CN103346025A - Method for preparing super capacitor electrode materials with laver - Google Patents
Method for preparing super capacitor electrode materials with laver Download PDFInfo
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- CN103346025A CN103346025A CN2013102587612A CN201310258761A CN103346025A CN 103346025 A CN103346025 A CN 103346025A CN 2013102587612 A CN2013102587612 A CN 2013102587612A CN 201310258761 A CN201310258761 A CN 201310258761A CN 103346025 A CN103346025 A CN 103346025A
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- laver
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a method for preparing super capacitor electrode materials with laver, and belongs to the field of high polymer materials. According to the method, the laver is washed sequentially with diluted hydrochloric acid of 1-3M and water and is pre-carbonized for 1-3h at the temperature of 300-450 DEG C after being dried. Then the pre-carbonized laver is immersed for 8-24h in alkali liquor, filtered, dried, and then carbonized for 2-6h at the temperature of 700-900 DEG C under the protection of N2. Ultimately, the carbonized laver is immersed in acid liquor for 6-18h, is washed in water to be under a neutral state, and dried, and then the super capacitor electrode materials are obtained. According to the method, the laver is taken as raw materials, renewability of the laver is strong, sources of the laver are wide, cost is low, and cost of electrode materials is effectively reduced; the super capacitor electrode materials are prepared through simple alkaline leaching, acid leaching and carbonization process, and the preparing process is simple and environmentally friendly; the prepared laver carbon base materials have the advantages of large specific capacitance, conductivity, excellent electrochemical performance and the like, and are ideal super capacitor electrode materials.
Description
Technical field
The present invention relates to a kind of preparation of electrode material for super capacitor, belong to polymeric material field; Relate in particular to a kind of method for preparing electrode material for super capacitor with laver.
Background technology
The energy is the important foundation of the good development of human survival and society, along with progress of science and technology, the development of electric automobile, Aero-Space, mobile communication, science and techniques of defence, generation of electricity by new energy (wind energy, solar energy etc.) and electromagnet weapon, people are more and more urgent with the demand of power supply to the high-performance memory device.These energy storage devices are except energy density being had certain requirement, and are also more and more higher to the requirement of power density.Super capacitor is as a kind of novel energy-storing element under this background, because its power density height, have extended cycle life, advantages such as charging rate is fast, serviceability temperature wide ranges, safety and environmental protection, receive increasing concern, become the important component part of new forms of energy application.
Ultracapacitor, from the material angle, vital namely be select to be fit to supercapacitor applications, in electrolyte, have an electrode material than height ratio capacity.At present be respectively carbon-based material, metal oxide materials and conducting polymer materials as electrode material for super capacitor.And in these three kinds of materials, carbon-based material is with its cheap price, and excellent material property and simple preparation technology more and more are subjected to various countries researcher's favor.And biomass are more promising carbon sources, therefore how fixed biologically matter carbon, and to replace the fossil resource product with it as a series of chemical products of feedstock production be that whole world scientist presses for the research task of finishing.
Laver is the general designation of marine alternate algae bio, generally lives in the seabed apart from tens of meters of intertidal zones, and it is green that appearance is usually, takes on a red color once in a while.Laver contains protein and iodine, multivitamin and the inorganic salts up to 29% ~ 35%.Because it has very high nutritive value, supply directly to eat mainly as material for cooking or with other food, then seldom use industrial.Because laver is the porousness layer structure, blade is the membranous body by the single or tool bifurcated of 1 confluent monolayer cells (a few species is by 2 layers or 3 layers) formation, structure after its charing is conducive to ion portion's transfer within it or the transportation in the electrolyte, so be expected to the electrode material as ultracapacitor.
Summary of the invention
The objective of the invention is at problems of the prior art, a kind of method for preparing electrode material for super capacitor with laver is provided.
The present invention prepares the method for electrode material for super capacitor with laver, is that laver is used 1 ~ 3M watery hydrochloric acid, water washing successively, and after the drying, in 300 ~ 450 ℃ of pre-carbonization 1 ~ 3 h down, the laver with pre-carbonization soaks 8 ~ 24 h in alkali lye again, filters, oven dry, then at N
2Protection is down in 700 ~ 900 ℃ of carbonization 2 ~ 6 h; Soak 6 ~ 18 h at last in acid solution, be washed with water to neutrality, oven dry namely gets electrode material for super capacitor.
The mass volume ratio of described laver and alkali lye is 1:1 ~ 1:3;
Described alkali lye is NaOH or the potassium hydroxide solution of concentration 1 ~ 3M;
Described acid solution is the hydrochloric acid solution of concentration 1 ~ 3M.
Described oven dry is to carry out vacuumize under 50 ~ 70 ℃.
Fig. 1 is the microscopic appearance figure (SEM) of the present invention with the ESEM of the electrode material for super capacitor of laver preparation.As seen from Figure 1, prepared laver carbon based material is layer structure, and its surface is the accordion lines of classification.The microstructure of laver is similar before this and the carbonization, illustrates that carbonisation does not destroy its structure.
