CN101774567A - Method for preparing multilevel pore carbon electrode material of super capacitor - Google Patents
Method for preparing multilevel pore carbon electrode material of super capacitor Download PDFInfo
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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 a multilevel pore carbon electrode material of a super capacitor, comprising the following steps: (1) preparing the mixing solution of ethyl alcohol and water, adding a surfactant and a phenol compound into the mixture, stirring until the mixture is dissolved, adding concentrated hydrochloric acid into the solution, stirring until the solution is pink, then adding methanal, stirring to generate solid phenolic resin at the bottom of the solution, aging the phenolic resin in the solution, taking out, and then aging at 100 DEG C; (2) carbonizing aged phenolic resin under the protection of nitrogen at 850 DEG C to obtain a mesoporous carbon material; (3) smashing the mesoporous carbon material to less than 50 meshes, and then activating by an activating agent under the protection of nitrogen; and (4) washing the activated product by deionized water and drying to obtain the microporous-mesoporus multilevel pore carbon electrode material. In the invention, mesoporus carbon with even pore size distribution is prepared firstly, and then micropores are produced on the pore wall of the mesoporus carbon in the activation process to obtain the multilevel pore carbon electrode material with directly communicated mircropores and mesopores.
Description
Technical field
The present invention relates to the preparation method of electrode material for super capacitor, particularly a kind of preparation method of multilevel pore carbon electrode material.
Background technology
Ultracapacitor is the another novel energy-storing device that has the widespread use potentiality after lithium ion battery, and it promptly has the high-specific-power and the high cycle characteristics of conventional electrical condenser, has the high energy storage capacity characteristics of battery again.Therefore, it can satisfy the demand of high-specific-power, can satisfy the needs than high-energy-density again.Since it compare with secondary cell have leakage current little, discharge and recharge characteristics such as simple, that specific power is high and have extended cycle life, thereby can with secondary cell form hybrid power system be used to satisfy automobile start, quicken, superpower requirement when climbing.The electrostatic double layer that the energy storage mechanism of ultracapacitor is based on electrode formation under charging comes energy storage.Electrode materials is one of key factor of decision ultracapacitor performance, and the electrochemical capacitor performance of common gac and active carbon with high specific surface area is unsatisfactory, and especially power out-put characteristic is relatively poor.This is because gac contains too much micropore, lacks mesoporously, and the diffusional resistance of electrolyte ion in the gac duct is too big.In recent years, people have studied novel mesoporous carbon electrode materials such as charcoal gel, CNT (carbon nano-tube), ordered mesoporous carbon.These carbon electrode materials have bigger hole dimension, thereby power out-put characteristic is good.But these raw material of wood-charcoal material lack micropore, thereby littler than capacitance, and specific power is low.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of micropore-mesopore multilevel pore carbon electrode material, and it not only has high energy density, and has power out-put characteristic preferably.
The preparation method of a kind of multilevel pore carbon electrode material of super capacitor of the present invention is characterized in that comprising the steps:
(1) the configuration quality ratio is 10: 9 the alcohol and the mixing solutions 146g of water, 25g tensio-active agent and 25 gram phenol compounds are added in the mixing solutions, induction stirring is to dissolving fully, the concentrated hydrochloric acid that adds 1.6mL 37wt% then in the solution, induction stirring becomes pink until solution, at this moment, the formaldehyde that adds 26g 37wt% again in the solution, stir solution bottom generation resol solid after 5 hours, resol is aging after 12 hours in solution, from solution, take out, wore out 12 hours down at 100 ℃;
(2) resol after will wearing out under nitrogen protection 850 ℃ carbonization 1-4 hour, obtain meso-porous carbon material;
(3) meso-porous carbon material is crushed to below 50 orders, and activates under nitrogen protection after the activator mix;
(4) activation products obtain the multistage hole of micropore-mesopore carbon electrode material after deionized water thorough washing, oven dry.
Wherein optimized technical scheme is:
Institute's tensio-active agent that uses is the polyoxyethylene-poly-oxypropylene polyoxyethylene triblock polymer Pluronic P123 ((EO) of BASF Aktiengesellschaft's production in the step (1)
20(PO)
70(EO)
20, molecular weight 5800), Pluronic F88 ((EO)
104(PO)
39(EO)
104, molecular weight 11400), Pluronic F127 ((EO)
97(PO)
69(EO)
97, molecular weight 12600) in a kind of.A kind of as in phenol, Resorcinol, the Phloroglucinol of the phenol compound that uses.
The used activator of step (2) is a kind of in KOH, NaOH and the zinc chloride, and the mass ratio of meso-porous carbon material and activator is 1: 1-1: 5.Activation temperature is 800-1000 ℃.
