CN102101668A - Method for preparing activated carbon of high-specific capacitance super capacitor - Google Patents
Method for preparing activated carbon of high-specific capacitance super capacitor Download PDFInfo
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- CN102101668A CN102101668A CN2010105831342A CN201010583134A CN102101668A CN 102101668 A CN102101668 A CN 102101668A CN 2010105831342 A CN2010105831342 A CN 2010105831342A CN 201010583134 A CN201010583134 A CN 201010583134A CN 102101668 A CN102101668 A CN 102101668A
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a method for preparing activated carbon of a high-specific capacitance super capacitor. The method is characterized by comprising the following steps of: selecting low-rank coal as a raw material; separating a vitrinite and an inertinite from the low-rank coal by steps such as pretreatment, maceral separation and the like; and preparing the activated carbon of the super capacitor in the activation mode of combining rapid temperature raise, low and medium-temperature activation and rapid reaction termination by taking two organic macerals as precursors and KOH as an active agent. Thus, an activation process of the activated carbon is greatly shortened, a part of rich surface functional groups in the precursors are maintained while the activated carbon has a higher specific surface area and rational pore size distribution so as to improve the surface wettability of the activated carbon, and a pseudo-capacitance effect is introduced to further improve the specific capacitance of the super capacitor. The specific surface area of the activated carbon prepared by the method can reach 2,523m<2>/g, the mesopore rate reaches 58.5 percent, and the specific capacitance can reach 421F/g and the energy density can reach 11.8Wh/kg when the activated carbon is used as a super capacitor electrode.
Description
Technical field
The present invention relates to a kind of preparation method of active carbon, relate to a kind of preparation method of high specific capacitance amount activated carbon for super capacitors specifically, this method is particularly useful for preparing high specific capacitance amount activated carbon for super capacitors.
Background technology
Ultracapacitor is the novel energy-storing device of a class between ordinary capacitor and battery, it has the big and high advantage of secondary cell energy density of ordinary capacitor power density concurrently, and charge velocities fast, have extended cycle life, environmentally safe, have broad application prospects in fields such as electromobile, information technology, space flight and aviation and science and techniques of defence.In recent years, along with the continuous expansion in supercapacitor applications field, people have proposed urgent requirement to the ultracapacitor with height ratio capacity, good stability.
Ultracapacitor mainly is made up of parts such as current collection fluid, electrolytic solution, electrode materials, barrier films, and wherein electrode materials plays key effect to the performance of ultracapacitor, and it is the core component of ultracapacitor.At present, although new material emerges in an endless stream, gac with its good electrical conductivity, high specific surface area, stable chemical property, controlled pore structure and cheap advantages such as price, is the first-selection of electrode material for super capacitor still always.
Coal is not only fine fuel, and is valuable raw material of wood-charcoal material, is the high quality raw material of producing gac.The technology that with the coal is the feedstock production gac is quite ripe.Be that the patent documentation of CN1202004C and CN1178853C discloses with the coal as publication number be raw material, adopt the active carbon from coal of physical activation method preparation as gas phase and liquid phase adsorption agent.Publication number is the preparation method that the patent documentation of CN1120800C discloses a kind of coal-based mesopore activated carbon.Publication number is that the patent documentation of CN1032056C discloses and utilizes high quality brown coal to prepare the high absorption property gac.
Mainly rely on static charge between electrode and electrolyte interface, to form the electrostatic double layer storage power based on ultracapacitor, therefore require electrode materials should have higher specific surface area.Theoretically, the specific surface area of active carbon electrode material is big more, and the specific capacitance of ultracapacitor is big more, but practical situation are much complicated.Because except specific surface area, the pore size distribution of gac, surface wettability, surface functional group and electroconductibility etc. all have material impact to the chemical property of ultracapacitor.Only take all factors into consideration various factors, select reasonable raw material and activating process, just can prepare activated carbon for super capacitors with high specific capacitance amount.Obviously, the prepared gac of above-mentioned patented method and being unwell to as activated carbon for super capacitors.
