to find that the patent of invention of Publication No. CN102381703A reports a kind of method for preparing activated carbon with waste of flax, wherein making
Use a kind of oxidant-low concentration potassium permanganate (mass concentration is 0.2 ~ 1.0 %) as activator, it will pretreatment over dry material
With activator solution according to mass ratio 1 ~ 6:100 are uniformly mixed, and powder activated carbon is obtained after drying, 700 ~ 900 DEG C of carbonization-activations
Sample.Patent specification, which discloses, uses series of oxidation agent to activate pore creating material, uses high quality ratio (oxidant:Presoma
Weight ratio) condition, the method for preparing the graphited classifying porous carbon material of micropore-mesoporous.
Graded porous carbon is rich in mesoporous and micropore, is applied to supercapacitor and ion battery electrode materials, and property is bright
The aobvious porous carbon materials being different from based on micropore, the micropore of graded porous carbon provide active site, mesoporous for the accumulation of charge
Unobstructed channel is provided for the diffusion of electrolyte ion, reduces transport resistance of the electrolyte ion in hole, and shorten electrolyte
Transmission range of the ion in hole is conducive to obtain high power density (Wang Dawei, Li Feng, Liu Min, Lu
Gaoqing, Cheng Huiming. Angewandte Chemie International Edition, 2008, 47(2):
373-376.).And the degree of graphitization of graded porous carbon is improved, it is also beneficial to appropriately improve the electric conductivity (Mun of material
Yeongdong, Jo Changshin, Hyeon Taeghwan, Lee Jaehyuk, Ha Kyoung-Su, Jun Ki-
Won, Lee Sang-Hyup, Hong Seok-Won, Lee Hyung Ik, Yoon Songhun, Lee Jinwoo.
Carbon, 2013, 64:391-402.), the electrode material as supercapacitor and ion battery can obtain high power
Density.
Summary of the invention
The purpose of the present invention is to provide a kind of technologies of preparing of graphited classifying porous carbon material, are to live with oxidant
Agent handles carbonization presoma by oxidizing agent solution, multiple through drying, synchronous carbonization and activation preparation graphitization micropore-mesoporous
The method for closing classifying porous carbon material takes full advantage of the redox reaction in oxidant between high valence elements and carbon and comes
Pore-creating, specific step is as follows for this method.
1. pretreatment of raw material and ingredient：Raw material precursor is broken into powder, crosses 40 meshes, washing powder, filtering 2 ~ 4 times
Afterwards, 70 ~ 100 DEG C of 12 ~ 24 h of drying are placed in, are 0.5 according to presoma butt and oxidant mass ratio (g/g):1.0~10:
1.0, preferably 0.75 ~ 5.0:1.0, more preferable 1.0 ~ 3.0:1.0, most preferably 1.25 ~ 2.0:1.0 ingredients weigh quantitative forerunner
Body and oxidant are pulverized and mixed uniformly, obtain oxidation of precursor agent composition.According to the quality of oxidant and water:Volume ratio (g/
It ml) is 0.01:1.0~1.0:1.0, preferably 0.015:1.0~0.5:1.0, more preferable 0.02:1.0~0.2:1.0, most preferably
0.03:1.0~0.1:1.0, the water for weighing determining volume is uniformly mixed with oxidation of precursor agent, and it is dry that evaporation is boiled in 70 ~ 100 DEG C
It is dry, obtain oxidation of precursor agent dry basis mixture.
2. in above-mentioned 1, oxidation of precursor agent dry basis mixture is placed in inert atmosphere high temperature furnace, heat temperature raising is carried out
Carbonization-activation, control temperature range be 400 ~ 1000 DEG C, preferably 500 ~ 800 DEG C, more preferable 550 ~ 750 DEG C, most preferably 550 ~
700 DEG C, the control time is 0.5 ~ 8.0 h, preferably 1.0 ~ 6.0 h, more preferable 2.0 ~ 5.0 h, most preferably 2.5 ~ 4.0 h, inertia
100 ~ 300 ml/min of gas flow rate, inert atmosphere high temperature furnace are down to room temperature naturally, obtain carbonized product.
