CN103426650A - Asymmetric electrochemical supercapacitor on basis of rice-husk-based activated carbon materials - Google Patents
Asymmetric electrochemical supercapacitor on basis of rice-husk-based activated carbon materials Download PDFInfo
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Abstract
The invention relates to application of rice-husk-based activated carbon materials to an asymmetric electrochemical supercapacitor, belongs to the technical field of chemical power sources, and aims to provide an asymmetric electrochemical supercapacitor on the basis of rice-husk-based activated carbon. The asymmetric electrochemical supercapacitor comprises a positive pole, a negative pole, a diaphragm, electrolyte, a positive lead, a negative lead and a shell. The positive pole or the negative pole of the asymmetric electrochemical supercapacitor contains the rice-husk-based activated carbon which is used as an activated substance, the pole containing the rice-husk-based activated carbon is used for implementing an electric double-layer energy storage principle, the other pole is a pseudo-capacitive pole or battery pole, and the electrolyte is aqueous electrolyte or organic electrolyte. The asymmetric electrochemical supercapacitor has the advantages that the electric double-layer energy storage pole of the asymmetric electrochemical supercapacitor is made of the rice-husk-based activated carbon which has wide raw material sources and is advantageous in terms of price, accordingly, the cost of the electrochemical supercapacitor can be lowered, and the application range of the rice-husk-based activated carbon which is made of agricultural waste is broadened.
Description
Technical field
Patent of the present invention relates to the application of a kind of rice husk matrix activated carbon material in the asymmetrical type electric chemical super capacitor, belongs to technical field of chemical power.
Background technology
Electric chemical super capacitor is a kind of energy-storage travelling wave tube between battery and traditional capacitor, with secondary cell, compare, electric chemical super capacitor has life-span length, power density high, be specially adapted to need the occasion of heavy-current discharge, startup as electric automobile, just get more and more people's extensive concerning.Yet ultracapacitor also is faced with many problems in commercial applications, its energy density and battery are compared low as lithium ion battery, Ni-MH battery etc.In order to improve the energy density of electric chemical super capacitor, an effective approach is to adopt the asymmetrical type structure, and a utmost point adopts the electrode of electric double layer energy storage principle, and another utmost point adopts fake capacitance or battery electrode.Adopt the asymmetrical type structure can improve the operating voltage of electrochemical capacitor on the one hand, can, in conjunction with the high power capacity of fake capacitance class or battery class electrode, improve the energy density of electric chemical super capacitor on the other hand.So the asymmetrical type electric chemical super capacitor can meet the whole requirement of load to energy density and the power density of power-supply system in practical application better.
In the asymmetrical type electric chemical super capacitor, the electrode of electric double layer energy storage principle is generally carbon resistance rod, as active carbon, carbon fiber, carbon nano-tube etc.Compare other class Carbon Materials such as carbon fiber, carbon nano-tube, absorbent charcoal material is because the characteristics such as its cost is low, high-specific surface area are most widely used general.Open source literature (J.Electrochem.Soc., 2004,151 (4): A614-A622) reported a kind of asymmetrical type electric chemical super capacitor, take manganese dioxide as anodal, active carbon prepared as raw material by the coconut husk of take is negative pole; Patent CN101286418A discloses a kind of manganese bioxide electrochemical super capacitor, belongs to a kind of asymmetrical type electric chemical super capacitor, and negative pole adopts the bigger serface absorbent charcoal material.
