CN107364862A - Activated carbon for electric double layer capacitor electrode and its manufacture method - Google Patents
Activated carbon for electric double layer capacitor electrode and its manufacture method Download PDFInfo
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- CN107364862A CN107364862A CN201610429441.2A CN201610429441A CN107364862A CN 107364862 A CN107364862 A CN 107364862A CN 201610429441 A CN201610429441 A CN 201610429441A CN 107364862 A CN107364862 A CN 107364862A
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- China
- Prior art keywords
- activated carbon
- double layer
- layer capacitor
- electric double
- capacitor electrode
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 261
- 238000000034 method Methods 0.000 title claims abstract description 85
- 239000003990 capacitor Substances 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 41
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052796 boron Inorganic materials 0.000 claims abstract description 33
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- 125000000524 functional group Chemical group 0.000 claims abstract description 25
- 239000001301 oxygen Substances 0.000 claims abstract description 25
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 25
- 230000004913 activation Effects 0.000 claims abstract description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 238000001179 sorption measurement Methods 0.000 claims abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 31
- 239000002994 raw material Substances 0.000 claims description 24
- 239000002006 petroleum coke Substances 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- 239000012190 activator Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 244000060011 Cocos nucifera Species 0.000 claims description 6
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 239000012448 Lithium borohydride Substances 0.000 claims description 5
- 238000003763 carbonization Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000003245 coal Substances 0.000 claims description 3
- 239000000571 coke Substances 0.000 claims description 3
- 239000012279 sodium borohydride Substances 0.000 claims description 3
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 abstract description 15
- 238000012805 post-processing Methods 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 14
- 238000004140 cleaning Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 239000012535 impurity Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 5
- 229910001868 water Inorganic materials 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 4
- 125000000686 lactone group Chemical group 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 238000007086 side reaction Methods 0.000 description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 150000001339 alkali metal compounds Chemical class 0.000 description 3
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 241000234282 Allium Species 0.000 description 2
- 235000002732 Allium cepa var. cepa Nutrition 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- 239000006245 Carbon black Super-P Substances 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 229910010082 LiAlH Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 229920006311 Urethane elastomer Polymers 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- PPWPWBNSKBDSPK-UHFFFAOYSA-N [B].[C] Chemical class [B].[C] PPWPWBNSKBDSPK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229920000800 acrylic rubber Polymers 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000011335 coal coke Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000007603 infrared drying Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229920003049 isoprene rubber Polymers 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- BCVXHSPFUWZLGQ-UHFFFAOYSA-N mecn acetonitrile Chemical compound CC#N.CC#N BCVXHSPFUWZLGQ-UHFFFAOYSA-N 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 229920005670 poly(ethylene-vinyl chloride) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000009771 scanning electron microscopy-energy dispersive analysis Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005406 washing Methods 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
- H01G11/24—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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/33—Preparation characterised by the starting materials from distillation residues of coal or petroleum; from petroleum acid sludge
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/36—Reactivation or regeneration
- C01B32/366—Reactivation or regeneration by physical processes, e.g. by irradiation, by using electric current passing through carbonaceous feedstock or by using recyclable inert heating bodies
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
-
- 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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
-
- 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)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to activated carbon for electric double layer capacitor electrode and its manufacture method.The specific surface area BET using nitrogen adsorption method of the activated carbon for electric double layer capacitor electrode is 500~3,000m2/ g, and internally, surface or this include boron (B) at two, the weight of boron and carbon is below 15 weight % than B/C in activated carbon.In the present invention, the a large amount of oxygen-containing functional groups (OFGs) for being present in activated carbon surface after activation procedure are effectively reduced and removed by normal temperature wet method process, so as to improve economy and productivity, and minimized by reducing the specific surface area (BET) of the activated carbon after heat treatment, excellent initial capacity and life characteristic can be provided to possess its double layer capacitor.
Description
Technical field
The present invention relates to the activated carbon and its manufacture method of the electrode included for manufacturing double layer capacitor (EDLC).
Background technology
Activated carbon (activated carbon) is as composition double layer capacitor (electric double-layer
Capacitor, EDLC) electrode core material, device cost and aspect of performance in occupation of maximum proportion.
