CN107039193A - A kind of garlic skin matrix activated carbon electrode material and preparation method for ultracapacitor - Google Patents
A kind of garlic skin matrix activated carbon electrode material and preparation method for ultracapacitor Download PDFInfo
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- CN107039193A CN107039193A CN201710243663.XA CN201710243663A CN107039193A CN 107039193 A CN107039193 A CN 107039193A CN 201710243663 A CN201710243663 A CN 201710243663A CN 107039193 A CN107039193 A CN 107039193A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 151
- 235000004611 garlic Nutrition 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000007772 electrode material Substances 0.000 title claims abstract description 20
- 239000011159 matrix material Substances 0.000 title claims abstract description 14
- 244000245420 ail Species 0.000 title 1
- 240000002234 Allium sativum Species 0.000 claims abstract description 95
- 238000001994 activation Methods 0.000 claims abstract description 52
- 230000004913 activation Effects 0.000 claims abstract description 49
- 239000000463 material Substances 0.000 claims abstract description 49
- 239000005539 carbonized material Substances 0.000 claims abstract description 27
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract description 19
- 239000003610 charcoal Substances 0.000 claims abstract description 17
- 238000007598 dipping method Methods 0.000 claims abstract description 17
- 238000010792 warming Methods 0.000 claims abstract description 16
- 229910001854 alkali hydroxide Inorganic materials 0.000 claims abstract description 5
- 238000012805 post-processing Methods 0.000 claims abstract description 5
- 238000001802 infusion Methods 0.000 claims abstract description 4
- 238000009413 insulation Methods 0.000 claims abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 60
- 239000000243 solution Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 238000005554 pickling Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000012047 saturated solution Substances 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 230000002745 absorbent Effects 0.000 abstract description 5
- 239000002250 absorbent Substances 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 description 22
- 229910052783 alkali metal Inorganic materials 0.000 description 12
- 150000001340 alkali metals Chemical class 0.000 description 12
- 230000000694 effects Effects 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000012153 distilled water Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 239000012190 activator Substances 0.000 description 7
- 239000003990 capacitor Substances 0.000 description 7
- 239000003792 electrolyte Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000005416 organic matter Substances 0.000 description 6
- 239000002956 ash Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 239000002028 Biomass Substances 0.000 description 4
- 230000003213 activating effect Effects 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000006258 conductive agent Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000010431 corundum Substances 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000010903 husk Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- 235000017060 Arachis glabrata Nutrition 0.000 description 2
- 244000105624 Arachis hypogaea Species 0.000 description 2
- 235000010777 Arachis hypogaea Nutrition 0.000 description 2
- 235000018262 Arachis monticola Nutrition 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002154 agricultural waste Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012620 biological material Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 235000020232 peanut Nutrition 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- 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 1
- 240000007049 Juglans regia Species 0.000 description 1
- 235000009496 Juglans regia Nutrition 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012611 container material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- -1 timber Substances 0.000 description 1
- 235000020234 walnut Nutrition 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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
- C01P2006/14—Pore volume
-
- 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
- Y02E60/13—Energy storage using capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a kind of garlic skin matrix activated carbon electrode material and preparation method for ultracapacitor.Garlic skin is heated to 550~700 DEG C under an inert atmosphere, insulation a period of time carries out charing and obtains garlic skin carbonized material, garlic skin carbonized material is added to alkali hydroxide soln high temperature time of infusion again and obtains dipping material, then dipping material is warming up to 400~450 DEG C of progress low-temperature activations, low-temperature activation continues to be heated to 700~850 DEG C of progress high-temperature activations for a period of time afterwards, high-temperature activation obtains activated material afterwards for a period of time, and activated material progress post processing finally is produced into activated carbon.Activated carbon can be made to activate completely, increase the specific surface area of absorbent charcoal material, improve the energy density of ultracapacitor.
Description
Technical field
The present invention relates to super active carbon material technical field, and in particular to a kind of garlic skin base for ultracapacitor is lived
Property carbon electrode material and preparation method.
Background technology
Ultracapacitor (also referred to as electrochemical capacitor, double layer capacitor) is one kind between traditional capacitor and battery
Between new type of energy storage device, it has high-energy-density, and high power density has extended cycle life, and fast charging and discharging is economic and environment-friendly
The advantages of.There is of crucial importance and wide answer in multiple fields such as information technology, electric automobile, Aero-Space and science and techniques of defence
Use prospect.Wherein, electrode material is the critical material for determining performance of the supercapacitor index.