3. in above-mentioned 2, carbonized product washing：Carbonized product, which is first placed in excessive hot hydrochloric acid solution, impregnates 2.0 ~ 5.0
H carries out pickling, filtering, then is washed repeatedly with deionized water, until pH=6.0 ~ 7.0,70 ~ 100 DEG C drying, is made graphitization
Classifying porous carbon material.
4. being graphitized the application of classifying porous carbon material in above-mentioned 3：It is graphitized graded porous carbon and makes super capacitor
The electrode of device and ion battery assembles supercapacitor and ion battery with electrolyte.
5. in above-mentioned 1, the raw material presoma includes cork oak cork, fruit tree, pine, beans root, luffa, willow
Wadding, bombax cotton, cotton fiber, Yang Xu, catkin, ramee, sisal fiber, mycelia fiber, big waste of flax, falx straw, burnt fiber crops
Bar, corncob, corn stover, wheat stalk, rice straw, rice husk, peanut shell, bagasse, sugarcane skin, pomelo peel, tremella, black wood
Ear, soybean, coconut husk, walnut shell.
6. in above-mentioned 1, the oxidant includes potassium permanganate, ammonium permanganate, sodium permanganate, high manganese lithium, Gao Meng
Sour calcium, barium permanganate, zinc permanganate, magnesium permanganate, cadmium permanganate, permanganic acid rubidium, potassium bichromate, ammonium dichromate, sodium dichromate
One or more of oxidant.
7. in above-mentioned 2, the inert gas includes argon gas, neon or nitrogen.
8. in above-mentioned 3, the acid elution condition of the carbonized product is 1.0 ~ 6.0 M hydrochloric acid solutions, 50 ~ 80
DEG C dipping 2 ~ 5 h.
9. in above-mentioned 4, the electrolyte, including KOH, Na2SO4, 1- ethyl-3-methylimidazole tetrafluoroborate
([EMIm]BF4)、H2SO4, double pyrrolidines spiro quaternary ammonium salt (SBP BF4)。
10. in above-mentioned 4, the application should also include electrode material for battery and gas adsorption material.
The method of the invention and material prepared have following advantages.
(1) of the invention to use oxidant as activator, activation effect is obvious.
(2) technical process carbonization-activation of the invention is synchronous carries out, and optimizes the preparation process of regular activated carbon.
(3) carbon material prepared by the present invention has carbonization structure, contains macropore, mesoporous and micropore simultaneously.
(4) graded porous carbon prepared by the present invention is applied to electrode of super capacitor and ion-conductance as electrode material
Pond electrode shows excellent chemical property.
Detailed description of the invention
Fig. 1 is 1 raw material of embodiment (cork oak cork) electron scanning micrograph.
Fig. 2 is the transmission electron microscope photo of cork oak cork base graded porous carbon prepared by embodiment 1.
Fig. 3 is the transmission electron microscope photo that graded porous carbon graphite flake layer is graphitized prepared by embodiment 1.
Fig. 4 is the Raman spectroscopy of cork oak cork base graded porous carbon prepared by embodiment 1.
Fig. 5 is cork oak cork base graded porous carbon N prepared by embodiment 12Adsorption and desorption isotherms.
Fig. 6 is cork oak cork base graded porous carbon pore size distribution curve prepared by embodiment 1.
Fig. 7 is that constant current of the cork oak cork base graded porous carbon under different current densities prepared by embodiment 1 fills
Discharge curve.
Specific embodiment
Below in conjunction with the specific embodiment of the invention, technical solution of the present invention is described.
Embodiment 1
Cork oak cork crushes, crosses 40 meshes, after washing, in 80 DEG C of dry 24 h, according to potassium permanganate and cork oak cork
Mass ratio is 1.25:1.0, weigh 3.75 g potassium permanganate and 3 g cork oak corks respectively, be uniformly mixed, obtain potassium permanganate with
Cork oak cork compound.According to the quality of potassium permanganate and water:Volume ratio (g/ml) is 0.0375:1.0, it measures 100 ml and goes
Said mixture is uniformly mixed by ionized water with deionized water, and 70 DEG C of evaporation dryings obtain dry basis mixture.By dry basis mixture
It is placed in tube-type atmosphere furnace, is warming up to 600 DEG C, under nitrogen protection 2 h of carbonization-activation, gas flow rate is 200 ml/min, pipe
Formula atmosphere furnace Temperature fall, obtains carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 4 at 60 DEG C
H, filtering, deionization washs several times repeatedly, until pH=6.0 ~ 7.0,80 DEG C drying, it is classifying porous to obtain cork oak cork base
Carbon, specific surface area are 689 m2/ g, by calculating, sample yield is 17.4 %.