Such activated carbon generally manufactures by the following method：By carbonaceous such as petroleum, coal system coke or cocoanut shells
Raw material is handled and chemical activation with KOH or NaOH etc. aqueous slkali, or utilizes 900~1000 DEG C of gas (e.g., H2O
Or CO2) and activated.However, the surface of the activated carbon so manufactured can have metal impurities or oxygen-containing functional group, so as to deposit
Double layer capacitor performance reduce the problem of.That is, it is present in metal impurities or the oxygen-containing functional group meeting on the surface of activated carbon
The capacity of double layer capacitor is set to reduce (long term life as the factor for causing side reaction when double layer capacitor works
It can reduce).
It is such in order to solve the problems, such as, the method for manufacturing activated carbon via following process was proposed in the past：By activated carbon
Cleaned, removed so as to will be present in the metal impurities on the surface of activated carbon, Ran Houjin with acid solutions such as hydrochloric acid, sulfuric acid, nitric acid
Row neutralisation treatment.Such method is effective in terms of the metal impurities on the surface for being present in activated carbon are removed, but is being cleaned
During on the contrary can because produce carboxyl, lactone group, phenolic group, the oxygen-containing functional group such as carbonyl (oxygen functional group,
OFG) make the quantity of oxygen-containing functional group increase on the surface of activated carbon, thus deposited in the aspect of performance for improving double layer capacitor
Limiting to.
In order to reduce and remove foregoing oxygen-containing functional group (OFG), implemented in the past after activation procedure, at 700~1,000 DEG C
Scope carries out activated carbon the postprocessing working procedures of certain time heat treatment.However, such postprocessing working procedures not only need high price,
The heating furnace of high temperature and the additional incinerator for the ejected matter that burns, and running expense required during the said equipment operating
And maintenance cost is high, therefore it is noneconomic in terms of expense.In addition, the activated carbon by postprocessing working procedures is because of high warm
The specific surface area for handling and activated carbon occurring reduces, so as to necessarily cause the initial capacity of double layer capacitor (EDLC) to reduce.
The content of the invention
Problem to be solved
The present invention proposes to solve the problems, such as conventional art as described above, it is understood that in the activation procedure of activated carbon
Afterwards if being inorganic reducing agent from the boron (B) that can effectively reduce oxygen-containing functional group (OFG) and implementing normal temperature wet method process
To replace conventional high-temperature heat treatment, then it can not only reduce the specific surface area of the side effect as heat treatment and minimize, and
Unnecessary investment cost, operating and the maintenance cost of heat treatment step can be cut down.
Thus, it is an object of the present invention to provide effectively remove to contain while enabling specific surface area to reduce and minimize
The manufacture method of the activated carbon of oxygen functional group and the activated carbon for electric double layer capacitor electrode being produced from it.
The method for solving problem
To achieve these goals, the present invention provides a kind of activated carbon for electric double layer capacitor electrode, utilizes nitrogen adsorption method
Specific surface area (BET) be 500~3,000m2/ g, and internally, surface or this include boron (B) at two, in activated carbon boron with
The weight ratio (B/C) of carbon is below 15 weight %.
In the present invention, the oxygen-containing functional group (OFG) that above-mentioned activated carbon is preferably in surface is less than 0.5meq/g.
In addition, the present invention provides the manufacture method of foregoing activated carbon for electric double layer capacitor electrode.More specifically, it is above-mentioned
Manufacture method may include：(i) the step of carbon raw material being activated and manufacturing activated carbon；And (ii) exists the activated carbon of above-mentioned activation
The solution containing boron system (B) reducing agent is impregnated under normal temperature, the step of being then stirred and clean, and be dried.
In the present invention, the carbon raw material of above-mentioned steps (i) can be by selected from by coal system coke, petroleum coke and coconut palm
Material obtained by raw material carbonization in the group of sub- shell composition.
In the present invention, the activation of above-mentioned steps (i) can be the chemical activation using activator, or utilize H2O or CO2
Gas it is physically activated.
