CN106430187A - Method of using uncured carbon felt leftover material for preparing supercapacitor electrode activated carbon - Google Patents

Method of using uncured carbon felt leftover material for preparing supercapacitor electrode activated carbon Download PDF

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Publication number
CN106430187A
CN106430187A CN201610832863.4A CN201610832863A CN106430187A CN 106430187 A CN106430187 A CN 106430187A CN 201610832863 A CN201610832863 A CN 201610832863A CN 106430187 A CN106430187 A CN 106430187A
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China
Prior art keywords
activated carbon
uncured
carbon
carbon felt
leftover pieces
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CN201610832863.4A
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Inventor
周南
刘俊锋
戴开瑛
张治军
康志卫
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Hunan Southern Stroke Cloud New Material Ltd By Share Ltd
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Hunan Southern Stroke Cloud New Material Ltd By Share Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention relates to a method of using an uncured carbon felt leftover material for preparing supercapacitor electrode activated carbon. The method includes the following steps that the uncured carbon felt leftover material is cut into small pieces, the leftover material pieces are put into a strong base water solution to be soaked, dried, put into a high-temperature tubular muffle furnace under protection of the inert gas atmosphere and heated to 700-1200 DEG C, the temperature is kept for 1-8 h, the product is obtained through carbonization and activation, after natural cooling, washing, acid pickling and washing are carried out on the product until the product is neutral, and the activated carbon material which has good electrochemical performance and can be used as a supercapacitor electrode material is obtained through suction filtration, drying and grinding. The obtained activated carbon material is uniform in granularity and large in specific surface area, and a prepared supercapacitor has high specific capacity and cycling stability. The industrial waste carbon felt leftover material is used in the method, the carbon electrode material used for the supercapacitor is prepared through the simple and fast method, waste is turned into wealth, resources are fully used, environment pollution is reduced, economic benefits are large, and the method is beneficial for industrial production.

