CN105702479A - Preparation method and application of polyurethane-based porous carbon electrode material for supercapacitor - Google Patents
Preparation method and application of polyurethane-based porous carbon electrode material for supercapacitor Download PDFInfo
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- CN105702479A CN105702479A CN201610222338.0A CN201610222338A CN105702479A CN 105702479 A CN105702479 A CN 105702479A CN 201610222338 A CN201610222338 A CN 201610222338A CN 105702479 A CN105702479 A CN 105702479A
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- polyurethane
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 41
- 239000007772 electrode material Substances 0.000 title claims abstract description 38
- 239000004814 polyurethane Substances 0.000 title claims abstract description 35
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 40
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052786 argon Inorganic materials 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000004970 Chain extender Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 239000012948 isocyanate Substances 0.000 claims abstract description 5
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 3
- 239000003990 capacitor Substances 0.000 claims description 29
- 229920005862 polyol Polymers 0.000 claims description 18
- 150000003077 polyols Chemical class 0.000 claims description 18
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 16
- 229920000570 polyether Polymers 0.000 claims description 16
- 238000003763 carbonization Methods 0.000 claims description 13
- 239000011668 ascorbic acid Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 238000010000 carbonizing Methods 0.000 abstract 1
- 238000005266 casting Methods 0.000 abstract 1
- 230000007935 neutral effect Effects 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 53
- 239000003792 electrolyte Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 4
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical group NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 238000007605 air drying Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Polyurethanes Or Polyureas (AREA)
- Power Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
Abstract
The invention relates to a preparation method and application of a polyurethane-based porous carbon electrode material for a supercapacitor. The preparation method comprises the following steps of mixing a polyhydric alcohol constituent and a chain extender constituent, carrying out vacuum pumping in 110 DEG C, and reducing a temperature to 60 DEG C after half an hour; adding isocyanate for mixing, casting and forming, and enabling reaction to obtain a polyurethane material; carbonizing the obtained polyurethane material under argon protection, and activating the polyurethane material with KOH in 600-800 DEG C; and washing the obtained activated product with a diluted acid solution; washing the obtained activated product with distilled water to be neutral, drying the activated product, and finally obtaining the polyurethane-based porous carbon electrode material for the supercapacitor. The preparation method is simple in preparation process and is controllable; the polyurethane-based porous carbon electrode material for the supercapacitor, obtained through preparation, has the advantages of stable structure, excellent electrochemical performance, high cycle performance, high specific capacity and the like, and is very suitably taken as the electrode material applied to the field of the supercapacitor.
Description
Technical field
The invention belongs to new forms of energy technical field of electronic materials, relate to the preparation method and application of a kind of polyurethane-base porous carbon electrode material for super capacitor。
Background technology
Polyurethane full name is polyurethanes, is the general designation containing the macromolecular compound repeating carbamate groups on main chain, and it contains substantial amounts of carbamate groups, it is possible to prepare nitrogenous active carbon material as presoma。J.Hayashi et al. uses KOH 800oUnder C, polyurethane is activated, obtain specific surface area up to 2800m2Active carbon material (J.Hayashi, N.Yamamoto, T.Horikawa, K.Muroyama, V.G.Gomes, the Preparationandcharacterizationofhigh-specific-surface-ar eaactivatedcarbonsfromK of/g2CO3-treatedwastepolyurethane, JournalofColloidandInterfaceScience, 2005,281,437-443)。Chwang et al. makes aniline growth in situ on polyurethane, obtain the complex (Ching-PiouChwang of a kind of high-k (1120), Cheng-DarLiu, Sung-WeiHuang, Dean-YangChao, Sung-NungLee, Synthesisandcharacterizationofhighdielectricconstantpoly aniline/polyurethaneblends, SyntheticMetals, 2004,142,275-281)。Tai et al. passes through Graphene and polyurethane compound, obtain a kind of reasonable electrode material for super capacitor of electrical property, ratio electric capacity at 1A/g is 156F/g(ZhixinTai, XingbinYan, QunjiXue, Shape-alterableand-recoverablegraphene/polyurethanebi-la yeredcompositefilmforsupercapacitorelectrode, JournalofPowerSources, 2012,213,350-357)。