In the present invention, the boron system inorganic reducing agent of above-mentioned steps (ii) can be selected from by LiBH4And NaBH4The group of composition
One or more of.
In the present invention, the concentration of the solution containing boron system inorganic reducing agent of above-mentioned steps (ii) can be 0.1~2mol
Scope.
In the present invention, the manufacture method of activated carbon for electric double layer capacitor electrode is characterised by, at above-mentioned steps (ii)
In, in the case where activated carbon content is 20~80 weight % slurry form stir within 1~12 hour.
Invention effect
In the present invention, the oxygen-containing functional group of activated carbon surface can be will be present in no heat treatment process at normal temperatures
(OFG) effectively reduce and remove, it is thus possible to substantially reduce the original expense such as investment cost and operating.
In addition, in the present invention, by implementing normal temperature wet method process, the activated carbon of side effect as heat treatment can be made
Specific surface area, which reduces, to be minimized, so as to improve the double layer capacitor for possessing it (EDLC) initial capacity.
Embodiment
Hereinafter, the present invention is described in detail.
It is a feature of the present invention that activated carbon is manufactured using carbon raw material and via activation procedure, in above-mentioned activation work
After sequence, the oxygen-containing functional group (OFG) for implementing to will be present in activated carbon surface by normal temperature wet method process is effectively reduced and removed
Postprocessing working procedures.
That is, exist on the surface of the activated carbon of activation carboxyl (carboxylic group), lactone group (lactonic,
Cyclic ester group), the oxygen-containing functional group such as phenolic group (phenolic group).If the number of such oxygen-containing functional group
Amount increase, then in terms of EDLC elements, leakage current (Leakage Current) increase, self discharge (Self can be made
Discharge) performance reduces, and side reaction can be induced when applying voltage because electrolyte is directly contacted with OFG, so as to lead
Cause reliability to reduce to produce with gas.Therefore, limitation be present in the aspect of performance for improving double layer capacitor.
It is reducing agent from boron (B), by normal temperature as the inorganic reducing agent for postprocessing working procedures in the present invention
It is lower that using boron (B) to be reducing agent be present in a large amount of OFG of activated carbon surface to reduce and remove.
Above-mentioned boron (B) is that reducing agent is different from the organic reducing agent with toxicity (toxic), harmless.In addition, with
The aluminium (Al) of boron (B) (race of periodic table 13) of the same clan be inorganic reducing agent compared with boron (B) is inorganic reducing agent, although with stronger
Reducing power, but with the surface of activated carbon and the internal property largely remained, therefore blocking and live after postprocessing working procedures
Property charcoal stomata, and induce stomata in the reaction and cave in, initiation makes specific surface area (BET) significantly reduced side reaction.
Compared to this, the boron (B) selected is that reducing agent has can be by foregoing three kinds of oxygen-containing functional group parts in the present invention
Or the reducing power of Restore All, so that the OFG residual quantities of activated carbon surface are minimized afterwards, will not trigger as specific surface area
Side reaction as reduction.Therefore, by by conventional high-temperature heat treatment (post processing) process instead of normal temperature wet method process, can
The cost of technology and maintenance cost are cut down, furthermore it is possible to which the reduction of the specific surface area (BET) caused by making heat treatment is minimized and provided
Activated carbon with high initial capacity (F/g, F/cc).
In fact, the high-temperature heat treatment process implemented in manufacturing process in the present invention by abandoning conventional activated carbon,
The specific surface area of activated carbon reduces after can solving the problems, such as to be heat-treated while obtaining the cost of technology and cutting down effect, so as to
Enough show the capacity of double layer capacitor to maximize.Thus can be in terms of process time, expense and quality and conventional art
Compared to possessing competitiveness.
<Activated carbon for electric double layer capacitor electrode>
The activated carbon for electric double layer capacitor electrode of the present invention is because via the normal temperature wet method work using boron system inorganic reducing agent
Sequence, thus the inside of activated carbon, surface or this include boron (B) at two.