Description

The method preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces
Technical field
The present invention relates to a kind of method preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces.
Background technology
The increasingly depleted of global warming and Fossil fuel forces people to greatly develop sustainable and regenerative resource.At present, Solve the energy problem of shortage increasingly, be still one of huge challenge of facing mankind.Finding cleaning, efficient and regenerative resource While, energy stores also can not be ignored.It is considered as example solar energy and the wind energy of new forms of energy most with prospects, be all subject to The impact of the factors such as time, place, weather is it is impossible to steady operation.Therefore, particularly need energy-storage system that energy is deposited It is used after storage again.In recent years, ultracapacitor played the part of more and more important role as energy storage device, in particular with letter The developing rapidly of new technique in the fields such as breath technology, electronic product and vehicle used energy, people focus more on grinding of ultracapacitor Study carefully and exploitation.
Carbon/carbon compound material is due to having low-density, high intensity, high ratio modulus, high-termal conductivity, low-expansion coefficient, friction Performance is good, and thermal shock resistance is good, the multiple advantages such as dimensional stability is high are it is considered to be the most rising high temperature material One of material, is widely used to the fields such as Aero-Space, auto industry, military project, medical science.Preparation work in carbon/carbon compound material In skill, substantial amounts of corner tailing can be produced (i.e.:Carbon felt leftover pieces).These materials are with carbon as main constituents, such as straight Connect discarded, not only cause the great wasting of resources, more due to the refractory organicses of carbon, by precarious natural ring Pollution threat difficult to the appraisal is caused in border.Therefore, innoxious resource reutilization is carried out to the carbon leftover bits based on carbon felt With exploitation, it is then applied to energy storage field, there is great economic worth and Practical significance.
Content of the invention
The technical problem to be solved is to provide one kind and prepares ultracapacitor using uncured carbon felt leftover pieces The method of electrode activity carbon.Using the present invention, carbon felt leftover pieces resource not only can be made to be effectively used, slow down ecological environment Pressure, the activated carbon being simultaneously obtained has preferable chemical property, can serve as the electrode material of ultracapacitor, is conducive to Promote the development of new energy field.
The technical solution adopted for the present invention to solve the technical problems is:Prepare super electricity using uncured carbon felt leftover pieces The method of container electrode activated carbon, comprises the following steps:
Uncured carbon felt leftover pieces are cut into fritter, puts in strong alkali aqueous solution and soak, after being dried, be placed in inert gas atmosphere In the high-temperature tubular Muffle furnace of protection, it is warming up to 700-1200 DEG C, be incubated 1-8h, carbonization-activation obtains product, after natural cooling, Using washing, pickling, wash again until neutral, sucking filtration, be dried, grind, obtain having good chemical property, can be used as super The active carbon material of capacitor electrode material.
Further, described fritter is 1-3cm3Cubic block.
Further, described highly basic is KOH, NaOH, K2CO3、Na2CO3、NaHCO3One or more of.
Further, described strong alkali aqueous solution concentration is 6-8mol/L.
Further, described fritter and strong alkali aqueous solution press solid-liquid w/v is 1g:The ratio mixing of 30-60ml, The time soaked is 12-24h.
Further, soak after 100-120 DEG C(Preferably 110 DEG C)Convection oven in be dried to constant weight.
Further, heating rate is 3-10 DEG C/min, and heating rate has large effect to the property of material with carbon element, and heat up speed If rate is too fast, surface carbonation is too fast, and internal carbonization does not catch up with, and can cause bulk property difference, affects end-use properties.
Further, described pickling is washed with the HCl solution of 1M.
Further, sucking filtration is after 75-85 DEG C(Preferably 80 DEG C)Convection oven in 11-13h is dried.
Further, described noble gases are nitrogen or argon etc..
Further, described inert gas atmosphere is the noble gases of more than purity 99wt%, and the flow velocity that is passed through of gas is 3- 8ml/min.
Weigh the above-mentioned active carbon material of 0.8g, with acetylene black by weight 8:It is ground after 1 mixing, be subsequently adding Mass concentration is 10% polytetrafluoroethyl-ne aqueous solution, wherein, activated carbon:Acetylene black:Politef=8:1:1(Mass ratio), Add ethanol as solvent, continue after mixing to grind, roll piece, prepare carbon electrode material.The carbon electrode piece being obtained is pressed onto stainless On steel collector, then after vacuum drying 12h at 110 DEG C, with the KOH aqueous solution of 6mol/L as electrolyte, it is assembled into super Capacitor, tests chemical property.
Uncured carbon felt refers to be not wetted by the carbon felt through cured for the resin, and uncured carbon felt is with carbon fiber as group Become composition, the surface of carbon fiber only has very small amount of polymer covering layer, and it is solidified resin that solidification carbon felt has very big composition.
Using active carbon material epigranular obtained by the present invention, specific surface area is about 726m2/ g, prepared electrode assembling After becoming ultracapacitor, specific discharge capacity is 191.23F/g, has good cyclical stability, can be used for energy storage field. The method utilizes trade waste carbon felt leftover pieces, prepares ultracapacitor carbon electrode material by simple and quick method, Turn waste into wealth, make full use of resource, reduce environmental pollution, good in economic efficiency, it is beneficial to industrialized production.