The present invention at first adopts, and organic-organic self-assembly method prepares the mesoporous charcoal of even aperture distribution, makes micropore on by the hole wall of reactivation process in mesoporous carbon, obtains the multilevel pore carbon electrode material of micropore and mesoporous direct UNICOM.This carbon electrode material has overcome gac class electrode materials and has lacked the shortcoming that mesoporous and carbon nanotube, carbon gel etc. lack micropore, and high-specific-power and high-energy-density are combined.
Embodiment
Embodiment 1
The configuration quality ratio is 10: 9 the alcohol and the mixing solutions 146g of water, and 25g Pluronic F127 and 25 gram Phloroglucinols are added in the mixing solutions, and induction stirring is to dissolving fully.Add the concentrated hydrochloric acid of 1.6mL 37wt% then in the solution, induction stirring becomes pink until solution.At this moment, add the formaldehyde of 26g 37% in the solution, stirs solution bottom generation resol solid after 5 hours.Resol is aging in solution to be taken out from solution after 12 hours, wore out 12 hours down at 100 ℃.Resol after aging at 850 ℃ of following carbonization 1-4 hours, is obtained meso-porous carbon material.Carbonized product is crushed to below 50 orders, mixes back 800 ℃ of activation under nitrogen protection at 1: 2 with the KOH mass ratio.Activation products obtain the multistage hole of micropore-mesopore carbon electrode material after deionized water thorough washing, oven dry.The nitrogen adsorption test shows, the specific surface area of multistage hole carbon is 1204m
2/ g, wherein mesoporous specific surface area is 603m
2/ g, micropore specific area are 601m
2/ g, pore volume are 0.88cm
3/ g.Below can carry out routinely, be electrode materials with the multistage hole carbon that makes, with the preparation multistage hole charcoal and the polytetrafluoroethylene (PTFE) emulsion according to 95: 5 uniform mixing of mass ratio, size mixing, evenly spread upon on the nickel foam collector, be pressed into electrode slice, under 120 ℃, dry to constant weight.After vacuum is fully flooded in the KOH of 30wt% solution with the electrode slice after two oven dry and porous polypropylene barrier film, be assembled into the capacitor unit of sandwich structure.On electrochemical workstation, carry out the constant current charge-discharge test.The test voltage scope is 0-0.9V.When output rating was 534W/kg, useful energy density was 4.18Wh/kg.When output rating was 5.34kW/kg, useful energy density was 2.94Wh/kg.
Embodiment 2
The configuration quality ratio is 10: 9 the alcohol and the mixing solutions 146g of water, and 25g Pluronic P123 and 25 gram Resorcinols are added in the mixing solutions, and induction stirring is to dissolving fully.Add the concentrated hydrochloric acid of 1.6mL 37wt% then in the solution, induction stirring becomes pink until solution.At this moment, add the formaldehyde of 26g 37% in the solution, stirs solution bottom generation resol solid after 5 hours.Resol is aging in solution to be taken out from solution after 12 hours, wore out 12 hours down at 100 ℃.Resol after aging at 850 ℃ of following carbonization 1-4 hours, is obtained meso-porous carbon material.Carbonized product is crushed to below 50 orders, mixes back 900 ℃ of activation under nitrogen protection at 1: 4 with the KOH mass ratio.Activation products obtain the multistage hole of micropore-mesopore carbon electrode material after deionized water thorough washing, oven dry.The nitrogen adsorption test shows, the specific surface area of multistage hole carbon is 1706m
2/ g, wherein mesoporous specific surface area is 910m
2/ g, micropore specific area are 796m
2/ g, pore volume are 1.32cm
3/ g.Below press embodiment 1 described ordinary method preparation and test.When output rating was 496W/kg, useful energy density was 4.92Wh/kg.When output rating was 4.7kW/kg, useful energy density was 3.83Wh/kg.
Embodiment 3
The configuration quality ratio is 10: 9 the alcohol and the mixing solutions 146g of water, and 25g Pluronic P123 and 25 gram Resorcinols are added in the mixing solutions, and induction stirring is to dissolving fully.Add the concentrated hydrochloric acid of 1.6mL 37wt% then in the solution, induction stirring becomes pink until solution.At this moment, add the formaldehyde of 26g 37% in the solution, stirs solution bottom generation resol solid after 5 hours.Resol is aging in solution to be taken out from solution after 12 hours, wore out 12 hours down at 100 ℃.Resol after aging at 850 ℃ of following carbonization 1-4 hours, is obtained meso-porous carbon material.Carbonized product is crushed to below 50 orders, mixes back 900 ℃ of activation under nitrogen protection at 1: 2 with the NaOH mass ratio.Activation products obtain the multistage hole of micropore-mesopore carbon electrode material after deionized water thorough washing, oven dry.The nitrogen adsorption test shows, the specific surface area of multistage hole carbon is 1296m
2/ g, wherein mesoporous specific surface area is 667m
2/ g, micropore specific area are 629m
2/ g, pore volume are 0.91cm
3/ g.Below press embodiment 1 described ordinary method preparation and test.When output rating was 528W/kg, useful energy density was 3.84Wh/kg.When output rating was 5.21kW/kg, useful energy density was 2.43Wh/kg.