Specifically, the weight ratio (B/C) for the carbon that boron is included with above-mentioned activated carbon can be below 15 weight %, preferably
For 0.1~14.5 weight %, more preferably 1~10 weight % scopes.
As long as above-mentioned activated carbon can show that high-specific surface area and oxygen-containing functional group (OFG) minimizing effect just without special
Limitation.For example, the specific surface area (BET) using nitrogen adsorption method of above-mentioned activated carbon is 500~3,000m2/ g range, it is preferably
1,000~3,000m2/ g range.
In addition, the above-mentioned oxygen-containing functional group (OFG) for being present in activated carbon surface can be less than 0.5meq/g, preferably can be
Below 0.45meq/g, more preferably can be more than 0 and below 0.40meq/g.
Thus, manufactured in the activated carbon of the invention for being minimized the content by high-specific surface area and oxygen-containing functional group
Application of electrode is in the case of double layer capacitor, it is possible to increase the initial capacity of double layer capacitor, and length can be improved
Phase reliability of service life (floating ground and cycle performance (Floating＆Cycle Performance)).
<The manufacture method of activated carbon for electric double layer capacitor electrode>
Hereinafter, the manufacture method of the activated carbon according to an embodiment of the invention is illustrated.But and not only
It is limited to following manufacture methods, as needed can be by changing each operation the step of or carries out that selectivity is mixed to be implemented.
As a preferable embodiment for the method for manufacturing above-mentioned activated carbon, can include：(i) carbon raw material is lived
The step of changing and manufacturing activated carbon；And the activated carbon after above-mentioned activation is impregnated in dissolved with boron system reducing agent by (ii) at normal temperatures
Solution after, the step of being stirred and clean.
Hereinafter, above-mentioned manufacture method is illustrated respectively by each operation step, its content is as follows.
(1) activation procedure (hereinafter referred to as " S10 steps ")
In above-mentioned S10 steps, carbon raw material is activated and manufactures activated carbon.
Now, activation refers to, carbon raw material is modified as into the Porous formed with a large amount of stomatas (pore), so that comparing table
The increased process of area.
In the present invention, conventional substances known in the art can be used in above-mentioned carbon raw material, are not particularly limited.It is non-as its
Limitative examples, can be petroleum coke, coal coke, pitch, the plant (for example, cocoanut shell) of carbonization, the kind skin carbon of plant
Compound, synthetic resin (for example, phenolic resin Polymer material), graphene (graphene), CNT (Carbon
Nanotube), the material of the carbonization such as carbon onion (carbon onion).
Above-mentioned carbon raw material can be implemented as needed conventional pretreatment procedure known in the art, pulverizing process or
The material of all these processes.
In the present invention, above-mentioned pretreatment procedure includes all volatile materials that will be present in carbon raw material surface
The process that (volatile materials, VM) is removed.For example, the heat treatment of certain time can be carried out at 400~800 DEG C, or
Normal temperature wet method process is carried out using organic solvents such as non-polar solvens.Therefore, via the carbon raw material of above-mentioned pretreatment procedure
Real density can be less than 1.4g/cc, preferably can be below 1.38g/cc.In addition, the volatile materials in above-mentioned carbon raw material
(VM) content can be less than 2.0 weight % (400~700 DEG C), preferably can be more than below 0 and 1.5 weight %.
In addition, pulverizing process can be by using common disc mill (disk mill) known in the art, ball mill
(ball mill), rotation mill (rotary mill) and vibromill (vibration mill) etc. conventional method are carried out, preferred powder
It is broken into about 50~500 μm of sizes.
In the S10 steps according to the present invention, the method that above-mentioned carbon raw material activates is not particularly limited.It is such as favourable
With the chemical activation of the alkali salts such as KOH or NaOH (alkali metal compound) activator, or utilization high-temperature gas (H2O or CO2) physics
Activation etc..
In above-mentioned activation procedure, the blending ratio of carbon raw material powder and activator after crushing is not particularly limited, example
Such as can be with 1:0.1~10 weight ratio (that is, the coke powder after crushing:Activator=1:0.1~10 weight ratio) carry out
Mix and activate.It is preferred that with 1:2.0~3.0 weight ratio is mixed and activated.