Embodiment 2
Cork oak cork is crushed, crosses 40 meshes, it is after washing, soft with cork oak according to potassium permanganate in 80 DEG C of dry 24 h
The wooden mass ratio is 2:1.0,6 g potassium permanganate and 3 g cork oak corks are weighed respectively, are uniformly mixed, are obtained potassium permanganate and cork
Oak cork compound.According to the quality of potassium permanganate and water:Volume ratio (g/ml) is 0.06:1.0, measure 100 ml deionizations
Said mixture is uniformly mixed by water with deionized water, and 80 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in
In tube-type atmosphere furnace, 600 DEG C are warming up to, under protection of argon gas 3 h of carbonization-activation, gas flow rate is 200 ml/min, tubular type gas
Atmosphere furnace Temperature fall, obtains carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 5 h, mistake at 70 DEG C
Filter, deionization wash several times repeatedly, until pH=6.0 ~ 7.0,70 DEG C drying, obtains cork oak cork base graded porous carbon,
Specific surface area is 726 m2/ g, by calculating, sample yield is 15.3 %.
Embodiment 3
Cork oak cork is crushed, crosses 40 meshes, it is after washing, soft with cork oak according to potassium permanganate in 80 DEG C of dry 24 h
The wooden mass ratio is 3:1.0,9 g potassium permanganate and 3 g cork oak corks are weighed respectively, are uniformly mixed, are obtained potassium permanganate and cork
Oak cork compound.According to the quality of potassium permanganate and water:Volume ratio (g/ml) is 0.045:1.0, measure 200 ml deionizations
Said mixture is uniformly mixed by water with deionized water, and 70 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in
In tube-type atmosphere furnace, 500 DEG C are warming up to, under nitrogen protection 1 h of carbonization-activation, gas flow rate is 200 ml/min, tubular type gas
Atmosphere furnace Temperature fall, obtains carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 5 h, mistake at 80 DEG C
Filter, deionization wash several times repeatedly, until pH=6.0 ~ 7.0,80 DEG C drying, obtains cork oak cork base graded porous carbon,
Specific surface area is 637 m2/ g, by calculating, sample yield is 14.2 %.
Embodiment 4
It is 1.5 according to ammonium permanganate and bombax cotton mass ratio in 80 DEG C of dry 24 h after bombax cotton washing:1.0, respectively
4.5 g ammonium permanganates and 3 g bombax cottons are weighed, is uniformly mixed, obtains ammonium permanganate and bombax cotton mixture.According to permanganic acid
The quality of ammonium and water:Volume ratio (g/ml) is 0.045:1.0,100 ml deionized waters are measured, by said mixture and deionization
Water is uniformly mixed, and 90 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace, is warming up to 700
DEG C, 5 h of carbonization-activation, gas flow rate are 200 ml/min under nitrogen protection, and tube-type atmosphere furnace Temperature fall obtains carbonization and produces
Object.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 3 h at 50 DEG C, is filtered, deionization washs several times repeatedly,
Until pH=6.0 ~ 7.0,90 DEG C drying, obtains bombax cotton base graded porous carbon, specific surface area is 1251 m2/ g, by meter
It calculates, sample yield is 16.1 %.
Embodiment 5
Big waste of flax crushes, crosses 40 meshes
0.5:1.0,1.5 g potassium bichromates and the big waste of flax of 3 g are weighed respectively, are uniformly mixed, are obtained potassium bichromate and big waste of flax mixture.It presses
According to the quality of potassium bichromate and water:Volume ratio (g/ml) is 0.01:1.0, measure 150 ml deionized waters, by said mixture with
Deionized water is uniformly mixed, and 100 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace, is risen
Temperature is to 1000 DEG C, 8 h of carbonization-activation under nitrogen protection, and gas flow rate is 300 ml/min, tube-type atmosphere furnace Temperature fall,
Obtain carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 2 h at 60 DEG C, is filtered, deionization is repeatedly
Washing several times, up to pH=6.0 ~ 7.0,100 DEG C drying, obtains big waste of flax base graded porous carbon, specific surface area 1095
m2/ g, by calculating, sample yield is 14.9 %.