The preparation method that Chinese patent literature CN104843673A discloses a kind of porous carbon materials, comprises the following steps: polyurethane material is carried out by (1), standby after drying；(2) polyurethane material that step (1) obtains be impregnated in 1 ~ 72h in activator solution；Or directly both are mixed homogeneously for the ratio of 1:1 ~ 7:1 in mass ratio by activator with polyurethane material, then in 300 ~ 1500 under inert gas shieldingoC carbonization 0.5 ~ 4 hour, naturally cools to room temperature；(3) the product dilute acid soln or the dilute alkaline soln that step (2) are obtained are washed 1 ~ 3 time, are then washed with water to pH for neutrality；(4) step (3) is obtained product 70 ~ 130oAfter the air drying 1 ~ 72h of C, obtain porous carbon materials。When but the porous carbon materials that the method obtains does electrode material, more relatively low than electric capacity, when with the KOH of 6mol/L for electrolyte, constant-current discharge electric current density is only 287F/g when 0.125A/g than electric capacity。
Summary of the invention
For the deficiencies in the prior art, the invention provides the preparation method and application of the polyurethane-base porous carbon electrode material for super capacitor of a kind of, good cycle higher than electric capacity。
Technical scheme is as follows:
According to the present invention, the preparation method of a kind of polyurethane-base porous carbon electrode material for super capacitor, comprise the following steps that
(1) polyol component and chain extender component are mixed, 110oEvacuation under C, is cooled to 60 after half an houroC；
(2) isocyanates mixing cast molding are added, 80oC~120oC reacts 20 hours, obtains polyurethane material；
(3) polyurethane material step (2) obtained is under argon shield, in 500oC carbonization 2h；
(4) material with carbon element obtained for step (3) be impregnated in 6 ~ 48h in KOH solution, then in 600 under argon shieldoC~800oC activates 1h ~ 4h, naturally cools to room temperature；Wherein, material with carbon element is 1:1 ~ 3:1 with the mass ratio of KOH；
(5) product dilute acid soln washing step (4) obtained, is then washed with distilled water to neutrality；
(6) product step (5) obtained is 40oC~80oUnder C after dry 12 ~ 24h, obtain polyurethane-base porous carbon electrode material for super capacitor。
According to the invention it is preferred to, the polyhydric alcohol in step (1) is polyether polyol 3600, polyether polyol 3628, and wherein polyether polyol 3600, polyether polyol 3628 can be passed through to be either commercially available。
According to the invention it is preferred to, the chain extender in step (1) is E300, and it can pass through to be either commercially available。
According to the invention it is preferred to, the isocyanates in step (2) is methyl diphenylene diisocyanate。
According to the invention it is preferred to, the reaction temperature described in step (2) is 100oC。
According to the invention it is preferred to, the activation temperature described in step (4) is 750oC。
According to the invention it is preferred to, the mass ratio of the material with carbon element described in step (4) and KOH is 2:1。
According to the invention it is preferred to, the soak time described in step (4) is 2h。
The application of a kind of polyurethane-base porous carbon electrode material for super capacitor, for the electrode material of ultracapacitor。
The technical advantage of the present invention is as follows:
(1) preparation process of the present invention is simple, has controllability, it is possible to control specific surface area and the pore structure of material with carbon element by controlling the ratio of polyurethane and KOH。
(2) the polyurethane-base porous carbon electrode material for super capacitor that the present invention prepares has Stability Analysis of Structures, electrochemical performance, good cycle and specific capacitance advantages of higher, is highly suitable as electrode material and is applied to ultracapacitor field。
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the polyurethane-base porous carbon electrode material for super capacitor that the embodiment of the present invention 1 prepares。
Fig. 2 is the constant current charge-discharge figure of the polyurethane-base porous carbon electrode material for super capacitor that the embodiment of the present invention 1 prepares。
Fig. 3 is the energy-power density map of the polyurethane-base porous carbon electrode material for super capacitor that the embodiment of the present invention 1 prepares。
Detailed description of the invention
Below in conjunction with specific embodiments and the drawings, the present invention is described further, but is not limited to this。
Experimental technique described in following embodiment, if no special instructions, is conventional method simultaneously；Described reagent and material, if no special instructions, all commercially obtain。
Embodiment 1:
3600,20 parts of polyether polyol 3628 of 40 parts of polyether polyol and 10 parts of chain extender E300 mixing, 110oEvacuation under C, is cooled to 60 after half an houroC；Then, add 65 parts of methyl diphenylene diisocyanate mixing cast molding, 80oC reacts 20 hours, obtains polyurethane material；The polyurethane material obtained is under argon shield, in 500oC carbonization 2h；
The polyurethane material of carbonization be impregnated in 24h in KOH solution, then in 750 under argon shieldoC activates 2h, naturally cools to room temperature；Wherein, material with carbon element is 2:1 with the mass ratio of KOH
The product dilute hydrochloric acid solution washing that will obtain, is then washed with distilled water to neutrality；The product obtained is 40oUnder C after dry 24h, obtain polyurethane-base porous carbon electrode material for super capacitor。
Adopting three-electrode system, with 6mol/L potassium hydroxide solution for electrolyte, it is 395F/g that 1A/g records than electric capacity, and stability is better。
The present embodiment prepare polyurethane-base porous carbon electrode material for super capacitor scanning electron microscope (SEM) photograph as it is shown in figure 1, as shown in Figure 1 polymer be by the tridimensional network of near-spherical material buildup。
The constant current charge-discharge of the polyurethane-base porous carbon electrode material for super capacitor that the present embodiment prepares is as shown in Figure 2, as shown in Figure 2, it is 395F/g that 1A/g records than electric capacity, it is 682F/g that 0.5A/g records than electric capacity, it is 337F/g that 2A/g records than electric capacity, it is 311F/g that 3A/g records than electric capacity, and stability is better。
The present embodiment prepare polyurethane-base porous carbon electrode material for super capacitor energy-power as it is shown on figure 3, from the figure 3, it may be seen that this material power density be 1440Wkg-1Time, energy density is 74.2Whkg-1。
Embodiment 2:
3600,20 parts of polyether polyol 3628 of 40 parts of polyether polyol and 10 parts of chain extender E300 mixing, 110oEvacuation under C, is cooled to 60 after half an houroC；Then, add 65 parts of methyl diphenylene diisocyanate mixing cast molding, 80oC reacts 20h, obtains polyurethane material；The polyurethane material obtained is under argon shield, in 500oC carbonization 2h；
The polyurethane material of carbonization be impregnated in 24h in KOH solution, then in 750 under argon shieldoC activates 2h, naturally cools to room temperature；Wherein, material with carbon element is 1:1 with the mass ratio of KOH；
Wash with dilute hydrochloric acid solution, be then washed with distilled water to neutrality；The product obtained is 40oUnder C after dry 24h, obtain polyurethane-base porous carbon electrode material for super capacitor。
Adopting three-electrode system, with 6mol/L potassium hydroxide solution for electrolyte, it is 197F/g that 1A/g records than electric capacity, and stability is better。
Embodiment 3:
3600,20 parts of polyether polyol 3628 of 40 parts of polyether polyol and 10 parts of chain extender E300 mixing, 110oEvacuation under C, is cooled to 60 after half an houroC；Then, add 65 parts of methyl diphenylene diisocyanate mixing cast molding, 80oC reacts 20 hours, obtains polyurethane material；The polyurethane material obtained is under argon shield, in 500oC carbonization 2h；
The polyurethane material of carbonization be impregnated in 24h in KOH solution, then in 750 under argon shieldoC activates 2h, naturally cools to room temperature；Wherein, material with carbon element is 3:1 with the mass ratio of KOH
Wash with dilute hydrochloric acid solution, be then washed with distilled water to neutrality；The product obtained is 40oUnder C after dry 24h, obtain polyurethane-base porous electrode material for super capacitor。
Adopting three-electrode system, with 6mol/L potassium hydroxide solution for electrolyte, it is 327F/g that 1A/g records than electric capacity, and stability is better。
Embodiment 4:
3600,20 parts of polyether polyol 3628 of 40 parts of polyether polyol and 10 parts of chain extender E300 mixing, 110oEvacuation under C, is cooled to 60 after half an houroC；Then, add 65 parts of methyl diphenylene diisocyanate mixing cast molding, 120oC reacts 20 hours, obtains polyurethane material；The polyurethane material obtained is under argon shield, in 500oC carbonization 2h；
The polyurethane material of carbonization be impregnated in 24h in KOH solution, then in 600 under argon shieldoC activates 1h, naturally cools to room temperature；Wherein, material with carbon element is 2:1 with the mass ratio of KOH
Wash with dilute hydrochloric acid solution, be then washed with distilled water to neutrality；The product obtained is 40oUnder C after dry 24h, obtain polyurethane-base porous electrode material for super capacitor。
Adopting three-electrode system, with 6mol/L potassium hydroxide solution for electrolyte, it is 182F/g that 1A/g records than electric capacity, and stability is better。
Embodiment 5:
