CN103943375B - A kind of sandwich-like manganese dioxide/polyaniline composite material and preparation method thereof - Google Patents
A kind of sandwich-like manganese dioxide/polyaniline composite material and preparation method thereof Download PDFInfo
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- CN103943375B CN103943375B CN201410193973.1A CN201410193973A CN103943375B CN 103943375 B CN103943375 B CN 103943375B CN 201410193973 A CN201410193973 A CN 201410193973A CN 103943375 B CN103943375 B CN 103943375B
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- potassium permanganate
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 38
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 28
- 239000003960 organic solvent Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 239000008367 deionised water Substances 0.000 abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 5
- 239000003990 capacitor Substances 0.000 abstract description 5
- 239000007772 electrode material Substances 0.000 abstract description 4
- 241000446313 Lamella Species 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract 1
- 238000007254 oxidation reaction Methods 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 44
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 10
- 239000010410 layer Substances 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 235000011149 sulphuric acid Nutrition 0.000 description 4
- 239000001117 sulphuric acid Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000010406 interfacial reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 208000035126 Facies Diseases 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000004627 transmission electron microscopy Methods 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
- H01G11/48—Conductive polymers
-
- 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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The present invention relates to a kind of sandwich-like manganese dioxide/polyaniline composite material and preparation method thereof, belong to novel energy Material Field.Aniline is dissolved and obtains aniline organic solution in organic solvent, potassium permanganate is dissolved and obtains potassium permanganate solution in deionized water, and control the pH value of potassium permanganate solution, two kinds of solution are carried out Cold pretreatment respectively；Potassium permanganate solution is introduced to aniline organic solution surface, forms two-phase interface, react 12 48 hours under the conditions of 04 DEG C；Product through filtering, washing, be dried prepare sandwich-like manganese dioxide/polyaniline composite material.In acid condition, the polyaniline of oxidation polymerization has the highest electrical conductivity, and polyaniline is between manganese dioxide lamella simultaneously, effectively prevent it and reunites, significantly play the performances such as high specific capacitance, laid a good foundation in the application of electrode material for super capacitor for it.
Description
Technical field
The invention belongs to novel energy Material Field, be specifically related to a kind of sandwich-like manganese dioxide/polyaniline composite material and preparation method thereof.
Background technology
Ultracapacitor, as a kind of novel energy storage element, has the many merits such as efficiency for charge-discharge height, service life cycle length, green non-pollution, has broad application prospects in fields such as mobile communication, electric automobile, Aero-Space.Since it is suggested, just paid close attention to by the world.Ultracapacitor is divided into double layer capacitor and Faraday pseudo-capacitance device according to energy storage mechnism, and main electrode material has material with carbon element, transition-metals and their oxides, conducting polymer and composite.
Manganese dioxide, because having high theoretical ratio electric capacity and energy density, has abundant reserves at nature simultaneously, is used as the ideal material of electrode of super capacitor.But, there is many problems to be solved in manganese dioxide: (1) manganese dioxide granule is easily reunited and caused actual capacity to be much smaller than theoretical capacity；(2) relative to other bi-materials, the electronic conductivity of manganese dioxide is relatively low, causes capacitor internal resistance excessive, easily generates heat, and capacitance fade is too fast simultaneously.Therefore, by preparing high-ratio surface with other material compound materials, the composite of high conductivity is current focus.In acid condition, the polyaniline of doped polymeric has very high conductivity, is the compound optimum selection of manganese dioxide.
Summary of the invention
It is an object of the invention to provide a kind of high performance sandwich-like manganese dioxide/polyaniline composite material and preparation method thereof, manganese dioxide lamella is alternately superposed with polyaniline and makes sandwich-like manganese dioxide/polyaniline composite material, in acid condition, the polyaniline that doped polymeric generates substantially increases the electric conductivity of composite, polyaniline effectively inhibits the reunion of manganese dioxide lamella simultaneously, the performance such as high specific capacitance having given full play to manganese dioxide.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of preparation method of sandwich-like manganese dioxide/polyaniline composite material, using aniline organic solution as organic facies, potassium permanganate acidic aqueous solution is as inorganic phase, use organic and inorganic interfacial reaction, react a period of time under cryogenic, last sucking filtration, wash, be dried and be prepared for manganese dioxide/polyaniline composite material alternately layer by layer.