The raw material for preparing active carbon has coal, timber, coconut husk, shell and macromolecular material etc., the rice husk matrix activated carbon is that a class be take the agricultural wastes rice husk as raw material, the absorbent charcoal material prepared through carbonization, activation, the method for utilizing rice husk to prepare absorbent charcoal material is reported more.Patent 98114553.1 has been announced and a kind ofly take rice husk and prepare the method for active carbon with high specific surface area as raw material, and its specific area can surpass 3000m
2/ g.Patent 200910310025.0 has been announced and a kind ofly take rice husk, stalk and prepare the method for active carbon as raw material, and the activated carbon-iodine adsorptive value that it prepares is greater than 1000mg/g, and the methylene blue adsorption number rate is greater than 135mg/g.Patent 201010586233.6 has also been announced and a kind ofly take rice husk and prepare the method for high-adsorption active carbon as raw material.Yet these active carbon prepared by rice husk application in electric chemical super capacitor, particularly be applied to the asymmetrical type electric chemical super capacitor and do not come into one's own.This is usually to contain more SiO due to active carbon prepared by rice husk
2, conductivity is descended, thereby cause the equivalent resistance of electric chemical super capacitor to increase, that is the active carbon that is suitable for sorbing material not necessarily just can be used as Electrode Materials in Electrochemical Supercapacitors.For example, open source literature " Performance of electrical double layer capacitors with porous carbons derived from rice husk " (Materials Chemistry and Physics80, 2003, 704-709.) take rice husk as raw material, the pore structure of the active carbon prepared under different preparation conditions, and the rice husk matrix activated carbon prepared of take is electrode, the structure that forms the symmetry type capacitance device, characterized its electric double layer capacitance performance in 3M KCl electrolyte, result shows that its operating voltage range is narrow, be only 0-0.6V, the energy density of narrower voltage range meeting decrease electric chemical super capacitor, open source literature " Nanoporous carbon derived from rice husk for electrochemical capacitor application " (Advanced Materials Research, 239-242, pp2101-2106.) reported a kind of method that is prepared porous charcoal by rice husk, be assembled into the symmetry type capacitance device by this porous charcoal, test result shows that its capacitive property is general.
Active carbon prepared as raw material by the rice husk of take, its raw material sources are more extensive, the preparation method is simple, our research is found, the rice husk matrix activated carbon all has good capacitive property and stability in water system and organic system, as electrode material, can be applicable to dissimilar asymmetrical type electric chemical super capacitor.
Summary of the invention
The object of the present invention is to provide a kind of asymmetrical type electric chemical super capacitor based on the rice husk matrix activated carbon, formed by positive pole, negative pole, barrier film, electrolyte, positive wire, negative wire and shell.The negative or positive electrode of described asymmetrical type electric chemical super capacitor contains the rice husk matrix activated carbon as active material, a utmost point of electric double layer energy storage principle very that contains the rice husk matrix activated carbon, another utmost point adopts fake capacitance electrode or battery class electrode, and electrolyte is aqueous electrolyte or organic electrolyte.
The described asymmetrical type electric chemical super capacitor fake capacitance electrode based on the rice husk matrix activated carbon is MnO
2, Mn
3O
4, Ni (OH)
2, the transition metal oxide such as NiO, battery electrode is PbO
2And lithium ion cell electrode.The rice husk matrix activated carbon at alkaline electrolyte (as KOH), acidic electrolysis bath (as H
2SO
4), neutral electrolyte is (as Na
2SO
4, K
2SO
4, Li
2SO
4), organic electrolyte (as tetraethylammonium tetrafluoroborate, TEABF
4) etc. all there is higher ratio electric capacity in the different electrolytes system, so the rice husk matrix activated carbon can be applied in different composing system asymmetrical type electric chemical super capacitors.
A kind of preparation method based on rice husk matrix activated carbon material: at least comprise the following steps:
(1) by rice husk cleaning, dry, grinding;
(2) by the rice husk charing under non-oxide condition after above-mentioned steps (1) grinding, with acid solution, process, then washing, drying, obtain carbide;
(3) carbide above-mentioned steps (2) obtained mixes in proportion with highly basic, adds certain water gaging to mix, and dries, and controls programming rate, and activation, obtain activation products;
(4) activation products that above-mentioned steps (3) obtained, with soaking in hot water, are filtered, and washing, to neutral, is ground to the 150-300 order and obtains the high specific capacitance absorbent charcoal material after drying;
In described step (2), non-oxide condition is that at least one gas by passing into to reaction system in carbon dioxide, nitrogen, argon gas obtains;
Carbonization temperature in described step (2) is 350-550 ℃, and carbonization time is 0.5-2h, and described acid solution can be at least one in hydrochloric acid, sulfuric acid;
In described step (3), highly basic is at least one in potassium hydroxide or NaOH, and carbide and highly basic mass ratio are 1:(1-5), programming rate is 2-15 ℃/min, activation temperature is 600-900 ℃, activation 0.5-4h;
In described step (4), the hot water temperature is controlled at 50-100 ℃, and baking temperature is 100-120 ℃, and be 12-24h drying time;
The prepared rice husk matrix activated carbon material specific area out of above method is 2000-3700m
2/ g, pore-size distribution is narrow, with micropore and mesopore, is distributed as the master.