3600,20 parts of polyether polyol 3628 of 40 parts of polyether polyol and 10 parts of chain extender E300 mixing, 110oEvacuation under C, is cooled to 60 after half an houroC；Then, add 65 parts of methyl diphenylene diisocyanate mixing cast molding, 100oC reacts 20 hours, obtains polyurethane material；The polyurethane material obtained is under argon shield, in 500oC carbonization 2h；
The polyurethane material of carbonization be impregnated in 24h in KOH solution, then in 800 under argon shieldoC activates 4h, naturally cools to room temperature；Wherein, material with carbon element is 2:1 with the mass ratio of KOH
Wash with dilute hydrochloric acid solution, be then washed with distilled water to neutrality；The product obtained is 40oUnder C after dry 24h, obtain polyurethane-base porous electrode material for super capacitor。
Adopting three-electrode system, adopting 6mol/L potassium hydroxide solution is electrolyte, and it is 306F/g that 1A/g records than electric capacity, and stability is better。
Claims (9)
1. a preparation method for polyurethane-base porous carbon electrode material for super capacitor, comprises the following steps that
(1) polyol component and chain extender component are mixed, 110oEvacuation under C, is cooled to 60 after half an houroC；
(2) isocyanates mixing cast molding are added, 80oC~120oC reacts 20 hours, obtains polyurethane material；
(3) polyurethane material step (2) obtained is under argon shield, in 500oC carbonization 2h；
(4) material with carbon element that step (3) obtains be impregnated in 6 ~ 48h in KOH solution, then in 600 under argon shieldoC~800oC activates 1h ~ 4h, naturally cools to room temperature；Wherein, material with carbon element is 1:1 ~ 3:1 with the mass ratio of KOH；
(5) product dilute acid soln washing step (4) obtained, is then washed with distilled water to neutrality；
(6) product step (5) obtained is 40oC~80oUnder C after dry 12 ~ 24h, obtain polyurethane-base porous carbon electrode material for super capacitor。
2. the preparation method of polyurethane-base porous carbon electrode material for super capacitor according to claim 1, it is characterised in that the polyhydric alcohol in step (1) is polyether polyol 3600, polyether polyol 3628。
3. the preparation method of polyurethane-base porous carbon electrode material for super capacitor according to claim 1, it is characterised in that the chain extender in step (1) is E300。
4. the preparation method of polyurethane-base porous carbon electrode material for super capacitor according to claim 1, it is characterised in that the isocyanates in step (2) is methyl diphenylene diisocyanate。
5. the preparation method of polyurethane-base porous carbon electrode material for super capacitor according to claim 1, it is characterised in that the reaction temperature described in step (2) is 100oC。
6. the preparation method of polyurethane-base porous carbon electrode material for super capacitor according to claim 1, it is characterised in that the activation temperature described in step (4) is 750oC。
7. the preparation method of polyurethane-base porous carbon electrode material for super capacitor according to claim 1, it is characterised in that the mass ratio of the material with carbon element described in step (4) and KOH is 2:1。
8. the preparation method of polyurethane-base porous carbon electrode material for super capacitor according to claim 1, it is characterised in that the soak time described in step (4) is 2h。
9. an application for polyurethane-base porous carbon electrode material for super capacitor, for the electrode material of ultracapacitor。
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| CN201610222338.0A CN105702479B (en) | 2016-04-12 | 2016-04-12 | A kind of preparation method and application of polyurethane porous carbon electrode material for super capacitor |
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| CN110407605A (en) * | 2019-08-07 | 2019-11-05 | 哈尔滨师范大学 | A kind of preparation process of porous super capacitor material |
| CN111261421A (en) * | 2020-01-20 | 2020-06-09 | 上海应用技术大学 | Polyurethane-based nitrogen-phosphorus co-doped carbon material and preparation and application thereof |
| CN112441583A (en) * | 2020-12-25 | 2021-03-05 | 齐鲁工业大学 | Preparation method and application of gelatin-based porous carbon electrode material |
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| CN110407605A (en) * | 2019-08-07 | 2019-11-05 | 哈尔滨师范大学 | A kind of preparation process of porous super capacitor material |
| CN111261421A (en) * | 2020-01-20 | 2020-06-09 | 上海应用技术大学 | Polyurethane-based nitrogen-phosphorus co-doped carbon material and preparation and application thereof |
| CN112441583A (en) * | 2020-12-25 | 2021-03-05 | 齐鲁工业大学 | Preparation method and application of gelatin-based porous carbon electrode material |
| CN115331969A (en) * | 2021-05-10 | 2022-11-11 | 万华化学(四川)有限公司 | Porous electrode material and preparation method thereof |
| CN115331969B (en) * | 2021-05-10 | 2023-07-11 | 万华化学(四川)有限公司 | Porous electrode material and preparation method thereof |
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