Activated carbon, as a kind of porous carbon material, because its specific surface area is big, pore structure abundant, stable chemical performance, easily anti-
Multiple use, preparation technology simple flow, it is cheap the advantages of, environmental protection, science and techniques of defence, chemical industry, food processing,
There is important application in the fields such as medical and health.China natural resources are enriched, and are production and the big export country of activated carbon.With the fast of production
Speed development, the application of various composites of the activated carbon and based on activated carbon in itself will be further expanded, activity
The consumption of charcoal also will constantly increase.Especially electric capacity is huge with the super-activated carbon market demand, but domestic production amount very little, portion big absolutely
Divide dependence on import.
Biomass is that a kind of important activated carbon prepares raw material, conventional mainly traditional agriculture and forestry biomass, bag
Include various crop stalks, timber, shell, fruit stone, rice husk etc..Such biological material is generally agriculture and forestry product discarded object, cost
It is cheap and content of ashes is low, it is internal to have many holes again, easily enter activator, reactivity worth is good, is conducive to hole knot
The formation of structure, high mechanical strength is the excellent material for preparing activated carbon, with wide market prospects.
At present in the various electrode materials of ultracapacitor, prepared by raw material of biomass by chemical activation method
Carbon material has higher specific surface area, is a kind of ideal electrode material for super capacitor.Chi-Chang Hu et al.
Its specific surface area is improved by chemical activation as raw material using Fructus Pistaciae Verae shell, but specific capacitance under speed is swept in 300mv/s height
Although only 47F/g (Electrhimica Acta52 (2007) 2498-2505), activated carbon prepared by this kind of method has higher
Specific surface area, but its specific capacitance value decays relatively serious at higher current densities, is not suitable for the operating condition under high current
Under use.
Chinese patent (publication number CN102417179A), which is disclosed, uses peanut shell for raw material, and activation process is carried out with KOH,
The specific surface area of gained absorbent charcoal material reaches 1227m2/ g, it shows preferable stability as capacitor electrode material.
But it is above-mentioned in the prior art using straw, timber, shell, fruit stone, the biomass such as rice husk as preparing capacitor
The raw material of electrode activity charcoal, the specific surface area that there is the absorbent charcoal material that the activation effect using activator is poor, prepare is smaller,
The problems such as being difficult to be adjusted the pore structure and specific surface area of activated carbon.
The content of the invention
In order to overcome the defect of prior art, one of mesh of the invention there is provided garlic skin and prepare the work of ultracapacitor
Application in property carbon electrode material.
China is agricultural production big country in the world, and substantial amounts of agricultural wastes are produced every year.It is very big in these discarded objects
A part is simply discarded, have impact on environment it is attractive in appearance, the pollution of environment is possibly even caused, while being also the very big wave of resource
Take.China is as the original producton location of garlic, and the plantation to garlic is with a long history, and cultivated area is big.However, due to traditional habit,
Garlic it is edible during most only selection garlics meats use, Cortex Bulbus Allii is often abandoned as processing byproduct.Cause resource wave
Take.The present inventor has found that garlic skin has natural pore structure by studying, while containing abundant mineral in garlic skin
Matter, these mineral matters can play certain activation instead of activator, so that activated carbon is activated completely.Garlic skin prepares super
Level activated carbon, agricultural wastes high-qualityization can be utilized, both expanded industrial chain added value, a kind of super capacitor can be obtained again
Use high performance electrode material.
In order to realize application of the garlic skin in the active carbon electrode material of ultracapacitor is prepared, increase absorbent charcoal material
The purposes such as specific surface area, the second object of the present invention is to provide a kind of garlic skin matrix activated carbon electrode material for ultracapacitor
Preparation method, activated carbon can be made to activate completely, increase absorbent charcoal material specific surface area, improve ultracapacitor energy
Density.