Embodiment 6
Beans root crushes, crosses 40 meshes, is 10 according to sodium permanganate and beans root mass ratio for 24 hours in 80 DEG C of dryings after washing:
1.0,30 g sodium permanganates and 3 g beans roots are weighed respectively, are uniformly mixed, are obtained sodium permanganate and beans root mixture.According to permanganic acid
The quality of sodium and water:Volume ratio (g/ml) is 0.1:1.0,300 ml deionized waters are measured, by said mixture and deionized water
It is uniformly mixed, 80 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace, is warming up to 400
DEG C, 0.5 h of carbonization-activation under neon protection, gas flow rate is 100 ml/min, and tube-type atmosphere furnace Temperature fall is carbonized
Product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 5 h at 60 DEG C, is filtered, deionization washs several repeatedly
Secondary, until pH=6.0 ~ 7.0,80 DEG C drying, obtains beans foundation graded porous carbon, specific surface area is 496 m2/ g, by calculating,
Sample yield is 13.7 %.
Embodiment 7
Luffa crushes, crosses 40 meshes
5:1.0,15 g ammonium dichromates and 3 g luffas are weighed respectively, are uniformly mixed, are obtained ammonium dichromate and luffa mixture.According to
The quality of ammonium dichromate and water:Volume ratio (g/ml) is 0.5:1.0, measure 30 ml deionized waters, by said mixture and go from
Sub- water is uniformly mixed, and 80 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace, is warming up to
800 DEG C, 1 h of carbonization-activation, gas flow rate are 200 ml/min under nitrogen protection, and tube-type atmosphere furnace Temperature fall obtains carbon
Change product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 5 h at 70 DEG C, is filtered, if deionization washs repeatedly
Dry time, until pH=6.0 ~ 7.0,80 DEG C drying, obtains luffa base graded porous carbon, specific surface area is 1279 m2/ g passes through
It calculates, sample yield is 12.4 %.
Embodiment 8
Peanut shell crushes, crosses 40 meshes
1:1.0,3 g sodium dichromates and 3 g peanut shells are weighed respectively, are uniformly mixed, are obtained sodium dichromate and peanut shell mixture.According to weight
The quality of sodium chromate and water:Volume ratio (g/ml) is 0.1:1.0,30 ml deionized waters are measured, by said mixture and deionization
Water is uniformly mixed, and 90 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace, is warming up to 900
DEG C, 3 h of carbonization-activation, gas flow rate are 200 ml/min under nitrogen protection, and tube-type atmosphere furnace Temperature fall obtains carbonization and produces
Object.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 5 h at 60 DEG C, is filtered, deionization washs several times repeatedly,
Until pH=6.0 ~ 7.0,90 DEG C drying, obtains peanut shell base graded porous carbon, specific surface area is 1163 m2/ g, by calculating,
Sample yield is 14.1 %.
Embodiment 9
Corncob crushes, crosses 40 meshes, after washing, in 80 DEG C of dry 24 h, according to potassium bichromate and potassium permanganate and corn
Core mass ratio is 1.5:1.0,2.25 g potassium bichromates, 2.25 g potassium permanganate and 3 g corncobs are weighed respectively, are uniformly mixed,
Obtain potassium bichromate and potassium permanganate and corncob mixture.According to the quality of two kinds of oxidants and water:Volume ratio (g/ml) is
0.045:1.0,100 ml deionized waters are measured, said mixture are uniformly mixed with deionized water, 80 DEG C of evaporation dryings obtain
Dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace, is warming up to 600 DEG C, under nitrogen protection 2 h of carbonization-activation,
Gas flow rate is 200 ml/min, and tube-type atmosphere furnace Temperature fall obtains carbonized product.Carbonized product is placed in excessive 6 M salt
5 h are impregnated in acid solution at 60 DEG C, are filtered, deionization washs several times repeatedly, until pH=6.0 ~ 7.0,90 DEG C drying,
Corncob base graded porous carbon is obtained, specific surface area is 723 m2/ g, by calculating, sample yield is 15.7 %.