In addition, when carrying out activation procedure, can after the carbon raw material powder after by above-mentioned crushing mixes with activator, with
400 DEG C~1,200 DEG C are heated and are carried out, and preferably can be 600~1,000 DEG C of temperature range.
On the other hand, the particle size of activated carbon is not particularly limited, and can be D10/D50/D90 (1~4 μm/5~11 μ
M/12~20 μm).
(2) washing/drying process (hereinafter referred to as " S20 steps ")
As needed, above-mentioned activated carbon can be via common cleaning known in the art and drying process.
Above-mentioned matting is carried out to will be present in the removal of the impurity of activated carbon.In matting, such as can
Carry out alkali cleaning, acid cleaning or these parallel cleanings, preferably parallel alkali cleaning and acid cleaning.
In addition, in the case of alkali metal compound (KOH etc.) is used as into activator in above-mentioned activation procedure, matting
Preferably at least include acid cleaning to remove above-mentioned alkali metal compound (KOH etc.) while removing and being present in the impurity of raw material
Deng.Now, as sour cleaning fluid, such as the aqueous acid such as hydrochloric acid or sulfuric acid can be used.In addition, can also carry out using go from
The matting of sub- water (deionized water).
After cleaning executed as described above, it is present in the moisture of activated carbon by drying to remove.Drying process does not limit especially
System, such as can be carried out by heated-air drying, natural drying or infrared drying.
(3) the normal temperature wet method postprocessing working procedures (hereinafter referred to as " S30 steps ") of inorganic reducing agent are utilized
If cleaned via the acid of foregoing S20 steps etc., the metal impurities on the surface of activated carbon can be reduced, opposite oxygen-containing
Functional group can increase, and such oxygen-containing functional group, which can turn into, makes the factor that the life characteristic of double layer capacitor (EDLC) reduces.
In the past, in order to remove oxygen-containing functional group (OFG), high-temperature heat treatment process (600~1000 DEG C) is implemented, but warm in such height
After processing, not only the specific surface area of activated carbon reduces and causes the initial capacity of double layer capacitor to reduce, and triggers economical
Property and productivity reduce.
Thus, in the S30 steps of the present invention, activated carbon is impregnated in dissolved with boron system inorganic reduction by implementation at normal temperatures
After the solution of agent, the postprocessing working procedures that are stirred and clean in the slurry state.Therefore, it is possible to will be present in the activity of activation
The oxygen-containing functional group of carbon surface is effectively reduced and removed, in fact, with conventional high-temperature heat treatment process (600~1000 DEG C) phase
Than being capable of OFG that is more efficient and removing activated carbon surface.
As the inorganic reducing agent of the present invention, using can be by 1) carboxyl, 2) lactone group and the 3) oxygen-containing functional group such as phenolic group
(OFG) part or all of 13 boron family of race (B) compound for reducing and removing in.As its specific example, can be selected from
By LiBH4And NaBH4One or more of group of composition.
As long as oxygen-containing functional group (OFG) can effectively reduce and removed by the usage amount of above-mentioned boron system inorganic reducing agent,
It can easily remove by follow-up cleaning minimum, just be not particularly limited simultaneously.For example, above-mentioned steps (ii's) contains
The concentration of the solution of boron system inorganic reducing agent can be 0.1~2mol scopes.
As the preferable example of above-mentioned S30 steps, above-mentioned activated carbon can be put into dissolved with inorganic reduction at normal temperatures
The solution (0.1~2mol) of agent, by the basis of the slurry 100 weight % activated carbon content be 20~80 weight % slurry enter
Row stirring in 1~12 hour and cleaning, and be dried and obtain final activated carbon.Now, meet the above-mentioned weight %'s of slurry 100
Surplus can be the weight of the solution (0.1~2mol) dissolved with inorganic reducing agent, such as can be 80~20 weight % scopes.