To achieve these goals, the technical scheme of preparation method of the invention is：
A kind of preparation method of garlic skin matrix activated carbon electrode material for ultracapacitor, by garlic skin under an inert atmosphere
550~700 DEG C are heated to, insulation a period of time carries out charing and obtains garlic skin carbonized material, then garlic skin carbonized material is added to alkali gold
Belong to hydroxide solution high temperature time of infusion and obtain dipping material, dipping material then is warming up into 400~450 DEG C enters
Row low-temperature activation, low-temperature activation continues to be heated to for a period of time 700~850 DEG C of progress high-temperature activations afterwards, during one section of high-temperature activation
Between after obtain activated material, finally by activated material progress post processing produce activated carbon.
The present invention, first, activated carbon is prepared using garlic skin, by being heated to 550~700 DEG C of charings to organic in garlic skin
Thing is pyrolyzed, and is changed the architectural feature and garlic skin pore character of organic matter, is obtained the garlic with certain hole and mechanical strength
Skin carbonized material is used as intermediate material.Secondly, garlic skin carbonized material is etched using alkali metal hydroxide as activator, on the one hand,
Low-temperature activation is carried out at 400~450 DEG C, the carbonate of generation alkali metal makes Pore development, on the other hand, 700~850 DEG C of progress
High-temperature activation, this temperature is higher than the boiling point of alkali metal, makes alkali metal formation vapour of an alkali metal, and vapour of an alkali metal can diffuse into difference
Carbon-coating, form new pore structure；Gaseous alkali metal is walked between the synusia of crystallite, struts its change that is distorted such as direction synusia
Shape, develops new micropore.3rd, decompose in alkali metal hydroxide activation process and produce CO2Deng gas, these gases can rise
To the progress of further promotion activation, the specific surface area of activated carbon is greatly increased, the quality and adsorptivity of activated carbon is improved
Energy.
The third object of the present invention is to provide activated carbon prepared by a kind of above-mentioned preparation method.
Activated carbon activation produced by the present invention is complete, and its specific surface area is up to 2818.22m2/ g, can provide the suction of more multipotency
The avtive spot of attached electric charge, is conducive to improving the energy density of ultracapacitor；Its pore volume is up to 1.32cm3/ g, pore-size distribution
Concentrate within 4nm, it is adjustable in pore-size distribution and porosity certain limit.
The fourth object of the present invention is to provide a kind of garlic skin matrix activated carbon electrode material for ultracapacitor, using upper
Activated carbon is stated to be prepared.
The fifth object of the present invention is to provide a kind of application of above-mentioned activated carbon in ultracapacitor.
First, the activated carbon that prepared by the present invention is applicable to various electrolyte systems, and is provided for the ion in electrolyte
Quick passage, makes it have more excellent high current charge-discharge ability and its energy density.Secondly, the activity that prepared by the present invention
Charcoal ash are point low, and wellability is good, be assembled into two electrode system double electric layers supercapacitors have higher specific capacitance, less etc.
Series resistance, higher efficiency for charge-discharge, and low time constant are imitated, discharge and recharge has higher particularly under high magnification
Energy density etc..
Beneficial effects of the present invention are：
1. garlic skin material itself has abundant fiber conduit, with other biological materials such as coconut husk, peanut shell, walnut shell phase
Than being more beneficial for obtaining larger specific surface area providing the storage area of electric charge, garlic skin matrix activated carbon specific surface area is up to
2800m2/g；Similarly serving to favor rational hole and pore-size distribution, (garlic skin base is lived to balance the requirement between specific capacitance and high rate performance
Property charcoal aperture integrated distribution in 0.6~1nm, what electric capacity was played a major role is the enterable micropore of ion, aperture be 0.5~
2nm)；
2. the invention provides a kind of ultracapacitor garlic skin matrix activated carbon material and preparation method thereof, using orthogonal reality
The method of testing have studied carbonization temperature, carbonization time, alkali carbon ratio, activation temperature, soak time to activated carbon specific surface area and aperture
Influence, the purpose is to reach the most probable pore size (0.5~2nm of aperture) of most suitable electron channel by aperture control, is carried
High electrochemical performance；
3. the electrode material ash content that the present invention is provided is low, series resistance is small, and conductance height ensures high rate charge-discharge
Can (such as Fig. 6) and high power density (power density is 3307.64W/kg when energy density is 8.79Wh/kg)；Good infiltration
Property to promote ion to spread, increase ion accessible surface product；
4. can prepare the ultracapacitor under high current use condition using the activated carbon of the present invention, it is in water system
Under electrolyte conditions, current density is 0.5A/g, 1.0A/g, 2.0A/g, 3.0A/g, and the specific capacitance under 5.0A/g is respectively reached
318.67F/g, 284.53F/g, 269.33F/g, 262.51F/g, 253.01F/g.