Embodiment 10
Walnut shell crushes, crosses 40 meshes
1.25:1.0,3.75 g high manganese lithiums and 3 g walnut shells are weighed respectively, are uniformly mixed, are obtained high manganese lithium and walnut shell mixture.
According to the quality of high manganese lithium and water:Volume ratio (g/ml) is 0.0375:1.0,100 ml deionized waters are measured, by above-mentioned mixing
Object is uniformly mixed with deionized water, and 70 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace,
Be warming up to 600 DEG C, under nitrogen protection 2 h of carbonization-activation, gas flow rate be 200 ml/min, tube-type atmosphere furnace Temperature fall,
Obtain carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 4 h at 60 DEG C, is filtered, deionization is repeatedly
Several times, until pH=6.0 ~ 7.0,80 DEG C drying, obtains walnut shell base graded porous carbon, specific surface area is 658 m for washing2/
G, by calculating, sample yield is 17.1 %.
Embodiment 11
Rice husk crushes, crosses 40 meshes
1.25:1.0,3.75 g acerdols and 3 g rice husks are weighed respectively, are uniformly mixed, are obtained acerdol and rice husk mixture.According to
The quality of acerdol and water:Volume ratio (g/ml) is 0.0375:1.0, measure 100 ml deionized waters, by said mixture with
Deionized water is uniformly mixed, and 70 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace, is heated up
To 600 DEG C, 2 h of carbonization-activation, gas flow rate are 200 ml/min under nitrogen protection, and tube-type atmosphere furnace Temperature fall obtains
Carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 4 h at 60 DEG C, is filtered, deionization washs repeatedly
Several times, until pH=6.0 ~ 7.0,80 DEG C drying, obtains rice husk base graded porous carbon, specific surface area is 635 m2/ g passes through
It calculates, sample yield is 18.3 %.
Embodiment 12
Rice straw crushes, crosses 40 meshes
1.25:1.0,3.75 g barium permanganates and 3 g rice straws are weighed respectively, are uniformly mixed, are obtained barium permanganate and rice straw mixture.According to
The quality of barium permanganate and water:Volume ratio (g/ml) is 0.0375:1.0, measure 100 ml deionized waters, by said mixture with
Deionized water is uniformly mixed, and 70 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace, is heated up
To 600 DEG C, 2 h of carbonization-activation, gas flow rate are 200 ml/min under nitrogen protection, and tube-type atmosphere furnace Temperature fall obtains
Carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 4 h at 60 DEG C, is filtered, deionization washs repeatedly
Several times, until pH=6.0 ~ 7.0,80 DEG C drying, obtains rice straw base graded porous carbon, specific surface area is 711 m2/ g passes through
It calculates, sample yield is 15.5 %.
Embodiment 13
Bagasse crushes, crosses 40 meshes
1.25:1.0,3.75 g zinc permanganates and 3 g bagasse are weighed respectively, are uniformly mixed, are obtained zinc permanganate and bagasse mixture.
According to the quality of zinc permanganate and water:Volume ratio (g/ml) is 0.0375:1.0,100 ml deionized waters are measured, by above-mentioned mixing
Object is uniformly mixed with deionized water, and 70 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace,
Be warming up to 600 DEG C, under nitrogen protection 2 h of carbonization-activation, gas flow rate be 200 ml/min, tube-type atmosphere furnace Temperature fall,
Obtain carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 4 h at 60 DEG C, is filtered, deionization is repeatedly
Several times, until pH=6.0 ~ 7.0,80 DEG C drying, obtains bagasse base graded porous carbon, specific surface area is 671 m for washing2/
G, by calculating, sample yield is 15.7 %.
Embodiment 14
Sugarcane skin crushes, crosses 40 meshes
1.25:1.0,3.75 g magnesium permanganates and 3 g sugarcane skins are weighed respectively, are uniformly mixed, are obtained magnesium permanganate and sugarcane skin mixture.