Brief description
Fig. 1 is the scanning electron microscope (SEM) photograph of the ultracapacitor activated carbon of the embodiment of the present invention 3 preparation;
Fig. 2 is the circulation volt after activated carbon prepared by the embodiment of the present invention 3 is assembled into ultracapacitor under 100mV/s sweeps speed Antu;
Fig. 3 is the discharge and recharge that is assembled into after ultracapacitor under 1A/g electric current density of activated carbon of the embodiment of the present invention 3 preparation Curve chart;
Fig. 4 is assembled into after ultracapacitor in 1A/g electric current density discharge and recharge condition for the activated carbon of the embodiment of the present invention 3 preparation Under cyclical stability.
Specific embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Embodiment 1
Uncured carbon felt leftover pieces are cut into the cubed pieces of 1cm × 1cm × 1cm, take wherein 4 pieces(Quality is 4g), by solid Liquid w/v is 1g:30ml puts in the KOH aqueous solution that concentration is 6mol/L and soaks 12h, is subsequently placed in 110 DEG C of air blast It is dried in baking oven to constant weight, be then passed through the high-temperature tubular Muffle furnace under the nitrogen atmosphere protection that flow velocity is 3ml/min in gas In, with the ramp of 10 DEG C/min to 700 DEG C, insulation 1h after, carbonization-activation obtains product, after natural cooling, using go from After sub- water cleans 3 times, then the HCl solution for 1M is carried out using concentration, repeatedly after 5 times, then deionized water cleaning until Neutrality, carries out sucking filtration to the product after cleaning, 12h is dried, after grinding, is had in the convection oven being placed into 80 DEG C Good chemical property, can be used as the active carbon material of electrode material for super capacitor.
Embodiment 2
Uncured carbon felt leftover pieces are cut into the cubed pieces of 1cm × 1cm × 1cm, take wherein 4 pieces(Quality is 4g), by solid Liquid w/v is 1g:30ml puts in the KOH aqueous solution that concentration is 6mol/L and soaks 18h, is subsequently placed in 110 DEG C of air blast It is dried in baking oven to constant weight, be then passed through the high-temperature tubular Muffle furnace under the nitrogen atmosphere protection that flow velocity is 3ml/min in gas In, with the ramp of 6 DEG C/min to 800 DEG C, after insulation 1h, carbonization-activation obtains product, after natural cooling, using deionization After water cleans 3 times, then the HCl solution for 1M is carried out using concentration, repeatedly after 5 times, then deionized water cleaning until in Property, sucking filtration is carried out to the product after cleaning, 12h in the convection oven being placed into 80 DEG C, is dried, after grinding, obtain having good Good chemical property, can be used as the active carbon material of electrode material for super capacitor.
Embodiment 3
Uncured carbon felt leftover pieces are cut into the cubed pieces of 1cm × 1cm × 1cm, take wherein 4 pieces(Quality is 4g), by solid Liquid w/v is 1g:30ml puts in the KOH aqueous solution that concentration is 6mol/L and soaks 24h, is subsequently placed in 110 DEG C of air blast It is dried in baking oven to constant weight, be then passed through the high-temperature tubular Muffle furnace under the nitrogen atmosphere protection that flow velocity is 3ml/min in gas In, with the ramp of 6 DEG C/min to 900 DEG C, after insulation 3h, carbonization-activation obtains product, after natural cooling, using deionization After water cleans 3 times, then the HCl solution for 1M is carried out using concentration, repeatedly after 5 times, then deionized water cleaning until in Property, sucking filtration is carried out to the product after cleaning, 12h in the convection oven being placed into 80 DEG C, is dried, after grinding, good to having Chemical property, can be used as the active carbon material of electrode material for super capacitor.
Comparative example
Take undressed uncured carbon felt waste material directly to grind, adopt and prepare electrode slice in a like fashion, load electric capacity In device device test, its chemical property can not show a candle to treated by the present method after active carbon product.
Adopt the inventive method to prepare gained activated carbon with uncured carbon felt corner dead meal, load after being prepared into electrode slice Tested in supercapacitor device, wherein the scanning electron microscope of the electrode of super capacitor activated carbon obtained in embodiment 3 Figure as shown in figure 1, every chemical property such as Fig. 2, shown in 3,4, the experimental results such as table 1 of embodiment 1-3 and comparative example Shown.From the point of view of experimental result, the active carbon material that embodiment 3 is obtained has uniform particle size, 726m2The ratio table of/g Area, prepared ultracapacitor has the specific discharge capacity of 191.23F/g, has good cyclical stability.
Table 1
Project Embodiment 1 Embodiment 2 Embodiment 3 Comparative example
Specific surface area(m2/g) 688 693 726 102
Initial discharge specific capacity(F/g, when electric current density is for 1A/g) 182.37 180.43 191.23 87.66
In sum, adopt the side of pyroreaction after the dead meal with aqueous slkali soaking uncured carbon felt corner provided by the present invention Method:On the one hand, with carbon felt corner dead meal for process object, the recycling of achievable resource, effectively reduces environmental pollution, fall Low production cost;On the other hand, preparation process is simple, simple flow, low cost, the activation carbon product obtaining has good electricity Chemical property, can be used for energy storage field;Raw material sources are extensive, simple production process, suitable industrial application.