5. professional application of the present invention is strong, and design technology process is simple, and cost is relatively low, clean environment firendly, it is easy to industry
Change and realize.
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrate be used for explain the application, do not constitute the improper restriction to the application.
Fig. 1 is the stereoscan photograph of activated carbon made from embodiment 1；
Fig. 2 is the N of activated carbon made from embodiment 12Adsorption/desorption figure；
Fig. 3 is activated carbon pore size distribution map made from embodiment 1；
Fig. 4 is activated carbon capillary graph of pore diameter distribution made from embodiment 1；
Fig. 5 is the constant current charge-discharge curve under 0.5A/g electric currents of activated carbon electrodes prepared by embodiment 1；
Fig. 6 be embodiment 1 prepare activated carbon electrodes in 5mV/s, 10mV/s, 20mV/s, 50mV/s, 100mV/s's sweeps
Retouch the cyclic voltammetry curve under speed；
Fig. 7 is 5000 cycle performances of activated carbon electrodes prepared by embodiment 1 (assay method is constant current charge-discharge).
Embodiment
It is noted that described further below is all exemplary, it is intended to provide further instruction to the application.Unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
Heretofore described low-temperature activation refers to the step of being activated for 400~450 DEG C, and described high-temperature activation
Refer to 700~850 DEG C the step of activated.
Unit " M " expression " mol/L " in the present invention.
The step of heretofore described high temperature dipping refers to the dipping that temperature is 80~100 DEG C.
As background technology is introduced, there is that the activation effect using activator is poor, activated carbon is lived in the prior art
Change incomplete defect, in order to solve technical problem as above, the activity of ultracapacitor is being prepared present applicant proposes garlic skin
Application in carbon electrode material.
The present inventor has found that garlic skin has natural pore structure by studying, while containing what is enriched in garlic skin
Mineral matter, these mineral matters can play certain activation instead of activator, so that activated carbon is activated completely.Utilize garlic
The raw material that skin is prepared as activated carbon, had both solved the utilization of discarded object high-qualityization, solved that to prepare a kind of absorption property excellent again
Environmental protection, energy and material.
There is provided a kind of garlic skin matrix activated carbon electricity for ultracapacitor in a kind of typical embodiment of the present invention
The preparation method of pole material, garlic skin is heated under an inert atmosphere 550~700 DEG C, insulation a period of time carries out charing acquisition
Garlic skin carbonized material, then garlic skin carbonized material is added into alkali hydroxide soln high temperature time of infusion impregnated
Material, is then warming up to 400~450 DEG C of progress low-temperature activations by dipping material, and low-temperature activation continues to be heated to for a period of time afterwards
700~850 DEG C of progress high-temperature activations, high-temperature activation obtains activated material, is finally post-processed activated material i.e. afterwards for a period of time
Obtain activated carbon.
First, activated carbon is prepared using garlic skin, the organic matter in garlic skin carried out by being heated to 550~700 DEG C of charings
Pyrolysis, changes the architectural feature and garlic skin pore character of organic matter, obtains with certain hole and the charing of the garlic skin of mechanical strength
Material is used as intermediate material.Secondly, garlic skin carbonized material is etched using alkali metal hydroxide as activator, on the one hand, 400~
450 DEG C of progress low-temperature activations, the carbonate of generation alkali metal makes Pore development, on the other hand, 700~850 DEG C of progress high temperature work
Change, this temperature is higher than the boiling point of alkali metal, make alkali metal formation vapour of an alkali metal, vapour of an alkali metal can diffuse into different carbon
Layer, forms new pore structure；Gaseous alkali metal is walked between the synusia of crystallite, struts its deformation that is distorted such as direction synusia,
Develop new micropore.3rd, decompose in alkali metal hydroxide activation process and produce CO2Deng gas, these gases can be played
Further promote the progress of activation, greatly increase the specific surface area of activated carbon, improve the quality and absorption property of activated carbon.