According to the quality of magnesium permanganate and water:Volume ratio (g/ml) is 0.0375:1.0,100 ml deionized waters are measured, by above-mentioned mixing
Object is uniformly mixed with deionized water, and 70 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace,
Be warming up to 600 DEG C, under nitrogen protection 2 h of carbonization-activation, gas flow rate be 200 ml/min, tube-type atmosphere furnace Temperature fall,
Obtain carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 4 h at 60 DEG C, is filtered, deionization is repeatedly
Several times, until pH=6.0 ~ 7.0,80 DEG C drying, obtains sugarcane scytoblastema graded porous carbon, specific surface area is 657 m for washing2/
G, by calculating, sample yield is 16.7 %.
Embodiment 15
Pine crushes, crosses 40 meshes
1.25:1.0,3.75 g cadmium permanganates and 3 g pines are weighed respectively, are uniformly mixed, are obtained cadmium permanganate and pine mixture.According to
The quality of cadmium permanganate and water:Volume ratio (g/ml) is 0.0375:1.0, measure 100 ml deionized waters, by said mixture with
Deionized water is uniformly mixed, and 70 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in tube-type atmosphere furnace, is heated up
To 600 DEG C, 2 h of carbonization-activation, gas flow rate are 200 ml/min under nitrogen protection, and tube-type atmosphere furnace Temperature fall obtains
Carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 4 h at 60 DEG C, is filtered, deionization washs repeatedly
Several times, until pH=6.0 ~ 7.0,80 DEG C drying, obtains pine base graded porous carbon, specific surface area is 635 m2/ g passes through
It calculates, sample yield is 17.7 %.
Embodiment 16
Corn straw smashing crosses 40 meshes, after washing, in 80 DEG C of dry 24 h, according to permanganic acid rubidium and corn stover quality
Than being 1.25:1.0,3.75 g permanganic acid rubidiums and 3 g corn stovers are weighed respectively, are uniformly mixed, are obtained permanganic acid rubidium and corn stalk
Stalk mixture.According to the quality of permanganic acid rubidium and water:Volume ratio (g/ml) is 0.0375:1.0,100 ml deionized waters are measured,
Said mixture is uniformly mixed with deionized water, 70 DEG C of evaporation dryings obtain dry basis mixture.Dry basis mixture is placed in pipe
In formula atmosphere furnace, 600 DEG C are warming up to, under nitrogen protection 2 h of carbonization-activation, gas flow rate is 200 ml/min, tubular type atmosphere
Furnace Temperature fall, obtains carbonized product.Carbonized product is placed in excessive 6 M hydrochloric acid solutions and impregnates 4 h at 60 DEG C, is filtered,
Deionization washs several times repeatedly, until pH=6.0 ~ 7.0,80 DEG C drying, obtains corn stover base graded porous carbon, specific surface
Product is 735 m2/ g, by calculating, sample yield is 17.3 %.
Claims (8)
1. oxidizing reduction preparation is graphitized the methods and applications of classifying porous carbon material, this method includes：Before raw material
It drives body and is ground into powder, cross 40 meshes, washing powder after filtering 2 ~ 4 times, is placed in 70 ~ 100 DEG C of 12 ~ 24 h of drying, according to preceding
It drives soma base and oxidant mass ratio (g/g) is 0.5:1.0~10:1.0, preferably 0.75 ~ 5.0:1.0, more preferable 1.0 ~ 3.0:
1.0, most preferably 1.25 ~ 2.0:1.0 ingredients weigh quantitative presoma and oxidant, are pulverized and mixed uniformly, obtain presoma oxygen
Agent mixture, according to the quality of oxidant and water:Volume ratio (g/ml) is 0.01:1.0~1.0:1.0, preferably 0.015:1.0~
0.5:1.0, more preferable 0.02:1.0~0.2:1.0, most preferably 0.03:1.0~0.1:1.0, weigh water and the forerunner of determining volume
Body oxidant is uniformly mixed, and is boiled evaporation drying in 70 ~ 100 DEG C, is obtained oxidation of precursor agent dry basis mixture, then through inertia
Synchronous carbonization-activation, hydrochloric acid and water washing under atmosphere protection, it is dry to get the classifying porous carbon material of graphitization.