Characteristics such as in addition, coal kind is various, metamorphic grade is different, content of mineral substances is big have determined to be that the difficulty of activated carbon for super capacitors of feedstock production stable performance is very big with the coal.Coal is a kind of baroque organic mixture, can be divided into the maceralss such as vitrinite, chitin group and inertinite of different in kind at microscopically.Can break the investigator and often coal be made the as a whole conventional thought mode for preparing gac, and be that the research that raw material prepares activated carbon for super capacitors does not appear in the newspapers as yet with the organic micropetrological unit of coal.Document 1(novel charcoal material, 2000,15(2): 61-64), document 2(coal journal, 2000,25(3): 299-302) and document 3(novel charcoal material, 2005,20(1): be raw material once 63-66) with the vitrinite and the inertinite of enrichment, through processes such as moulding, charing and steam activations, make specific surface and be about 1000m
2The common columnar activated carbon of/g, such gac specific surface area is relatively low, and pore structure is based on micropore, and do not consider the particular requirement of activated carbon for super capacitors in the preparation process, so also be not suitable for use in electrode material for super capacitor.
The KOH activation method is subjected to vast scientific research person's favor, and is successfully applied to the activated carbon for super capacitors preparation field as one of effective ways that prepare active carbon with high specific surface area.Disclosing with the stalk as the patent documentation of publication number CN100572270C is raw material, KOH is that activator prepares the organic system activated carbon for super capacitors, be that 3:1 mixes with KOH according to mass ratio after the raw material charing, activate 1.5 hours down at 680～760 ℃, can make than electric capacity is the absorbent charcoal material of 221F/g; Application number is that 200810121556.0 patent documentation discloses with biomass is raw material, KOH is an activator, adopt the two stage activation legal system to be equipped with activated carbon for super capacitors, its two stage activation temperature is respectively 500～600 ℃, 700～900 ℃, and soak time is 2～3 hours.Analyze and find, adopt the KOH activation method to prepare in the prior art of activated carbon for super capacitors, activation condition is relatively harsher, generally all adopt the temperature rise rate of 5～20 ℃/min, under high temperature (700～900 ℃) condition, activate 1～3 hour, and activation is generally adopted the naturally cooling mode after finishing, and the activation course is long, energy consumption and production cost height.In addition, high-temperature activation is strong to the corrodibility of equipment, and manual operation is dangerous high, is unfavorable for large-scale commercial production.
Summary of the invention
Purpose of the present invention provides at existing weak point in the above-mentioned prior art just that a kind of raw material sources are extensive, activation condition is gentle, with short production cycle, cost is low, specific surface area is high, pore size distribution is reasonable, good conductivity, and have the preparation method of the high specific capacitance amount activated carbon for super capacitors of excellent electrochemical performance.
The present invention is that precursor prepares activated carbon for super capacitors with vitrinite in the low-rank coal and inertinite, its method characteristics are that the brown coal or the long-flame coal of selection low metamorphic grade is raw material, pass through processing steps such as raw materials pretreatment, micropetrological unit separation, activation, acidleach, washing successively, make the activated carbon for super capacitors material; In the reactivation process of gac, adopt be rapidly heated, activation method that middle low-temperature activation and reaction stop combining fast carries out.
Purpose of the present invention can realize by following technique measures:
Preparation method of the present invention comprises the steps:
A, raw materials pretreatment: with one or both the mixture in brown coal, the long-flame coal (brown coal of low metamorphic grade, long-flame coal) be raw material, by broken, screening, collect the material of granularity 2～0.5mm;
B, micropetrological unit are separated: with ZnCl
2Solution adopts the material after densimetry is handled step a to carry out sorting as heavy-fluid, roughly select out vitrinite and inertinite in the material, wash repeatedly with distilled water, filtration, dry, fine grinding, make granularity less than 0.074mm, further selected to two kinds of micropetrological units of roughly selecting out in separating centrifuge then, isolate final vitrinite and inertinite, distilled water washes repeatedly, filtration, drying;
C, activation: vitrinite and inertinite that step b is separated mix, flood by mass ratio 1:1～1:5 with the powdery KOH of purity more than 85% respectively; Then the gained solidliquid mixture is placed the reaction that has nickel metal reaction still to stop device fast, under nitrogen atmosphere, temperature rise rate with 30～50 ℃/min is warming up to 180 ℃, and under this temperature constant temperature 0.5 hour to remove the moisture in the mixture, being warming up to 400～600 ℃ with identical temperature rise rate again activates, when activation temperature reaches preset temperature, stop priming reaction by reacting quick termination device fast cooling;
D, product aftertreatment: the activation products that step c obtains are passed through acidleach successively, are washed to neutrality, filtration, drying, promptly obtain final activated carbon for super capacitors product.