Specifically, a kind of preparation method of sandwich-like manganese dioxide/polyaniline composite material, aniline is dissolved and obtains aniline organic solution in organic solvent, potassium permanganate is dissolved and obtains potassium permanganate solution in deionized water, two kinds of solution are carried out respectively Cold pretreatment, and the pH value regulating potassium permanganate solution is 1 ~ 4；Potassium permanganate solution is introduced to aniline organic solution surface, forms two-phase interface, react 12-48 hour under the conditions of 0-4 DEG C；Product through filtering, washing, be dried prepare sandwich-like manganese dioxide/polyaniline composite material.
Described organic solvent is one or more in carbon tetrachloride, toluene, dichlorotoleune.
In aniline organic solution, aniline with the volume ratio of organic solvent is: 1-10:100.
The concentration of potassium permanganate solution is 0.001 ~ 0.01mg/mL.
Described Cold pretreatment is for sealing solution, be positioned over 0 ~ 5 DEG C of K cryogenic treatment 30 ~ 50min.
The application of sandwich-like manganese dioxide/polyaniline composite material that preparation method as above prepares, is specially the electrode material being used as ultracapacitor.
The beneficial effects of the present invention is:
(1) in acid condition, the polyaniline that doped polymeric generates has good electrical conductivity, utilize organic and inorganic interfacial reaction, the manganese dioxide/polyaniline composite material of preparation sandwich-like simultaneously, effectively inhibit manganese dioxide agglomeration during cycle charge-discharge；
(2) due to manganese dioxide and polyaniline layer by layer between synergism, composite has the performance such as high conductivity, high specific capacitance, lays a good foundation in the application of electrode material for super capacitor for it.
Accompanying drawing explanation
Fig. 1 is the TEM figure of the manganese dioxide/polyaniline composite material of the sandwich-like that example 1 prepares；
Fig. 2 is the FT-IR figure of the manganese dioxide/polyaniline composite material of the sandwich-like that example 1 prepares；
Fig. 3 is the charge-discharge figure of the manganese dioxide/polyaniline composite material of the sandwich-like that example 1 prepares.
Detailed description of the invention
Present invention the following example further illustrates the present invention, but protection scope of the present invention is not limited to the following example.
The preparation method of a kind of sandwich-like manganese dioxide/polyaniline composite material, concretely comprises the following steps:
(1) measure aniline (through 2 distilations), be dissolved in 100mL organic solvent, be configured to the organic solution of respective concentration；
(2) weigh potassium permanganate solid, be dissolved in 100mL deionized water, and use sulfur acid for adjusting pH, be configured to the aqueous solution of respective concentration；
(3) the above-mentioned solution prepared is positioned under cryogenic conditions (0 ~ 5 DEG C) pretreatment 30 ~ 50min, then potassium permanganate solution is slowly introduced in aniline organic solution, after forming stable organic and inorganic solution, under the conditions of being placed in 0-4 DEG C, react 12-48h；
(4) by above-mentioned solution sucking filtration, wash, be dried, obtain end product.
Embodiment
1
(1) measure 1mL aniline monomer, be dissolved in the carbon tetrachloride organic solvent of 100mL, obtain aniline organic solution；
(2) weigh 0.1mg potassium permanganate solid, be dissolved in the deionized water of 100mL, obtain the potassium permanganate solution of 0.001mg/mL, be 3 with concentrated sulphuric acid regulation pH value；
(3) pretreatment 30min under the conditions of above-mentioned solution being placed in 0 ~ 5 DEG C, is then introduced to potassium permanganate solution aniline organic solution surface, forms organic-inorganic solution；Under the conditions of being placed in 0 DEG C again, react 24h；
(4) by solution sucking filtration obtained above, wash, be dried, obtain end product, be sandwich-like manganese dioxide/polyaniline composite material.