Embodiment 4
The configuration quality ratio is 10: 9 the alcohol and the mixing solutions 146g of water, and 25g Pluronic F127 and 25 gram Phloroglucinols are added in the mixing solutions, and induction stirring is to dissolving fully.Add the concentrated hydrochloric acid of 1.6mL 37wt% then in the solution, induction stirring becomes pink until solution.At this moment, add the formaldehyde of 26g 37% in the solution, stirs solution bottom generation resol solid after 5 hours.Resol is aging in solution to be taken out from solution after 12 hours, wore out 12 hours down at 100 ℃.Resol after aging at 850 ℃ of following carbonization 1-4 hours, is obtained meso-porous carbon material.Carbonized product is crushed to below 50 orders, mixes back 800 ℃ of activation under nitrogen protection at 1: 4 with the NaOH mass ratio.The nitrogen adsorption test shows, the specific surface area of multistage hole carbon is 1605m
2/ g, wherein mesoporous specific surface area is 955m
2/ g, micropore specific area are 650m
2/ g, pore volume are 1.23cm
3/ g.Activation products obtain the multistage hole of micropore-mesopore carbon electrode material after deionized water thorough washing, oven dry.Below press embodiment 1 described ordinary method preparation and test.When output rating was 488W/kg, useful energy density was 5.09Wh/kg.When output rating was 4.90kW/kg, useful energy density was 3.93Wh/kg.
Embodiment 5
The configuration quality ratio is 10: 9 the alcohol and the mixing solutions 146g of water, and 25g Pluronic F127 and 25 gram Phloroglucinols are added in the mixing solutions, and induction stirring is to dissolving fully.Add the concentrated hydrochloric acid of 1.6mL 37wt% then in the solution, induction stirring becomes pink until solution.At this moment, add the formaldehyde of 26g 37% in the solution, stirs solution bottom generation resol solid after 5 hours.Resol is aging in solution to be taken out from solution after 12 hours, wore out 12 hours down at 100 ℃.Resol after aging at 850 ℃ of following carbonization 1-4 hours, is obtained meso-porous carbon material.Carbonized product is crushed to below 50 orders, with ZnCl
2Mass ratio mixes back 700 ℃ of activation under nitrogen protection at 1: 4.Activation products obtain the multistage hole of micropore-mesopore carbon electrode material after deionized water thorough washing, oven dry.The nitrogen adsorption test shows, the specific surface area of multistage hole carbon is 1578m
2/ g, wherein mesoporous specific surface area is 832m
2/ g, micropore specific area are 746m
2/ g, pore volume are 1.21cm
3/ g.Below press embodiment 1 described ordinary method preparation and test.When output rating was 448W/kg, useful energy density was 4.78Wh/kg.When output rating was 4.84kW/kg, useful energy density was 3.49Wh/kg.
Claims (5)
1. the preparation method of a multilevel pore carbon electrode material of super capacitor is characterized in that comprising the steps:
(1) the configuration quality ratio is 10: 9 the alcohol and the mixing solutions 146g of water, 25g tensio-active agent and 25 gram phenol compounds are added in the mixing solutions, induction stirring is to dissolving fully, the concentrated hydrochloric acid that adds 1.6mL 37wt% then in the solution, induction stirring becomes pink until solution, at this moment, the formaldehyde that adds 26g 37wt% again in the solution, stir solution bottom generation resol solid after 5 hours, resol is aging after 12 hours in solution, from solution, take out, wore out 12 hours down at 100 ℃;
(2) resol after will wearing out under nitrogen protection 850 ℃ carbonization 1-4 hour, obtain meso-porous carbon material;
(3) meso-porous carbon material is crushed to below 50 orders, and activates under nitrogen protection after the activator mix;
(4) activation products obtain the multistage hole of micropore-mesopore carbon electrode material after deionized water thorough washing, oven dry.
2. preparation method according to claim 1 is characterized in that tensio-active agent described in the step (1) is a kind of among PluronicP123, Pluronic F88, the Pluronic F127.
3. preparation method according to claim 1 is characterized in that phenol compound described in the step (1) is a kind of in phenol, Resorcinol, the Phloroglucinol.
4. preparation method according to claim 1 is characterized in that activator described in the step (3) is a kind of in KOH, NaOH and the zinc chloride, and the mass ratio of meso-porous carbon material and activator is 1: 1-1: 5.
5. preparation method according to claim 1 is characterized in that activation temperature is 700-1100 ℃ described in the step (3).
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