If via as above postprocessing working procedures, can the inside of activated carbon, surface or this at two part residual boron system without
Machine reducing agent.Especially since boron system inorganic reducing agent mainly be present in activated carbon surface OFG react, therefore with activity
The inside of charcoal is compared, and can largely be present in surface.For example, it is activated carbon after inorganic reducing agent implements postprocessing working procedures with boron (B)
Interior B/C weight % maximums can be below 15 weight %, preferably 0.1~14.5 weight % scopes.
(4) classification/de-iron process (hereinafter referred to as " S40 steps ")
As needed, granularity can be adjusted by crushing the activated carbon of post processing.
Now, it can make activated carbon that there is 3 μm~7 μm of particle mean size in granularity regulation.In particular, by above-mentioned work
After property charcoal Crushing of Ultrafine, by being sorted, to make it have the particle mean size of 3 μm~7 μm sizes.Now, classification can make
It is carried out by sieving (sieve).In the case of with so appropriately sized size distribution, tap density (Tap
Density) uprise, output characteristics is improved.
<Electric double layer capacitor pole>
The present invention provides the electric double layer capacitor pole for including above-mentioned activated carbon.
Specifically, electric double layer capacitor pole of the invention include described above activated carbon and conductive material,
Adhesive and collector.
As long as above-mentioned conductive material material well known in the art, is just not particularly limited, can as non-limitative example
Use carbon black, graphite, CNT etc..As long as above-mentioned adhesive material well known in the art, is just not particularly limited, as
Non-limitative example, it can be used PTFE (polytetrafluoroethylene (PTFE)), CMC (carboxymethyl cellulose), PVA (polyvinyl alcohol), PVDF (poly- inclined
PVF), PVP (polyvinylpyrrolidone), MC (methylcellulose), SBR (butadiene-styrene rubber), ethylene-vinyl chloride copolymer resins,
Vinylidene chloride latex, chlorinated resin, vinyl acetate resin, polyvinyl butyral resin, polyvinyl formal bis-phenol system asphalt mixtures modified by epoxy resin
Fat, butadiene rubber, isoprene rubber, nitrile rubber, urethane rubber, organic silicon rubber, acrylic rubber etc..
As long as the manufacture method method well known in the art of such electric double layer capacitor pole of the invention, does not just have
There is special limitation.
<Double layer capacitor>
The present invention provides the double layer capacitor for including above-mentioned electric double layer capacitor pole.
Specifically, double layer capacitor of the invention have the electrode of described above by barrier film be configured as negative electrode and
Anode, the negative electrode configured and anode are impregnated in the structure of electrolyte.
Such double layer capacitor of the invention includes the electrode manufactured by foregoing active charcoal, therefore has high power capacity,
Cycle characteristics is excellent.
Hereinafter, the present invention is illustrated by embodiment, but following embodiments and experimental example only illustrate one of the present invention
Form, the scope of the present invention are not limited by following embodiments and experimental example.
[embodiment 1]
Embodiment 1-1
By carbon raw material (petroleum coke) and activator (KOH) with 1:2.6 weight rates carry out chemical activation, and carry out
Clean and dry, so as to manufacture activated carbon.Afterwards, it is impregnated at normal temperatures dissolved with nothing via by the activated carbon 15g after cleaning
Machine reducing agent LiBH4THF solution (concentration 2mol) 100ml, then carry out 12 hours stir, be dried after being cleaned
Postprocessing working procedures, manufacture particle mean size are the activated carbon of 8 μm of sizes.
Embodiment 1-2
Using the activated carbon of above-mentioned manufacture, electrode material for electric double layer capacitor is used as.
In particular, using activated carbon, the carbon black (super P (Super-P) etc.) as conductive agent, as adhesive
CMC and SBR are with 90:5:1.5:3.5 weight after input than being mixed, so as to manufacture slurry.By the slurry of manufacture in Al paper tinsels
Upper progress unfilled corner wheel coating and after manufacturing electrode, itself and barrier film (NKK companies, the paper pulp material of 35 μ m thicks) are together wound into
2032- button cells (Coin Cell) form, so as to manufacture the double layer capacitor with about 1F ranges of capacity.Now, as
Electrolyte, use the material of the organic system acetonitrile (acetonitrile) of the TEABF4 (tetraethyl ammonium tetrafluoroborate) containing 1M.