Embodiment
2
(1) measure 2mL aniline monomer, be dissolved in the carbon tetrachloride organic solvent of 100mL, obtain aniline organic solution；
(2) weigh 1mg potassium permanganate solid, be dissolved in the deionized water of 100mL, obtain the potassium permanganate solution of 0.01mg/mL, be 3 with concentrated sulphuric acid regulation pH value；
(3) pretreatment 40min under the conditions of above-mentioned solution being all placed in 0 ~ 5 DEG C, then introduces potassium permanganate solution aniline organic solution surface, forms organic-inorganic solution；Under the conditions of being placed in 4 DEG C again, react 48h；
(4) by solution sucking filtration obtained above, wash, be dried, obtain end product, be sandwich-like manganese dioxide/polyaniline composite material.
Embodiment
3
(1) measure 10mL aniline monomer, be dissolved in the carbon tetrachloride organic solvent of 100mL, obtain aniline organic solution；
(2) weigh 0.2mg potassium permanganate solid to estimate, be dissolved in the deionized water of 100mL, obtain the potassium permanganate solution of 0.002mg/mL, be 3 with concentrated sulphuric acid regulation pH value；
(3) pretreatment 30min under the conditions of above-mentioned solution being all placed in 0 ~ 5 DEG C, then introduces potassium permanganate solution aniline organic solution surface, forms organic-inorganic solution；Under the conditions of being placed in 2 DEG C again, react 12h；
(4) by solution sucking filtration obtained above, wash, be dried, obtain end product, be sandwich-like manganese dioxide/polyaniline composite material.
Embodiment
4
(1) measure 1mL aniline monomer, be dissolved in the carbon tetrachloride organic solvent of 100mL, obtain aniline organic solution；
(2) weigh 0.5mg potassium permanganate solid, be dissolved in the deionized water of 100mL, obtain the potassium permanganate solution of 0.005mg/mL, be 1 with concentrated sulphuric acid regulation pH value；
(3) pretreatment 30min under the conditions of above-mentioned solution being all placed in 0 ~ 5 DEG C, then introduces potassium permanganate solution aniline organic solution surface, forms organic-inorganic solution；Under the conditions of being placed in 0 DEG C again, react 24h；
(4) by solution sucking filtration obtained above, wash, be dried, obtain end product, be sandwich-like manganese dioxide/polyaniline composite material.
Sandwich-like manganese dioxide/the polyaniline composite material preparing embodiment 1 carries out transmission electron microscopy sign, Fourier-infrared spectrum characterization, charge-discharge sign；Fig. 1 shows that unformed polyaniline molecule chain, along manganese dioxide layer growth, and then has constructed the structure in interlayer；524cm in Fig. 2-1For Mn-O-Mn absworption peak in manganese dioxide, 1050 cm-1For the C-H stretching vibration absworption peak in polyaniline, 1412 cm-1With 1635
cm-1Respectively phenyl ring and the vibration absorption peak of quinoid ring, 1635
cm-1For the C=N vibration absorption peak in polyaniline, 3425cm-1Then the absworption peak for the-OH in N-H and hydrone collectively forms, and shows to generate manganese dioxide/Polyaniline；From figure 3, it can be seen that the electrode prepared with sandwich-like manganese dioxide/polyaniline composite material has good charge-discharge performance, under the electric current density of 0.1A/g, electric capacity can reach 192.8F/g.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent and modification, all should belong to the covering scope of the present invention.