Below by to the present invention with the electrode material for super capacitor of laver preparation at 1 mol/L Na
2SO
4Cyclic voltammetry curve in the electrolyte (CV) is its charge transfer ability in electrolyte of explanation.
Fig. 2 is that carbonization obtains under the different temperatures (700 ℃, 800 ℃, 900 ℃) electrode material for super capacitor is at 1 mol/L Na
2SO
4Cyclic voltammetric in the electrolyte (CV) curve.As seen from Figure 2, the electrochemistry area of the laver carbon based material when carburizing temperature is 900 ℃ is 700 ℃ and 800 ℃ greater than carburizing temperature obviously, it is the electrochemistry area maximum of the laver carbon based material of carburizing temperature when being 900 ℃, the shape of the cyclic voltammetry curve of material more and more levels off to rectangle, shows that the laver carbon based material under high temperature cabonization has better charge transfer process.When carburizing temperature was low, the laver carbonization was complete inadequately, made the nonconducting composition that wherein is not carbonized limit the migration of electric charge, and the charge transfer process is obstructed.Therefore, the aggregation extent of material surface electric charge obviously reduces in the unit interval.Because ratio electric capacity and the CV area of electrode material are relations in direct ratio, therefore, the laver carbon based material when carburizing temperature is 900 ℃ than electric capacity maximum, be 180 F g
-1
The chemical property appraisement system is finished in the three-electrode system of routine, adopts the CHI 660D type electrochemical workstation of Shanghai occasion China Co., Ltd to test; The stable circulation property testing adopts the CT2001A type tester of the blue electric Electronics Co., Ltd. in Wuhan.Work electrode is glass-carbon electrode, is platinum electrode to electrode, and reference electrode is saturated calomel electrode, and electrolyte is 1 M Na
2SO
4The laver carbon based material is as the electrode material of ultracapacitor, through only having reduced by 3 % than electric capacity after 10000 charge and discharge cycles.Illustrated that its charge and discharge circulation life is long, cycle efficieny is advantages of higher relatively.
The present invention has the following advantages with respect to prior art:
1, the present invention is raw material with the laver, and its recyclability is strong, be easy to cultivate in nautical mile large tracts of land, thereby its source is abundant, and cost is low, effectively reduces the cost of electrode material;
2, product of the present invention by simple alkali soak, acidleach, carbonization technique get, its preparation technology is simple, environmental friendliness;
3, the laver carbon based material of the present invention preparation has bigger ratio electric capacity, has characteristics such as electric conductivity and chemical property thereof be more excellent, is a kind of more satisfactory electrode material for super capacitor.
Description of drawings
Fig. 1 is the ESEM of the electrode material for super capacitor of the present invention's preparation;
The electrode material for super capacitor that Fig. 2 obtains for carbonization under the different temperatures is at 1 mol/L Na
2SO
4Cyclic voltammetry curve in the electrolyte.
Embodiment
Be described further below by preparation and the chemical property thereof of specific embodiment to electrode material for super capacitor of the present invention.
Embodiment 1
Take by weighing 1.0 g lavers, spend the washing repeatedly of 1M watery hydrochloric acid, deionized water respectively after, 50 ℃ of dryings in vacuum drying chamber; Pre-carbonization 3 h under 400 ℃, the laver with carbonization is soaked in the 1M KOH solution of 100mL then, soaks 24 h under room temperature; Filtration is placed on oven dry in about 50 ℃ in the vacuum drying chamber; At last at N
2Protection after continuing carbonization 6 h under 700 ℃, places 1M HCl to soak 18 h down; Spend deionised water to neutral, oven dry namely gets electrode material for super capacitor.After testing, electrode material for super capacitor is at 1 mol/L Na
2SO
4Ratio electric capacity in the electrolyte is 138 F g
-1
Embodiment 2
Take by weighing 1.0 g lavers, go the washing repeatedly of watery hydrochloric acid, deionized water with 2M respectively after, 60 ℃ of dryings in vacuum drying chamber; Pre-carbonization 1 h under 450 ℃, the laver with carbonization is soaked in the 2M KOH solution of 100mL then, soaks 24 h under room temperature; Filtration is placed on oven dry about 60 ℃ in the vacuum drying chamber; At last at N
2Protection is soaked 10 h down in 800 ℃ of following carbonization 4 h in 2 M HCl, spend deionised water to neutral, and oven dry must namely get electrode material for super capacitor.After testing, electrode material for super capacitor is at 1 mol/L Na
2SO
4Ratio electric capacity in the electrolyte is 150 F g
-1
Embodiment 3
Take by weighing 1.0 g lavers, spend the washing repeatedly of 3M watery hydrochloric acid, deionized water respectively after, 70 ℃ of dryings in vacuum drying chamber; Pre-carbonization 1 h under 300 ℃; Laver with carbonization is soaked in the 3M KOH solution of 100mL then, soaks 24 h under room temperature; Filtration is placed on oven dry about 70 ℃ in the vacuum drying chamber; At N
2Protection is down in 900 ℃ of following carbonization 3 h; Soak 6 h in 3 M HCl, spend deionised water at last to neutral, oven dry namely gets electrode material for super capacitor.After testing, electrode material for super capacitor is at 1 mol/L Na
2SO
4Ratio electric capacity in the electrolyte is 180 F g
-1
Claims (5)
1. the method for preparing electrode material for super capacitor with laver is that laver is used 1 ~ 3M watery hydrochloric acid, water washing successively, after the drying, and pre-carbonization 1～3 h under 300～450 ℃, the laver with pre-carbonization soaks 8～24 h in alkali lye again, filters, dries, then at N
2Protection is down in 700～900 ℃ of carbonization 2～6h; Soak 6～18 h at last in acid solution, be washed with water to neutrality, oven dry namely gets electrode material for super capacitor.