The invention has the beneficial effects as follows by adopt raw material sources extensively, there is the electrode material of the rice husk matrix activated carbon of price advantage as the electric double layer energy storage electrode of asymmetrical type electric chemical super capacitor, can not only reduce the cost of electric chemical super capacitor, and widen the range of application of the rice husk matrix activated carbon prepared by agricultural wastes.
Embodiment
Below in conjunction with example, the invention will be further described.
Embodiment 1
The preparation of rice husk matrix activated carbon:
(1) by rice husk cleaning, dry, grinding;
(2) rice husk after step (1) is processed is under nitrogen protection, 400 ℃ of lower charing 1.5h, and the salt acid treatment with 10%, then wash, drying;
(3) by the carbonizing production of step (2) and potassium hydroxide in mass ratio 1:3 mix, the water added with the volume mass of mixture than being 3:1(mL/g), mix, dry, control 10 ℃/min of programming rate, activate 1h under 750 ℃;
(4) activation products are added to water and soak under 90 ℃, filter, with boiling water, wash neutrality, obtain rice husk matrix activated carbon material, specific area 3235m after 100 ℃ of dry 12h
2/ g, average pore size 2.0nm;
Rice husk matrix activated carbon electrode preparation: by rice husk matrix activated carbon, acetylene black, PTFE in mass ratio 85:10:5 evenly spread in ethanol, add thermal agitation, roll-in is in blocks, under 15MPa, is pressed on nickel foam, makes rice husk matrix activated carbon electrode.
MnO
2Electrode preparation: by MnO
2, acetylene black, PTFE in mass ratio 80:10:10 evenly spread in ethanol, add thermal agitation, roll-in is in blocks, under 15MPa, is pressed on the collector nickel foam, makes rice husk matrix activated carbon electrode.
At 1M Na
2SO
4In, rice husk matrix activated carbon electrode shows the electric double layer capacitance behavior, MnO in the scope of-1.0-0.8V (vs SCE)
2Electrode shows capacitance behavior in the scope of-0.1-1.0V (vs SCE).Rice husk matrix activated carbon electrode is negative pole, MnO
2Electrode is anodal, 1M Na
2SO
4For electrolyte, all-glass paper is barrier film, is assembled into the asymmetrical type electric chemical super capacitor, and maximum operating voltage is 2V, and when power density is 165.2W/kg, energy density is 19.5Wh/kg.
Embodiment 2
The preparation of rice husk matrix activated carbon:
(1) by rice husk cleaning, dry, grinding;
(2) rice husk after step (1) is processed is under argon shield, 400 ℃ of lower charing 2h, and the salt acid treatment with 5%, then wash, drying;
(3) by the carbonizing production of step (2) and potassium hydroxide in mass ratio 1:4 mix, the water added with the volume mass of mixture than being 2:1(mL/g), mix, dry, control 10 ℃/min of programming rate, activate 2h under 700 ℃;
(4) activation products are added to water and soak under 100 ℃, filter, with boiling water, wash neutrality, obtain rice husk matrix activated carbon material, specific area 2824m after 100 ℃ of dry 12h
2/ g, average pore size 2.4nm;
The preparation of rice husk matrix activated carbon electrode: by rice husk matrix activated carbon, acetylene black, PTFE in mass ratio 85:10:5 evenly spread in ethanol, add thermal agitation, roll-in is in blocks, under 15MPa, is pressed on stainless (steel) wire, makes rice husk matrix activated carbon electrode.
PbO
2The preparation of electrode: first by thermal decomposition method, on the titanium matrix, prepare SnO
2-Sb
2O
5Intermediate layer, with Ti/SnO
2-Sb
2O
5For matrix, 0.1M Pb (NO
3)
2+ 0.01M NaF+0.01M HNO
3For electroplate liquid, 10mA/cm
2The current density galvanostatic deposition prepare PbO
2Electrode.
The rice husk matrix activated carbon electrode of take is negative pole, PbO
2Electrode is anodal, 1M H
2SO
4For electrolyte, all-glass paper is barrier film, is assembled into the asymmetrical type electric chemical super capacitor, and operating voltage range is 0.8V-2.0V, and when power density is 424W/kg, energy density is 48Wh/kg.