It mainly is to utilize reaction to stop device fast to make the activation products under the hot conditions reduce to room temperature rapidly by the circulating water bath that reaction described in the step c of the present invention stops device fast.The concrete technical characterictic that reaction stops device fast sees publication number for details: CN201632255U, name are called " a kind of reaction stops device fast " utility model patent.
The present invention in gac reactivation process, adopt and be rapidly heated (30～50 ℃/min), middle low-temperature activation (400～600 ℃) and reaction stop the activation method that combines fast, can effectively shorten the activation course of gac.
The separation of micropetrological unit mainly adopts densimetry to roughly select-the selected sorting process of separating centrifuge, isolated organic micropetrological unit purity height.
Compared with the prior art, beneficial effect of the present invention is as follows:
1, for high specific capacitance amount ultracapacitor, gac is except requiring to have higher specific surface area and the rational pore size distribution, also should have suitable and compose and deposit stable surface functional group, to improve the surface wettability of gac, reduce electrolyte ion at the intrapore diffusional resistance of gac, improve the surface-area utilization ratio of gac, can also produce additional Faraday pseudo-capacitance simultaneously, and then improve the specific capacitance of ultracapacitor.The present invention is considering each organic micropetrological unit formation condition of coal, elementary composition, chemical property, on the basis of aspect such as structure and mineral content difference, it is good to make full use of the low-rank coal reactivity, short texture, characteristics such as functional group and side chain isoreactivity group rich, with vitrinite in the low-rank coal and inertinite is precursor, employing is rapidly heated, the activation method that the quick termination of middle low-temperature activation and reaction combines, shorten the activation course greatly, when guaranteeing that gac has higher specific surface area and reasonable pore size distribution, keep the part surface functional group of being rich in vitrinite and the inertinite, to improve the wettability of gac to electrolyte ion, and introduce the fake capacitance effect, and then improve the specific capacitance of ultracapacitor.
2, the present invention adopt be rapidly heated, middle low-temperature activation and reaction stop the activation method that combines fast, activation condition gentleness, technical process are simple, the safety coefficient height, have shortened the activation course, have reduced energy consumption, alleviate in the reactivation process equipment corrosion.
3, to adopt aboundresources, cheap low-rank coal be raw material in the present invention, reduced the production cost of gac, helps realizing suitability for industrialized production.In addition, utilize the coal micropetrological unit to prepare activated carbon for super capacitors, make the preparation of activated carbon for super capacitors not be subjected to the restriction in the coal kind and the place of production, also provide foundation simultaneously for the stable high performance active carbon of processability.
4, activated carbon for super capacitors provided by the invention has higher specific capacitance and energy density.Experimental results show that, through optimize the quality of activated carbon for super capacitors in 3mol/L KOH electrolytic solution that make behind the processing parameter than electrical capacity up to 421F/g, energy density is up to 11.8Wh/kg, with application number is that 200710171260.5 the disclosed active carbon electrode material of patent documentation is compared, chemical property is with the obvious advantage, has broad application prospects.
Description of drawings
Fig. 1 for the embodiment of the invention 2 at the constant current charge-discharge curve (current density 50mA/g) of activation temperature when being 600 ℃ of following institute preparing active carbons as electrode material for super capacitor
Fig. 2 for the embodiment of the invention 2 at the cyclic voltammetry curve of activation temperature when being 600 ℃ of following institute preparing active carbons as electrode material for super capacitor.
Embodiment
The present invention is further described below with reference to embodiment:
Embodiment 1
A, be raw material with in Inner Mongol brown coal, Yunnan brown coal or the Yima long-flame coal any one, through material broken, that granularity 2～0.5mm is collected in the screening back;
B, with ZnCl
2Solution adopts densimetry that the material to step a gained granularity 2～0.5mm is carried out sorting as heavy-fluid, roughly select out vitrinite and inertinite in each feed coal respectively, wash repeatedly with distilled water, filtration, dry, fine grinding, make granularity less than 0.074mm, further selected to two kinds of micropetrological units of roughly selecting out in separating centrifuge then, isolate final vitrinite and inertinite, distilled water washes repeatedly, filtration, drying;
C, isolated each vitrinite of step b and inertinite are mixed, flood by mass ratio 1:3 with the powdery KOH of purity more than 85% respectively; Then the gained solidliquid mixture being placed the reaction that has nickel metal reaction still to stop device fast activates; Temperature control program is: be warming up to 180 ℃ from room temperature with the temperature rise rate of 30 ℃/min, and constant temperature dehydration in 0.5 hour under this temperature, continuing to be warming up to 600 ℃ with identical temperature rise rate again activates, when activation temperature reaches 600 ℃, utilize reaction to stop device fast, bathing rapidly by circulating water, cooling stops priming reaction; Carry out in nitrogen atmosphere in the whole reactivation process, gas flow is 200ml/min;
After d, activation finish, collect activation products, adopt 5mol/L HCl to soak after 2 hours, distilled water washes repeatedly to neutrality, filters, promptly obtains the activated carbon for super capacitors product after the drying.Each structure of activated carbon parameter is as shown in table 1.