[embodiment 2]
As inorganic reducing agent, NaBH is used4Instead of LiBH4, in addition, implement in the same manner as above-described embodiment 1, from
And manufacture the petroleum coke activated carbon of embodiment 2 and possess its double layer capacitor.
[comparative example 1]
Without using inorganic reducing agent, but implement be mixed with the volume % of hydrogen 2 and the volume % of nitrogen 98 mixed gas
Under the conditions of the postprocessing working procedures of heat treatment in 1 hour are carried out with 700 DEG C of temperature, it is in addition, real in the same manner as above-described embodiment 1
Apply, so as to manufacture the petroleum coke activated carbon of comparative example 1 and possess its double layer capacitor.
[comparative example 2]
Do not implement postprocessing working procedures, in addition, implementation and the identical method of above-described embodiment 1, so as to manufacture comparative example 2
Petroleum coke activated carbon and possess its double layer capacitor.
[comparative example 3]
Petroleum coke raw material is replaced using coconut system raw material, and passes through gas (H2O or CO2) carry out physically activated and make
Make activated carbon, in addition, according to the above-mentioned identical method of comparative example 1, manufacture comparative example 3 coconut system activated carbon and possess
Its double layer capacitor.
[comparative example 4]
As inorganic reducing agent, LiAlH is used4, in addition, implement in the same manner as above-described embodiment 1, so as to manufacture ratio
Compared with example 4 petroleum coke activated carbon and possess its double layer capacitor.
[Boron contents are analyzed in the activated carbon of experimental example 1.]
The content of the composition included using the activated carbon of SEM-EDAX analysis embodiments 1, and the results are shown in following
Table 1.
[table 1]
Experimental result, it is known that include boron in the activated carbon of embodiment 1 (with reference to table 1).
[physical property and the electrochemical properties evaluation of the activated carbon after the postprocessing working procedures of experimental example 2.]
The activated carbon physical property manufactured in embodiment 1~2 and comparative example 1~4 is evaluated as follows, and the results are shown in
Table 2 below.
(1) specific surface area (m2/g)：0.5g activated carbon or its raw material are subjected to drying in 30 minutes in 2 hours at 250 DEG C,
So as to which the moisture in the stomata present in the surface of activated carbon and activated carbon be removed completely, then make its absorption nitrogen (N2),
The amount of the adsorbed nitrogen of measure, so as to be converted into per unit weight surface area.
(2) oxygen-containing functional group (meq/g)：After pKa value alkali different from each other is mixed with activated carbon, make itself and activity
Oxygen-containing functional group (carboxyl, the lactone group, phenolic group) reaction of carbon surface, and the amount of remaining alkali is anti-with 0.1N HCl standard liquids
Titrate (back-titration) and carry out quantitative Boehm methods to determine (used alkali：0.1N NaOH).
(3) Unit Weight capacity (F/g)：It is overall according to following computing units of mathematical expression 1 from the discharge curve of EDLC units
C [F] after, the weight of the activated carbon added during manufacturing is divided and calculated.
[mathematical expression 1]
C [F]=(I [mA] × Δ t [sec])/Δ V [V]
(wherein, the difference of 40%, 80% value of Δ t and Δ V expression rated voltages (rated voltage))
(4) unit volume capacity (F/cc)：The density (g/cc) of the electrode of manufacture is multiplied with the above-mentioned F/g tried to achieve and counted
Calculate.
[table 2]
Experimental result, it is known that via the postprocessing working procedures using boron system inorganic reducing agent embodiment 1~2 activated carbon with
Comparative example 1~4 is compared, while has high-specific surface area, low OFG contents and excellent electrochemical properties (with reference to table 2).
Now, be not carried out the comparative example 2 of postprocessing working procedures activated carbon show specific surface area and electrochemical properties (F/g,
F/cc it is) excellent, but OFG content is very high.Understand such high OFG contents cause the activated carbon of comparative example 2 applied to
Life characteristic significantly reduces and can not carry out commercialization during EDLC.