In order to which garlic skin charing efficiency will be improved, it is preferred that carry out charing process after garlic skin is pre-processed.
It is further preferred that the step of pretreatment is, takes garlic skin to dry or dry for the first time after cleaning, crush, mistake
80 mesh sieves.Garlic skin charing efficiency can further be improved.
Still more preferably, the temperature dried is 20~30 DEG C, and the temperature of the drying is 100~110 DEG C.
It is preferred that, the heating rate for being heated to 550~700 DEG C is 5 DEG C/min, and soaking time is 2~5h.It ensure that garlic
Organic matter in skin is pyrolyzed completely.
Above-mentioned inert atmosphere refers to the one or more in nitrogen, argon gas, helium.
It is preferred that, the alkali hydroxide soln is the saturated solution of alkali metal hydroxide.Garlic skin charcoal can be made
Material can impregnate more alkali metal hydroxides.
It is preferred that, alkali metal hydroxide is one or both of potassium hydroxide, sodium hydroxide.Potassium hydroxide, hydrogen-oxygen
That changes sodium compares otheralkali metal hydroxide, and abundance, cost is relatively low.
It is preferred that, the mass ratio of alkali metal hydroxide and garlic skin carbonized material is 3.0~4.5:1.
It is preferred that, the temperature of the dipping is 80 DEG C, and the time of the dipping is 2h.Alkali metal hydroxide at this temperature
Molecular motion performance it is higher, alkali metal hydroxide can be made to rapidly enter in garlic skin carbonized material.2h ensure that enough
Alkali metal hydroxide is entered in garlic skin carbonized material.
It is preferred that, it is 5 DEG C/min to be warming up to 400~450 DEG C and be warming up to 700~850 DEG C of heating rate.
It is preferred that, the time of the low-temperature activation is 45min.
It is preferred that, the time of the high-temperature activation is 1~2.5h.
It is preferred that, the post processing includes washing for the first time, pickling, second of washing, second of drying, grinding successively.
Washing for the first time described in present embodiment, second washing be in order to represent water-washing steps different twice, and
Be not configured to limit the precedence of water-washing step.
Drying for the first time described in present embodiment, second drying be in order to represent baking steps different twice, and
Be not configured to limit the precedence of baking step.
It is further preferred that the temperature of the first time washing and second of washing is 80 DEG C.
Enter preferred, concretely comprising the following steps for the pickling is washed till pH 6~7 using acid solution at 80 DEG C.
It is further preferred that the concentration for the acid solution that the pickling is used is 0.1M.Prevent acid solutions too high, destroy
The hole of activated carbon, so as to reduce the specific surface area of activated carbon.
It is further preferred that the acid solution is the one or more in hydrochloric acid, sulfuric acid, nitric acid.
Present embodiment additionally provides activated carbon prepared by a kind of above-mentioned preparation method.
Obtained activated carbon activation is complete, and specific surface area is up to 2818.22m2/ g super-activated carbon, can be provided more
The active sites of energy adsorption charge, are conducive to improving the energy density of ultracapacitor；Pore volume is up to 1.32cm3/ g, pore-size distribution
Concentrate within 4nm, it is adjustable in pore-size distribution and porosity certain limit.
Present embodiment additionally provides a kind of garlic skin matrix activated carbon electrode material for ultracapacitor, using above-mentioned work
Property charcoal is prepared.
Present embodiment additionally provides a kind of application of above-mentioned activated carbon in ultracapacitor.
First, the activated carbon that prepared by the present invention is applicable to various electrolyte systems, and is provided for the ion in electrolyte
Quick passage, makes it have more excellent high current charge-discharge ability and its energy density.Secondly, the activity that prepared by the present invention
Charcoal ash are point low, and wellability is good, be assembled into two electrode system double electric layers supercapacitors have higher specific capacitance, less etc.
Series resistance, higher efficiency for charge-discharge, and low time constant are imitated, discharge and recharge has higher particularly under high magnification
Energy density etc..
In order that the technical scheme of the application can clearly be understood by obtaining those skilled in the art, below with reference to tool
The embodiment of body describes the technical scheme of the application in detail with comparative example.
Raw material explanation：The raw material garlic skin used in following examples, is derived from Shandong Jinxiang, wherein moisture account for 3.2~
3.6wt%, 4.5~4.9wt% of ash content, 91.5~92.3wt% of organic matter, organic matter is mainly cellulose and lignin.