Claims (10)

1. prepare the method for electrode of super capacitor activated carbon it is characterised in that including following using uncured carbon felt leftover pieces Step:
Uncured carbon felt leftover pieces are cut into fritter, puts in strong alkali aqueous solution and soak, after being dried, be placed in inert gas atmosphere In the high-temperature tubular Muffle furnace of protection, it is warming up to 700-1200 DEG C, be incubated 1-8h, carbonization-activation obtains product, after natural cooling, Using washing, pickling, wash again until neutral, sucking filtration, be dried, grind, obtain having good chemical property, can be used as super The active carbon material of capacitor electrode material.
2. the method preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces according to claim 1, It is characterized in that, described fritter is 1-3cm3Cubic block.
3. the side preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces according to claim 1 and 2 Method is it is characterised in that described highly basic is KOH, NaOH, K2CO3、Na2CO3、NaHCO3One or more of.
4. the method preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces according to claim 3, It is characterized in that, described strong alkali aqueous solution concentration is 6-8mol/L.
5. the method preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces according to claim 4, It is characterized in that, described fritter presses solid-liquid w/v 1g with strong alkali aqueous solution:30-60ml mixes, and the time of immersion is 12-24h.
6. the side preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces according to claim 1 and 2 Method is dried to constant weight in 100-120 DEG C of convection oven it is characterised in that soaking.
7. the side preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces according to claim 1 and 2 Method is it is characterised in that heating rate is 3-10 DEG C/min.
8. the side preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces according to claim 1 and 2 Method is it is characterised in that sucking filtration is dried 11-13h in 75-85 DEG C of convection oven.
9. the side preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces according to claim 1 and 2 Method is it is characterised in that described noble gases are nitrogen or argon.
10. the method preparing electrode of super capacitor activated carbon using uncured carbon felt leftover pieces according to claim 9, It is characterized in that, described inert gas atmosphere is the noble gases of more than purity 99wt%, and the flow velocity that is passed through of gas is 3-8ml/ min.
CN201610832863.4A 2016-09-20 2016-09-20 Method of using uncured carbon felt leftover material for preparing supercapacitor electrode activated carbon Pending CN106430187A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106816650A (en) * 2017-04-01 2017-06-09 帅福得(珠海保税区)电池有限公司 A kind of sustainable discharge battery of high current and its assembly technology
CN108074751A (en) * 2017-12-08 2018-05-25 中北大学 A kind of flexible 3 D porous carbon materials and its preparation method and application
CN108962625A (en) * 2018-06-22 2018-12-07 东莞理工学院 A kind of supercapacitor carbon material and preparation method thereof prepared using humin as raw material
CN110277557A (en) * 2018-03-17 2019-09-24 中国海洋大学 The preparation method and storage sodium performance of the biological carbon material of multi-element doping, high-specific surface area, threadiness
CN113307267A (en) * 2021-06-24 2021-08-27 中国矿业大学 Preparation method of coal-based porous carbon

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CN105244178A (en) * 2015-10-28 2016-01-13 王彦博 Super capacitor and preparation method thereof
CN105529471A (en) * 2016-01-21 2016-04-27 湖南省银峰新能源有限公司 Treatment method for all-vanadium redox flow battery electrode

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CN1203887A (en) * 1998-06-12 1999-01-06 吉林大学 Preparation of superhigh specific surface area active carbon
CN1524611A (en) * 2003-09-18 2004-09-01 武汉理工大学 Composite material comprising photocatalyst and phenolic resin group active carbon and preparation method thereof
CN101777652A (en) * 2010-01-13 2010-07-14 东南大学 Production method of active carbon of direct carbon conversion fuel cell
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106816650A (en) * 2017-04-01 2017-06-09 帅福得(珠海保税区)电池有限公司 A kind of sustainable discharge battery of high current and its assembly technology
CN108074751A (en) * 2017-12-08 2018-05-25 中北大学 A kind of flexible 3 D porous carbon materials and its preparation method and application
CN110277557A (en) * 2018-03-17 2019-09-24 中国海洋大学 The preparation method and storage sodium performance of the biological carbon material of multi-element doping, high-specific surface area, threadiness
CN108962625A (en) * 2018-06-22 2018-12-07 东莞理工学院 A kind of supercapacitor carbon material and preparation method thereof prepared using humin as raw material
CN113307267A (en) * 2021-06-24 2021-08-27 中国矿业大学 Preparation method of coal-based porous carbon

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Application publication date: 20170222