Prepared gac is processed into the electrode for super capacitor material, and is assembled into the simulation ultracapacitor and carries out electro-chemical test, the concrete grammar of electrode materials processing and the assembling of simulation ultracapacitor is with reference to " material Leader " 2009,23(22): P107.Through constant current charge-discharge test (current density 50mA/g), the chemical property index of each active carbon electrode material is as follows:
Made structure of activated carbon parameter of table 1 different material and chemical property index thereof
Embodiment 2
Adopt the method identical to isolate inertinite in Indonesia's brown coal, and it is mixed, floods by mass ratio 1:4 with the powdery KOH of purity more than 85% with embodiment 1; Then the gained solidliquid mixture being placed the reaction that has nickel metal reaction still to stop device fast activates; Temperature control program is: be warming up to 180 ℃ from room temperature with the temperature rise rate of 40 ℃/min, and constant temperature dehydration in 0.5 hour under this temperature, continuing to be warming up to predefined temperature with identical temperature rise rate again activates, when activation temperature reaches preset temperature, utilize reaction to stop device fast, bathe cooling termination priming reaction rapidly by circulating water, wherein predetermined activation temperature is respectively 400 ℃, 450 ℃, 500 ℃, 550 ℃, 600 ℃; Carry out in nitrogen atmosphere in the whole reactivation process, gas flow is 400ml/min; After activating end, collect activation products, adopt 5mol/L HCl to soak after 2 hours, distilled water washes repeatedly to neutrality, promptly obtains the activated carbon for super capacitors product after filtration, the drying.Each structure of activated carbon parameter and chemical property index thereof are as shown in table 2.
Made structure of activated carbon parameter and chemical property index thereof under the different activation temperatures of table 2
Embodiment 3
Is that 1:1 mixes with Shenmu County, Shaanxi long-flame coal and Inner Mongol brown coal according to mass ratio, adopt the method identical to isolate vitrinite and inertinite in the mixed coal, and two kinds of micropetrological units are mixed, flooded by mass ratio 1:5 with the powdery KOH of purity more than 85% respectively with embodiment 1; Then the gained solidliquid mixture being placed the reaction that has nickel metal reaction still to stop device fast activates; Temperature control program is: be warming up to 180 ℃ from room temperature with the temperature rise rate of 50 ℃/min, and constant temperature dehydration in 0.5 hour under this temperature, continuing to be warming up to 500 ℃ with identical temperature rise rate again activates, when activation temperature reaches 500 ℃, utilize reaction to stop device fast, bathing rapidly by circulating water, cooling stops priming reaction; Carry out in nitrogen atmosphere in the whole reactivation process, gas flow is 500ml/min; After activating end, collect activation products, adopt 5mol/L HCl to soak after 2 hours, distilled water washes repeatedly to neutrality, promptly obtains the activated carbon for super capacitors product after filtration, the drying.Two kinds of structure of activated carbon parameters and chemical property index thereof are as shown in table 3.