2. method according to claim 1, wherein during the carbonization-activation of oxidation of precursor agent dry basis mixture, control temperature
Spending range is 400 ~ 1000 DEG C, and preferably 500 ~ 800 DEG C, more preferable 550 ~ 750 DEG C, most preferably 550 ~ 700 DEG C control the time
For 0.5 ~ 8.0 h, preferably 1.0 ~ 6.0 h, more preferable 2.0 ~ 5.0 h, most preferably 2.5 ~ 4.0 h, inert gas flow velocity 100 ~ 300
Ml/min, inert atmosphere high temperature furnace are down to room temperature naturally.
3. method according to claim 1, wherein carbonized product washing is that carbonized product is placed in excessive 1.0 ~ 6.0 M salt
In acid solution, 50 ~ 80 DEG C of 2.0 ~ 5.0 h of dipping, filtering, deionized water is washed repeatedly, until pH=6.0 ~ 7.0, and detect nothing
Cl-1Ion, in 70 ~ 100 DEG C of dryings.
4. according to the method described in claim 1, wherein the raw material presoma includes cork oak cork, fruit tree, pine, beans
Root, luffa, catkin, bombax cotton, cotton fiber, Yang Xu, catkin, ramee, sisal fiber, mycelia fiber, big waste of flax,
Falx straw, burnt waste of flax, corncob, corn stover, wheat stalk, rice straw, rice husk, peanut shell, bagasse, sugarcane skin, pomelo peel,
Tremella, black fungus, soybean, coconut husk, walnut shell.
5. according to the method described in claim 1, wherein the oxidant include potassium permanganate, ammonium permanganate, sodium permanganate,
High manganese lithium, acerdol, barium permanganate, zinc permanganate, magnesium permanganate, cadmium permanganate, permanganic acid rubidium, potassium bichromate, weight chromium
The oxidant of one or more of sour ammonium, sodium dichromate.
6. according to the method described in claim 1, the graphited classifying porous carbon material described in wherein, has carbonization structure
The classifying porous feature of micropore, the nm of 5 nm ~ 50 mesoporous and the combination of the nm macropore of 50 nm ~ 80 with aperture less than 2 nm.
7. feature according to claim 6, the application for being graphitized classifying porous carbon material include：It is graphitized graded porous carbon
The electrode for making supercapacitor and ion battery assembles supercapacitor and ion battery with electrolyte.
8. application according to claim 7, wherein the electrolyte includes：KOH,Na2SO4, 1- ethyl -3- methyl miaow
Azoles tetrafluoroborate ([EMIm] BF4)、H2SO4, double pyrrolidines spiro quaternary ammonium salt (SBP BF4)。
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN109482161A (en) * | 2019-01-15 | 2019-03-19 | 广东省生物工程研究所（广州甘蔗糖业研究所） | The modified bagasse graded porous carbon of two sections of amine of energy efficient absorption mercury and preparation method and application |
| CN110436459A (en) * | 2019-09-19 | 2019-11-12 | 盐城工学院 | A kind of preparation method being graphitized graded porous carbon |
| CN113247887A (en) * | 2021-04-13 | 2021-08-13 | 齐鲁工业大学 | Preparation method of hierarchical porous graphene and application of hierarchical porous graphene |
| CN113636550A (en) * | 2021-07-14 | 2021-11-12 | 东北农业大学 | Method for preparing straw-based nitrogen-rich mesoporous carbon by one-step method and application thereof |
| CN114203457A (en) * | 2021-11-23 | 2022-03-18 | 东北农业大学 | NiCo2S4Preparation method of/MC |
| CN114203457B (en) * | 2021-11-23 | 2024-02-23 | 东北农业大学 | NiCo 2 S 4 Preparation method of/MC |
| WO2023160017A1 (en) * | 2022-02-28 | 2023-08-31 | 广东邦普循环科技有限公司 | Plant pompon hard carbon composite negative electrode material, and preparation method therefor and use thereof |
| CN114613611A (en) * | 2022-03-23 | 2022-06-10 | 黄山学院 | Preparation method and application of oxygen-enriched hollow tubular porous carbon |
| CN116726877A (en) * | 2023-07-03 | 2023-09-12 | 河北省科学院能源研究所 | Preparation of biomass porous carbon and carbon dioxide adsorption application thereof |
| CN116726877B (en) * | 2023-07-03 | 2024-08-20 | 河北省科学院能源研究所 | Preparation of biomass porous carbon and carbon dioxide adsorption application thereof |
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