Embodiment 1
Take garlic skin to dry or dry after cleaning, crush, cross 80 mesh sieves, garlic skin powder is made；Garlic skin powder is positioned over tubular type
In resistance furnace, 600 DEG C are heated under inert atmosphere (flow is 2L/min), heating rate is 5 DEG C/min, are incubated 2h, cooling
To room temperature, garlic skin carbonized material is made；At room temperature, it is 4 according to the mass ratio of KOH solids and garlic skin carbonized material:1, take garlic skin to carbonize
Expect 6g, corresponding KOH solids be 24g, saturation KOH solution is thoroughly mixed with garlic skin carbonized material, after put it into air blast
Drying box impregnates 2h, material after must impregnating with 80 DEG C of high temperature；Material after dipping is put into Muffle furnace to be activated, from room temperature to rise
Warm 5 DEG C/min of speed be warming up to 400 DEG C progress low-temperature activations, be incubated 45min, after be warming up to 800 DEG C with identical heating rate
High-temperature activation is carried out, 2.5h is incubated, corundum crucible is taken out, naturally cools to room temperature, produce activated material by activation after terminating；Take out
Activated material, is washed with 80 DEG C of distilled water, the rear HCl solution with 0.1M under 80 DEG C of high temperature pickling to neutral pH 6~7, then according to
So washed, dried under the conditions of last 105 DEG C with 80 DEG C of distilled water, activated carbon 3.03g is made in grinding.The activated carbon of preparation is entered
Row structural characterization, structural characterization result as shown in figures 1-4, can show that prepared activated carbon activation is complete from Fig. 1~4,
Micropore is flourishing, specific surface area 2818.22m2/ g, pore volume is 1.32cm3/ g, average pore size 2.62nm.By above-mentioned garlic skin matrix activated carbon
By activating substance：Conductive agent：Binding agent=80：10：10 ratio is mixed, and electrode slice is made.Adopted in 6M KOH solutions
The test of specific capacitance is carried out under different scanning rates with cyclic voltammetry.Its test result is as shown in Fig. 5~7, for example, in 6M
Current density is 0.5A/g, 1.0A/g, 2.0A/g, 3.0A/g in KOH electrolyte, and the specific capacitance under 5.0A/g is respectively reached
318.67F/g, 284.53F/g, 269.33F/g, 262.51F/g, 253.01F/g, 5000 times under 3.0A/g current density
Constant current charge-discharge capacitance conservation rate reaches 94%, is the ideal hyper electricity of a kind of high power of practicality, high-energy-density
Container material.
Embodiment 2
Take garlic skin to dry or dry after cleaning, crush, cross 80 mesh sieves, garlic skin powder is made；Garlic skin powder is positioned over tubular type
In resistance furnace, 600 DEG C are heated under inert atmosphere (flow is 2L/min), heating rate is 5 DEG C/min, are incubated 2h, cooling
To room temperature, garlic skin carbonized material is made；At room temperature, it is 3.5 according to the mass ratio of KOH solids and garlic skin carbonized material:1, take garlic skin charcoal
Material 6g, corresponding KOH solids be 24g, saturation KOH solution is thoroughly mixed with garlic skin carbonized material, after put it into drum
Wind drying box impregnates 2h, material after must impregnating with 80 DEG C of high temperature；Material after dipping is put into Muffle furnace to be activated, from room temperature with
5 DEG C/min of heating rate be warming up to 400 DEG C progress low-temperature activations, be incubated 45min, after be warming up to 850 with identical heating rate
DEG C carry out high-temperature activation, be incubated 2h, activation terminate after corundum crucible is taken out, naturally cool to room temperature, produce activated material；Take out
Activated material, is washed with 80 DEG C of distilled water, the rear HCl solution with 0.1M under 80 DEG C of high temperature pickling to neutral pH 6~7, then according to
So washed, dried under the conditions of last 105 DEG C with 80 DEG C of distilled water, activated carbon 3.91g is made in grinding.The activated carbon of preparation is entered
Row structural characterization, specific surface area 2542.77m2/ g, pore volume is 0.93cm3/ g, average pore size 2.17nm.By above-mentioned garlic skin base activity
Charcoal presses activating substance：Conductive agent：Binding agent=80：10：10 ratio is mixed, and electrode slice is made.In 6M KOH solutions
Constant current charge-discharge is used to measure under 0.5A/g current density capacitance for 253.70F/g.And the methylene of activated carbon
Blue adsorptive value is 39mL/0.1g.