Claims (2)
1. the preparation method of sandwich-like manganese dioxide/polyaniline composite material, it is characterised in that: first aniline organic solution, potassium permanganate solution are carried out Cold pretreatment, and the pH value regulating potassium permanganate solution is 1-3；Then potassium permanganate solution is introduced to aniline organic solution surface, forms two-phase interface, react 12-48 hour under the conditions of 0-4 DEG C；Product through filtering, washing, be dried prepare sandwich-like manganese dioxide/polyaniline composite material；The concentration of potassium permanganate solution is 0.001 ~ 0.01mg/mL；Described Cold pretreatment processes 30 ~ 50min for solution seals, is positioned over 0 ~ 5 DEG C.
The preparation method of sandwich-like manganese dioxide/polyaniline composite material the most according to claim 1, it is characterised in that: in aniline organic solution, aniline with the volume ratio of organic solvent is: 1-10:100.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410193973.1A CN103943375B (en) | 2014-05-09 | 2014-05-09 | A kind of sandwich-like manganese dioxide/polyaniline composite material and preparation method thereof |
| PCT/CN2015/070020 WO2015169104A1 (en) | 2014-05-09 | 2015-01-04 | Sandwich-like manganese dioxide/polyaniline composite material and preparation method therefor |
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| CN201410193973.1A CN103943375B (en) | 2014-05-09 | 2014-05-09 | A kind of sandwich-like manganese dioxide/polyaniline composite material and preparation method thereof |
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| CN103943375B true CN103943375B (en) | 2016-10-05 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103943375B (en) * | 2014-05-09 | 2016-10-05 | 福州大学 | A kind of sandwich-like manganese dioxide/polyaniline composite material and preparation method thereof |
| CN105070514B (en) * | 2015-07-06 | 2017-10-20 | 常州大学 | Interface method prepares polyaniline/graphene/manganese dioxide composite material applied to ultracapacitor |
| CN106215522B (en) * | 2016-09-12 | 2018-04-13 | 福州大学 | The method of in-situ preparation nano flower-like manganese dioxide-catalyst on filtrate |
| CN112125334A (en) * | 2019-06-24 | 2020-12-25 | 厦门稀土材料研究所 | Metal oxide/carbon intercalated layer two-dimensional composite material and preparation method and application thereof |
| CN110922752B (en) * | 2019-11-26 | 2022-03-01 | 武汉工程大学 | Polyaniline and manganese dioxide nano composite material and preparation method and application thereof |
| CN111627716B (en) * | 2020-04-28 | 2022-06-10 | 沈阳大学 | Porous flower spherical conductive polyaniline/MnO2Process for preparing nano composite material |
| CN112795052A (en) * | 2020-12-30 | 2021-05-14 | 苏州中科先进技术研究院有限公司 | Porous polyaniline nano-film loaded with nano zero-valent iron and preparation method and application thereof |
| CN114976166A (en) * | 2022-06-20 | 2022-08-30 | 中国科学技术大学 | Oxidation-resistant cation exchange membrane, preparation method thereof and oxidation-resistant membrane electrode |
| CN115612486B (en) * | 2022-10-31 | 2024-02-13 | 扬州大学 | Cobalt/manganese dioxide quantum dot with uricase-like activity and preparation method thereof |
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| CN1303138C (en) * | 2005-07-21 | 2007-03-07 | 华东理工大学 | Preparation method of conductive polyaniline intercalated laminated manganese dioxide nano-composite material |
| CN101696323B (en) * | 2009-10-30 | 2012-03-21 | 华南师范大学 | Method for preparing polyaniline/manganese dioxide composite material for super capacitor |
| CN102977602B (en) * | 2012-12-11 | 2014-08-20 | 华东理工大学 | Preparation method of manganese dioxide/carbon material/conducting polymer composite material |
| CN103943375B (en) * | 2014-05-09 | 2016-10-05 | 福州大学 | A kind of sandwich-like manganese dioxide/polyaniline composite material and preparation method thereof |
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| CN103943375A (en) | 2014-07-23 |
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