In addition, the feelings for using with the aluminium (Al) of the race of boron (B) identical periodic table 13 comparative example 4 for being inorganic reducing agent
For condition, excellent effect is shown in terms of OFG reduction and removal, but following phenomenon occur：On the surface of activated carbon and
The a large amount of Al of internal residual and block the stomata of activated carbon, and in the reaction induce caving in for stomata and make specific surface area (BET)
Significantly reduce.The activated carbon of such comparative example 4 is understood when applied to double layer capacitor (EDLC), in Unit Weight capacity
(F/g) inferior characteristic and in terms of unit volume capacity (F/cc) is shown, so as to almost there is no yield production type.
Claims (10)
1. a kind of activated carbon for electric double layer capacitor electrode, the specific surface area BET using nitrogen adsorption method is 500~3,000m2/ g,
And internally, surface or this include boron (B) at two, the weight of boron and carbon is below 15 weight % than B/C in activated carbon.
2. activated carbon for electric double layer capacitor electrode according to claim 1, it is characterised in that be present in the oxygen-containing of surface
Functional group OFG is less than 0.5meq/g.
3. a kind of electrical double layer capacitor electrodes, it includes the activated carbon described in claim 1 or 2.
4. a kind of double layer capacitor, it possesses the electrode described in claim 3.
5. a kind of manufacture method of activated carbon for electric double layer capacitor electrode, it includes：
(i) the step of carbon raw material being activated and manufacturing activated carbon；And
(ii) activated carbon after the activation is put into the solution containing boron system inorganic reducing agent at normal temperatures, and in slurry form
Under be stirred and clean, the step of being then dried.
6. the manufacture method of activated carbon for electric double layer capacitor electrode according to claim 5, the carbon raw material be by
What the raw material carbonization in the group being made up of coal system coke, petroleum coke and cocoanut shell formed.
7. the manufacture method of activated carbon for electric double layer capacitor electrode according to claim 5, it is characterised in that the step
Suddenly (i) implements to utilize the chemical activation of activator or utilizes H2O or CO2Gas it is physically activated.
8. the manufacture method of activated carbon for electric double layer capacitor electrode according to claim 5, it is characterised in that the step
Suddenly the boron system inorganic reducing agent of (ii) is selected from by LiBH4And NaBH4The group of composition.
9. the manufacture method of activated carbon for electric double layer capacitor electrode according to claim 5, it is characterised in that the step
Suddenly the concentration of the solution containing boron system inorganic reducing agent of (ii) is 0.1~2mol scopes.
10. the manufacture method of activated carbon for electric double layer capacitor electrode according to claim 5, it is characterised in that described
The slurry that activated carbon content is 20~80 weight % stir within 1~12 hour in step (ii).
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| CN111433872A (en) * | 2017-12-19 | 2020-07-17 | 韩国东海炭素株式会社 | Preparation method of activated carbon for electrode material |
| CN112707397A (en) * | 2020-12-30 | 2021-04-27 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Preparation method of super-capacitor activated carbon |
| CN114203460A (en) * | 2022-02-18 | 2022-03-18 | 天津普兰能源科技有限公司 | Manufacturing method of capacitor electrode and manufacturing method of capacitor |
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| KR102539683B1 (en) * | 2020-02-28 | 2023-06-02 | 한국화학연구원 | Preparation method for activated carbon with multi pore structure and activated carbon with multi pore structure prepared by the same |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111433872A (en) * | 2017-12-19 | 2020-07-17 | 韩国东海炭素株式会社 | Preparation method of activated carbon for electrode material |
| CN111433872B (en) * | 2017-12-19 | 2021-11-19 | 韩国东海炭素株式会社 | Preparation method of activated carbon for electrode material |
| CN112707397A (en) * | 2020-12-30 | 2021-04-27 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Preparation method of super-capacitor activated carbon |
| CN114203460A (en) * | 2022-02-18 | 2022-03-18 | 天津普兰能源科技有限公司 | Manufacturing method of capacitor electrode and manufacturing method of capacitor |
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