Embodiment 3
Take garlic skin to dry or dry after cleaning, crush, cross 80 mesh sieves, garlic skin powder is made；Garlic skin powder is positioned over tubular type
In resistance furnace, 600 DEG C are heated under inert atmosphere (flow is 2L/min), heating rate is 5 DEG C/min, are incubated 5h, cooling
To room temperature, garlic skin carbonized material is made；At room temperature, it is 4 according to the mass ratio of KOH solids and garlic skin carbonized material:1, take garlic skin to carbonize
Expect 6g, corresponding KOH solids be 24g, saturation KOH solution is thoroughly mixed with garlic skin carbonized material, after put it into air blast
Drying box impregnates 2h, material after must impregnating with 80 DEG C of high temperature；Material after dipping is put into Muffle furnace to be activated, from room temperature to rise
Warm 5 DEG C/min of speed be warming up to 400 DEG C progress low-temperature activations, be incubated 45min, after be warming up to 800 DEG C with identical heating rate
High-temperature activation is carried out, 1h is incubated, corundum crucible is taken out, naturally cools to room temperature, produce activated material by activation after terminating；Take out and live
Material, is washed with 80 DEG C of distilled water, and pickling is to neutral pH 6~7 under 80 DEG C of high temperature for the rear HCl solution with 0.1M, then still
Washed, dried under the conditions of last 105 DEG C with 80 DEG C of distilled water, activated carbon 3.72g is made in grinding.Prepared activated carbon activation
Completely, micropore is flourishing.Specific surface area is 2077.21m2/ g, pore volume is 0.89cm3/ g, average pore size is 2.24nm.By above-mentioned garlic
Scytoblastema activated carbon presses activating substance：Conductive agent：Binding agent=80：10：10 ratio is mixed, and electrode slice is made.In 6M
Constant current charge-discharge is used to measure under 0.5A/g current density capacitance for 191.06F/g in KOH solution.And activity
The methylene blue adsorption value of charcoal is 35mL/0.1g.
Embodiment 4
Take garlic skin to dry or dry after cleaning, crush, cross 80 mesh sieves, garlic skin powder is made；Garlic skin powder is positioned over tubular type
In resistance furnace, 550 DEG C are heated under inert atmosphere (flow is 2L/min), heating rate is 5 DEG C/min, are incubated 5h, cooling
To room temperature, garlic skin carbonized material is made；At room temperature, it is 4.5 according to the mass ratio of KOH solids and garlic skin carbonized material:1, take garlic skin charcoal
Material 6g, corresponding KOH solids be 24g, saturation KOH solution is thoroughly mixed with garlic skin carbonized material, after put it into drum
Wind drying box impregnates 2h, material after must impregnating with 80 DEG C of high temperature；Material after dipping is put into Muffle furnace to be activated, from room temperature with
5 DEG C/min of heating rate be warming up to 400 DEG C progress low-temperature activations, be incubated 45min, after be warming up to 750 with identical heating rate
DEG C carry out high-temperature activation, be incubated 2h, activation terminate after corundum crucible is taken out, naturally cool to room temperature, produce activated material；Take out
Activated material, is washed with 80 DEG C of distilled water, the rear HCl solution with 0.1M under 80 DEG C of high temperature pickling to neutral pH 6~7, then according to
So washed, dried under the conditions of last 105 DEG C with 80 DEG C of distilled water, activated carbon 4.96g is made in grinding.Prepared activated carbon is lived
Change complete, micropore prosperity, specific surface area 1507.59m2/ g, aperture is 0.66cm3/ g, average pore size 2.30nm.By above-mentioned garlic skin
Matrix activated carbon presses activating substance：Conductive agent：Binding agent=80：10：10 ratio is mixed, and electrode slice is made.In 6M KOH
Constant current charge-discharge is used to measure under 0.5A/g current density capacitance for 159.30F/g in solution.And activated carbon
Methylene blue adsorption value be 22mL/0.1g.