Embodiment 3
The preparation of rice husk matrix activated carbon:
(1) by rice husk cleaning, dry, grinding;
(2) rice husk after step (1) is processed is under nitrogen protection, 450 ℃ of lower charing 1h, and the sulfuric acid treatment with 10%, then wash, drying;
(3) by the carbonizing production of step (2) and NaOH in mass ratio 1:3 mix, the water added with the volume mass of mixture than being 4:1(mL/g), mix, dry, control 15 ℃/min of programming rate, activate 2h under 700 ℃;
(4) activation products are added to water and soak under 70 ℃, filter, with boiling water, wash neutrality, obtain rice husk matrix activated carbon material, specific area 2932m after 100 ℃ of dry 12h
2/ g, average pore size 2.2nm;
The preparation of rice husk matrix activated carbon electrode: by rice husk matrix activated carbon, acetylene black, PVDF in mass ratio 80:10:10 mix, with NMP furnishing pulpous state, be coated onto on aluminium foil, 120 ℃ of lower vacuumizes, obtain rice husk matrix activated carbon electrode.
The preparation of lithium titanate electrode: by lithium titanate, acetylene black, PVDF in mass ratio 70:20:10 mix, with NMP furnishing pulpous state, be coated onto on aluminium foil, 120 ℃ of lower vacuumizes, obtain the lithium titanate electrode.
Take rice husk matrix activated carbon electrode as anodal, and the lithium titanate electrode is negative pole, 1M LiPF
6(EC:DMC:EMC=1:1:1) be electrolyte, polypropylene screen is barrier film, is assembled into the asymmetrical type electric chemical super capacitor in glove box, and operating voltage range is 1.5-3.0V, and when its power density is 281W/kg, energy density is 53Wh/kg.
Claims (8)
1. the asymmetrical type electric chemical super capacitor based on rice husk matrix activated carbon material, by positive pole, negative pole, barrier film, electrolyte, positive wire, negative wire and shell, formed, it is characterized in that: the negative or positive electrode of described asymmetrical type electric chemical super capacitor contains the rice husk matrix activated carbon as active material, a utmost point of electric double layer energy storage principle very that contains the rice husk matrix activated carbon, another utmost point adopts fake capacitance electrode or battery class electrode, and electrolyte is aqueous electrolyte or organic electrolyte.
2. a kind of asymmetrical type electric chemical super capacitor based on the rice husk matrix activated carbon as claimed in claim 1, it is characterized in that: described fake capacitance electrode or battery class electrode are MnO
2, Mn
3O
4, Ni (OH)
2, the transition metal oxide such as NiO, battery electrode is PbO
2And lithium ion cell electrode.
3. a kind of asymmetrical type electric chemical super capacitor based on the rice husk matrix activated carbon as claimed in claim 1, it is characterized in that: described electrolyte comprises alkaline electrolyte, acidic electrolysis bath, neutral electrolyte, organic electrolyte.
4. the preparation method based on rice husk matrix activated carbon material claimed in claim 1: at least comprise the following steps:
(1) by rice husk cleaning, dry, grinding;
(2) by the rice husk charing under non-oxide condition after above-mentioned steps (1) grinding, with acid solution, process, then washing, drying, obtain carbide;
(3) carbide above-mentioned steps (2) obtained mixes in proportion with highly basic, adds certain water gaging to mix, and dries, and controls programming rate, and activation, obtain activation products;
(4) activation products that above-mentioned steps (3) obtained, with soaking in hot water, are filtered, and washing, to neutral, is ground to the 150-300 order and obtains the high specific capacitance absorbent charcoal material after drying.
5. a kind of preparation method based on rice husk matrix activated carbon material according to claim 4, it is characterized in that: in described step (2), non-oxide condition is that at least one gas by passing into to reaction system in carbon dioxide, nitrogen, argon gas obtains;
Carbonization temperature in described step (2) is 350-550 ℃, and carbonization time is 0.5-2h, and described acid solution can be at least one in hydrochloric acid, sulfuric acid.
6. a kind of preparation method based on rice husk matrix activated carbon material according to claim 4, it is characterized in that: in described step (3), highly basic is at least one in potassium hydroxide or NaOH, carbide and highly basic mass ratio are 1:(1-5), programming rate is 2-15 ℃/min, activation temperature is 600-900 ℃, activation 0.5-4h.
7. a kind of preparation method based on rice husk matrix activated carbon material according to claim 4, it is characterized in that: in described step (4), the hot water temperature is controlled at 50-100 ℃, and baking temperature is 100-120 ℃, and be 12-24h drying time.