2. prepare the method for electrode material for super capacitor according to claim 1 with laver, it is characterized in that: the mass volume ratio of described laver and alkali lye is 1:1～1:3.
3. prepare the method for electrode material for super capacitor as claimed in claim 1 or 2 with laver, it is characterized in that: described alkali lye is NaOH or the potassium hydroxide solution of concentration 1～3M.
4. prepare the method for electrode material for super capacitor as claimed in claim 1 or 2 with laver, it is characterized in that: described acid solution is the hydrochloric acid solution of concentration 1～3M.
5. prepare the method for electrode material for super capacitor as claimed in claim 1 or 2 with laver, it is characterized in that: described oven dry is to descend vacuumize under 50～70 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909363A (en) * | 2015-05-18 | 2015-09-16 | 陕西科技大学 | Preparation method of network-like nanostructured carbon material |
| CN106082193A (en) * | 2016-06-14 | 2016-11-09 | 陕西科技大学 | A kind of method preparing multilevel hierarchy material with carbon element for carbon source with algae |
| CN106920966A (en) * | 2017-04-12 | 2017-07-04 | 同济大学 | A kind of carbon-based lithium ion cell negative electrode material and its preparation using sludge as precursor |
| CN106946250A (en) * | 2017-03-31 | 2017-07-14 | 北京化工大学 | It is a kind of that there are seaweed base Carbon Materials of three-dimensional graded porous structure and its preparation method and application |
| CN113122184A (en) * | 2021-05-11 | 2021-07-16 | 盐城工学院 | Preparation method of biomass porous carbon wave-absorbing material |
| KR102585809B1 (en) * | 2023-04-13 | 2023-10-06 | (주)코리아마그네슘 | Preparing method of carbon-based material using marine algae and seaweed |
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| CN1824604A (en) * | 2005-09-19 | 2006-08-30 | 古可隆 | Method of making special active carbon for capacitor using hard fruit shell |
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| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN101905876A (en) * | 2009-06-02 | 2010-12-08 | 中国科学院化学研究所 | Porous carbon, and preparation method and applications thereof |
| CN102942176A (en) * | 2012-12-04 | 2013-02-27 | 西北师范大学 | Preparation method of cotton fiber coal-base material, and application thereof as electrode material of supercapacitor |
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2013
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Patent Citations (5)
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| CN1824604A (en) * | 2005-09-19 | 2006-08-30 | 古可隆 | Method of making special active carbon for capacitor using hard fruit shell |
| WO2007070645A2 (en) * | 2005-12-14 | 2007-06-21 | Massachusetts Institute Of Technology | Bio-sensitized solar cells (bssc) |
| CN101905876A (en) * | 2009-06-02 | 2010-12-08 | 中国科学院化学研究所 | Porous carbon, and preparation method and applications thereof |
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| CN102942176A (en) * | 2012-12-04 | 2013-02-27 | 西北师范大学 | Preparation method of cotton fiber coal-base material, and application thereof as electrode material of supercapacitor |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909363A (en) * | 2015-05-18 | 2015-09-16 | 陕西科技大学 | Preparation method of network-like nanostructured carbon material |
| CN106082193A (en) * | 2016-06-14 | 2016-11-09 | 陕西科技大学 | A kind of method preparing multilevel hierarchy material with carbon element for carbon source with algae |
| CN106082193B (en) * | 2016-06-14 | 2018-03-16 | 陕西科技大学 | A kind of method that multilevel hierarchy carbon material is prepared using algae as carbon source |
| CN106946250A (en) * | 2017-03-31 | 2017-07-14 | 北京化工大学 | It is a kind of that there are seaweed base Carbon Materials of three-dimensional graded porous structure and its preparation method and application |
| CN106920966A (en) * | 2017-04-12 | 2017-07-04 | 同济大学 | A kind of carbon-based lithium ion cell negative electrode material and its preparation using sludge as precursor |
| CN106920966B (en) * | 2017-04-12 | 2019-10-01 | 同济大学 | A kind of carbon-based lithium ion cell negative electrode material and its preparation using sludge as precursor |
| CN113122184A (en) * | 2021-05-11 | 2021-07-16 | 盐城工学院 | Preparation method of biomass porous carbon wave-absorbing material |
| KR102585809B1 (en) * | 2023-04-13 | 2023-10-06 | (주)코리아마그네슘 | Preparing method of carbon-based material using marine algae and seaweed |
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Application publication date: 20131009 |