Although above-mentioned the embodiment of the present invention is described with reference to accompanying drawing, not to invention protection domain
Limitation, one of ordinary skill in the art should be understood that on the basis of technical scheme those skilled in the art are not required to
Pay various modifications or deform still within the scope of the present invention that creative work can make.
Claims (10)
1. application of the garlic skin in the active carbon electrode material of ultracapacitor is prepared.
2. a kind of preparation method of garlic skin matrix activated carbon electrode material for ultracapacitor, it is characterized in that, by garlic skin lazy
Property atmosphere under be heated to 550~700 DEG C, insulation a period of time carries out charing and obtains garlic skin carbonized material, then garlic skin carbonized material is added
Enter to alkali hydroxide soln high temperature time of infusion and obtain dipping material, dipping material is then warming up to 400
~450 DEG C of progress low-temperature activations, low-temperature activation continues to be heated to 700~850 DEG C of progress high-temperature activations for a period of time afterwards, and high temperature is lived
Activated material is obtained after changing a period of time, activated material progress post processing is finally produced into activated carbon.
3. preparation method as claimed in claim 2, it is characterized in that, carry out charing process after garlic skin is pre-processed；
It is preferred that, it is to take garlic skin to dry or dry for the first time after cleaning the step of the pretreatment, crushes, cross 80 mesh sieves；
It is further preferred that the temperature dried is 20~30 DEG C, the temperature of the drying is 100~110 DEG C.
4. preparation method as claimed in claim 2, it is characterized in that, the heating rate for being heated to 550~700 DEG C is 5 DEG C/min,
Soaking time is 2~5h.
5. preparation method as claimed in claim 2, it is characterized in that, the alkali hydroxide soln is alkali metal hydroxide
The saturated solution of thing；
Or, alkali metal hydroxide is one or both of potassium hydroxide, sodium hydroxide；
Or, the mass ratio of alkali metal hydroxide and garlic skin carbonized material is 3.0~4.5：1；
Or, the temperature of the dipping is 80 DEG C, the time of the dipping is 2h.
6. preparation method as claimed in claim 2, it is characterized in that, it is warming up to 400~450 DEG C and is warming up to 700~850 DEG C
Heating rate is 5 DEG C/min；
Or, the time of the low-temperature activation is 45min；
Or, the time of the high-temperature activation is 1~2.5h.
7. preparation method as claimed in claim 2, it is characterized in that, the post processing includes washing for the first time, pickling, the successively
Secondary washing, second of drying, grinding；
It is preferred that, the temperature of the first time washing and second of washing is 80 DEG C；
It is preferred that, concretely comprising the following steps for the pickling is washed till pH 6~7 using acid solution at 80 DEG C；
It is preferred that, the concentration for the acid solution that the pickling is used is 0.1M；
It is preferred that, the acid solution is the one or more in hydrochloric acid, sulfuric acid, nitric acid.
8. activated carbon prepared by a kind of any described preparation method of claim 2~7.
9. a kind of garlic skin matrix activated carbon electrode material for ultracapacitor, it is characterized in that, using the work described in claim 8
Property charcoal is prepared.
10. a kind of application of the activated carbon described in claim 8 in ultracapacitor.
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| CN108365184A (en) * | 2018-01-02 | 2018-08-03 | 江苏大学 | A kind of lithium ion battery porous SiOC negative materials of rich carbon and preparation method thereof |
| CN108493007A (en) * | 2018-03-13 | 2018-09-04 | 河南工程学院 | The preparation method of electrode slice with high electrochemical performance |
| CN108516548A (en) * | 2018-03-06 | 2018-09-11 | 合肥工业大学 | A kind of preparation method of high mesoporous rate activated carbon and its activated carbon of acquisition |
| CN108557819A (en) * | 2018-05-30 | 2018-09-21 | 山东大学 | Garlic base waste prepares the methods and applications of porous carbon material |
| WO2018188422A1 (en) * | 2017-04-14 | 2018-10-18 | 山东大学 | Garlic skin-based activated carbon electrode material for use with supercapacitor and preparation method |
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| CN110817867A (en) * | 2019-12-12 | 2020-02-21 | 山东大学 | Preparation method and application of garlic skin based super activated carbon |
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| WO2018188422A1 (en) | 2018-10-18 |
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