8. according to the described a kind of preparation method based on rice husk matrix activated carbon material of arbitrary claim in claim 4-7, it is characterized in that: prepared rice husk matrix activated carbon material specific area out is 2000-3700m
2/ g, pore-size distribution is narrow, with micropore and mesopore, is distributed as the master.
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Cited By (8)
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| CN105321729A (en) * | 2015-11-23 | 2016-02-10 | 黑龙江大学 | Preparation method for nanometer graded porous carbon material used for high-performance electrochemical supercapacitor based on rice hull ash |
| CN108946712A (en) * | 2018-09-26 | 2018-12-07 | 西安交通大学苏州研究院 | Three-dimensional porous class grapheme material of high area specific capacity based on rice husk and preparation method thereof |
| CN109019567A (en) * | 2018-09-26 | 2018-12-18 | 西安交通大学苏州研究院 | Rice husk base class graphene porous carbon materials of high-volume and capacity ratio and preparation method thereof |
| CN109192540A (en) * | 2018-09-18 | 2019-01-11 | 中联西北工程设计研究院有限公司 | A kind of biomass carbonization product and manganese dioxide composite electrode material and preparation method thereof |
| CN109727786A (en) * | 2018-12-14 | 2019-05-07 | 河南豫氢动力有限公司 | Electrode material for lithium ion super capacitor |
| CN110610817A (en) * | 2019-10-09 | 2019-12-24 | 浙江天能能源科技股份有限公司 | Based on Mn3O4Supercapacitor made of graphene composite material and preparation method of supercapacitor |
| CN110942926A (en) * | 2019-12-20 | 2020-03-31 | 广西大学 | Bagasse-based activated carbon layered structure electrode material, preparation method thereof and application thereof in supercapacitor |
| CN111785536A (en) * | 2020-08-11 | 2020-10-16 | 苏州柯诺思高新材料有限公司 | Preparation method of asymmetric capacitor nano lead dioxide based composite electrode |
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| CN105321729A (en) * | 2015-11-23 | 2016-02-10 | 黑龙江大学 | Preparation method for nanometer graded porous carbon material used for high-performance electrochemical supercapacitor based on rice hull ash |
| CN105321729B (en) * | 2015-11-23 | 2017-12-08 | 黑龙江大学 | The method that the nanometer grading-hole carbon material for high-performance electric chemistry ultracapacitor is prepared based on rice hull ash |
| CN109192540A (en) * | 2018-09-18 | 2019-01-11 | 中联西北工程设计研究院有限公司 | A kind of biomass carbonization product and manganese dioxide composite electrode material and preparation method thereof |
| CN108946712A (en) * | 2018-09-26 | 2018-12-07 | 西安交通大学苏州研究院 | Three-dimensional porous class grapheme material of high area specific capacity based on rice husk and preparation method thereof |
| CN109019567A (en) * | 2018-09-26 | 2018-12-18 | 西安交通大学苏州研究院 | Rice husk base class graphene porous carbon materials of high-volume and capacity ratio and preparation method thereof |
| CN108946712B (en) * | 2018-09-26 | 2020-11-27 | 西安交通大学苏州研究院 | Rice hull-based three-dimensional porous graphene-like material with high area specific capacity and preparation method thereof |
| CN109727786A (en) * | 2018-12-14 | 2019-05-07 | 河南豫氢动力有限公司 | Electrode material for lithium ion super capacitor |
| CN110610817A (en) * | 2019-10-09 | 2019-12-24 | 浙江天能能源科技股份有限公司 | Based on Mn3O4Supercapacitor made of graphene composite material and preparation method of supercapacitor |
| CN110942926A (en) * | 2019-12-20 | 2020-03-31 | 广西大学 | Bagasse-based activated carbon layered structure electrode material, preparation method thereof and application thereof in supercapacitor |
| CN110942926B (en) * | 2019-12-20 | 2021-10-08 | 广西大学 | Bagasse-based activated carbon layered structure electrode material, preparation method thereof and application thereof in supercapacitor |
| CN111785536A (en) * | 2020-08-11 | 2020-10-16 | 苏州柯诺思高新材料有限公司 | Preparation method of asymmetric capacitor nano lead dioxide based composite electrode |
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Application publication date: 20131204 |