Made structure of activated carbon parameter of table 3 mixed coal and chemical property index thereof
Claims (1)
1. the preparation method of a high specific capacitance amount activated carbon for super capacitors, it is characterized in that: described preparation method comprises the steps:
A, raw materials pretreatment: with one or both the mixture in brown coal, the long-flame coal be raw material, by broken, screening, collect the material of granularity 2～0.5mm;
B, micropetrological unit are separated: with ZnCl
2Solution adopts the material after densimetry is handled step a to carry out sorting as heavy-fluid, roughly select out vitrinite and inertinite in the material, wash repeatedly with distilled water, filtration, dry, fine grinding, make granularity less than 0.074mm, further selected to two kinds of micropetrological units of roughly selecting out in separating centrifuge then, isolate final vitrinite and inertinite, distilled water washes repeatedly, filtration, drying;
C, activation: vitrinite and inertinite that step b is separated mix, flood by mass ratio 1:1～1:5 with the powdery KOH of purity more than 85% respectively; Then the gained solidliquid mixture is placed the reaction that has nickel metal reaction still to stop device fast, under nitrogen atmosphere, temperature rise rate with 30～50 ℃/min is warming up to 180 ℃, and under this temperature constant temperature 0.5 hour to remove the moisture in the mixture, being warming up to 400～600 ℃ with identical temperature rise rate again activates, when activation temperature reaches preset temperature, stop priming reaction by reacting quick termination device fast cooling;
D, product aftertreatment: the activation products that step c obtains are passed through acidleach successively, are washed to neutrality, filtration, drying, promptly obtain final activated carbon for super capacitors product.
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Cited By (8)
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| CN103496698A (en) * | 2013-10-14 | 2014-01-08 | 中国林业科学研究院林产化学工业研究所 | Method for preparing activated carbon high in specific surface area by activation in self-generated pressure |
| CN103551238A (en) * | 2013-10-31 | 2014-02-05 | 神华集团有限责任公司 | Enrichment method of coal micromaceral |
| CN103964433A (en) * | 2013-09-03 | 2014-08-06 | 内蒙古工业大学 | Preparation method of coal-based activated carbon for electrode material of supercapacitor |
| CN108373155A (en) * | 2018-03-26 | 2018-08-07 | 北京合众汇能科技有限公司 | A method of preparing high volume energy density capacitor activated carbon |
| CN109179404A (en) * | 2018-09-12 | 2019-01-11 | 宁夏宝塔石化煤化工研究院有限公司 | A method of using jet coal prepare in big mesoporous activated carbon |
| US10475595B2 (en) | 2016-05-20 | 2019-11-12 | Avx Corporation | Ultracapacitor for use at high temperatures |
| US10658127B2 (en) | 2016-05-20 | 2020-05-19 | Avx Corporation | Nonaqueous electrolyte for an ultracapacitor |
| US10679798B2 (en) | 2016-05-20 | 2020-06-09 | Avx Corporation | Ultracapacitor containing thin electrodes in a metal container |
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| CN101037200A (en) * | 2007-03-19 | 2007-09-19 | 合肥工业大学 | Method for preparing active carbon material for organic super capacitor by using straw |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103964433A (en) * | 2013-09-03 | 2014-08-06 | 内蒙古工业大学 | Preparation method of coal-based activated carbon for electrode material of supercapacitor |
| CN103496698A (en) * | 2013-10-14 | 2014-01-08 | 中国林业科学研究院林产化学工业研究所 | Method for preparing activated carbon high in specific surface area by activation in self-generated pressure |
| CN103496698B (en) * | 2013-10-14 | 2016-03-23 | 中国林业科学研究院林产化学工业研究所 | The method of active carbon with high specific surface area is prepared in spontaneous pressure activation |
| CN103551238A (en) * | 2013-10-31 | 2014-02-05 | 神华集团有限责任公司 | Enrichment method of coal micromaceral |
| CN103551238B (en) * | 2013-10-31 | 2016-08-24 | 神华集团有限责任公司 | The enrichment method of coal macerals |
| US10475595B2 (en) | 2016-05-20 | 2019-11-12 | Avx Corporation | Ultracapacitor for use at high temperatures |
| US10658127B2 (en) | 2016-05-20 | 2020-05-19 | Avx Corporation | Nonaqueous electrolyte for an ultracapacitor |
| US10679798B2 (en) | 2016-05-20 | 2020-06-09 | Avx Corporation | Ultracapacitor containing thin electrodes in a metal container |
| US10840031B2 (en) | 2016-05-20 | 2020-11-17 | Avx Corporation | Ultracapacitor for use at high temperatures |
| CN108373155A (en) * | 2018-03-26 | 2018-08-07 | 北京合众汇能科技有限公司 | A method of preparing high volume energy density capacitor activated carbon |
| CN109179404A (en) * | 2018-09-12 | 2019-01-11 | 宁夏宝塔石化煤化工研究院有限公司 | A method of using jet coal prepare in big mesoporous activated carbon |
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