CN109192528B - Preparation method of polyaniline/manganese dioxide electrode material with three-dimensional network structure - Google Patents
Preparation method of polyaniline/manganese dioxide electrode material with three-dimensional network structure Download PDFInfo
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- CN109192528B CN109192528B CN201811026282.7A CN201811026282A CN109192528B CN 109192528 B CN109192528 B CN 109192528B CN 201811026282 A CN201811026282 A CN 201811026282A CN 109192528 B CN109192528 B CN 109192528B
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000007772 electrode material Substances 0.000 title claims abstract description 44
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 24
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 13
- MMCPOSDMTGQNKG-UJZMCJRSSA-N aniline;hydrochloride Chemical compound Cl.N[14C]1=[14CH][14CH]=[14CH][14CH]=[14CH]1 MMCPOSDMTGQNKG-UJZMCJRSSA-N 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 10
- 239000007800 oxidant agent Substances 0.000 claims abstract description 9
- 230000001590 oxidative effect Effects 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 239000007795 chemical reaction product Substances 0.000 claims description 9
- 239000012286 potassium permanganate Substances 0.000 claims description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- MMCPOSDMTGQNKG-UHFFFAOYSA-N anilinium chloride Chemical compound Cl.NC1=CC=CC=C1 MMCPOSDMTGQNKG-UHFFFAOYSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 229910021538 borax Inorganic materials 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 239000004328 sodium tetraborate Substances 0.000 claims description 3
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 3
- JYLNVJYYQQXNEK-UHFFFAOYSA-N 3-amino-2-(4-chlorophenyl)-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(CN)C1=CC=C(Cl)C=C1 JYLNVJYYQQXNEK-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 2
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 2
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 2
- 125000005619 boric acid group Chemical group 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 5
- 238000007599 discharging Methods 0.000 abstract description 3
- 230000008602 contraction Effects 0.000 abstract description 2
- 238000006116 polymerization reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 14
- 239000005457 ice water Substances 0.000 description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 4
- 238000012983 electrochemical energy storage Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- 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
- H01G11/46—Metal oxides
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- 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
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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
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Abstract
本发明的公开了一种具有增强三维网络结构的聚苯胺/二氧化锰电极材料的制备方法。该制备方法使苯胺盐酸盐、交联剂、高锰酸盐在聚乙烯醇水溶液中反应得聚苯胺/二氧化锰电极材料。本发明的制备方法在制备电极材料过程中，由于引入了聚乙烯醇和交联剂，得到了具有增强三维网络结构的聚苯胺/二氧化锰电极材料。这种增强的三维网络结构不仅可以克服聚苯胺在充放电过程中的膨胀与收缩，还可以对二氧化锰形成良好的保护，从而提升电极材料的稳定性；而且所有的原料，只需依次加入体系并混合均匀后，静置反应即可。在静置反应过程中，聚苯胺通过氧化聚合而形成，与此同时，氧化剂又被还原成二氧化锰。该制备方法简单易行。
The invention discloses a preparation method of polyaniline/manganese dioxide electrode material with enhanced three-dimensional network structure. In the preparation method, aniline hydrochloride, crosslinking agent and permanganate are reacted in a polyvinyl alcohol aqueous solution to obtain a polyaniline/manganese dioxide electrode material. In the preparation method of the present invention, in the process of preparing the electrode material, the polyaniline/manganese dioxide electrode material with enhanced three-dimensional network structure is obtained due to the introduction of polyvinyl alcohol and a cross-linking agent. This enhanced three-dimensional network structure can not only overcome the expansion and contraction of polyaniline during the charging and discharging process, but also form a good protection for manganese dioxide, thereby improving the stability of the electrode material; and all the raw materials only need to be added sequentially. After the system is mixed evenly, it can be allowed to stand for reaction. During the standing reaction, polyaniline is formed by oxidative polymerization, and at the same time, the oxidant is reduced to manganese dioxide. The preparation method is simple and easy to implement.
Description
Technical Field
The invention relates to the technical field of electrochemical energy storage, in particular to a preparation method of a polyaniline/manganese dioxide electrode material with an enhanced three-dimensional network structure.
Background
In recent years, the demand for clean and sustainable energy has been increasingly urgent due to serious environmental problems caused by the huge consumption of non-renewable fossil fuels. Supercapacitors are new electrochemical energy storage devices that have received much attention in the last decade, and compared to batteries and conventional capacitors, have the characteristics of high power density, long cycle life, and fast charge and discharge. Therefore, the super capacitor has been widely used in the fields of electric vehicles, mobile electronic products, and uninterruptible power supply. Supercapacitors can be broadly classified into various types according to the mechanism of electricity storage: (1) electric double layer capacitors, which store charge through the interface between an electrode and an electrolyte, such as supercapacitors using carbon materials as the electrode material; (2) pseudocapacitance (faraday capacitance), which generates electrical energy through reversible oxidation-reduction reaction (faraday charge transport reaction), such as supercapacitors using transition metal oxides, conductive polymers, etc. as electrode materials. Although the electrode material of the double-electric-conducting capacitance type, such as a carbon material, has excellent cycle stability, its specific volume is significantly lower than that of the pseudocapacitance electrode material. Therefore, the development of more novel pseudocapacitive electrode materials is a hot research content in the field of electrode materials of supercapacitors.
Polyaniline and manganese dioxide belong to conductive polymers and transition metal oxides respectively, and both have the advantages of simple synthesis method, low cost, environmental friendliness and high specific volume, and are two types of pseudo-capacitor electrode materials with the most development potential. However, they have inherent drawbacks such as poor conductivity of manganese dioxide and instability in acidic electrolytes, respectively; polyaniline is easy to expand and contract in the charging and discharging process, so that the cycle life is short and the like. In order to solve the above problems, researchers developed various polyaniline/manganese dioxide composite materials, which have good electrochemical energy storage characteristics, but the more complicated preparation methods may hinder their commercial applications to some extent.
Disclosure of Invention
The invention aims to provide a preparation method of a polyaniline/manganese dioxide electrode material with an enhanced three-dimensional network structure, aiming at the defects in the prior art.
The invention relates to a preparation method of a polyaniline/manganese dioxide electrode material with an enhanced three-dimensional network structure, which comprises the step of reacting aniline hydrochloride, a cross-linking agent and permanganate in a polyvinyl alcohol aqueous solution to obtain the polyaniline/manganese dioxide electrode material.
Preferably, the method further comprises placing the reaction product in a bulk deionized water purification equilibrium.
Preferably, the crosslinking agent is boric acid, borax, glutaraldehyde or epichlorohydrin.
Preferably, the mass concentration of the polyvinyl alcohol is 0.5-10 wt%.
Preferably, the mass concentration of the aniline hydrochloride is 0.02-2 mol/L.
Preferably, the mass ratio of the cross-linking agent to the polyvinyl alcohol is 0-0.5.
Preferably, the permanganate is potassium permanganate, sodium permanganate, or ammonium permanganate.
Preferably, the composite material further comprises an oxidant, wherein the oxidant is ammonium persulfate, ferric chloride, ferric nitrate or hydrogen peroxide.
Preferably, the mass ratio of the oxidant to the aniline hydrochloride is 0.01-2.
Preferably, the reaction time is 2-48 h.
According to the preparation method of the polyaniline/manganese dioxide electrode material with the enhanced three-dimensional network structure, in the process of preparing the electrode material, polyvinyl alcohol and a cross-linking agent are introduced, so that the polyaniline/manganese dioxide electrode material with the enhanced three-dimensional network structure is obtained. The enhanced three-dimensional network structure can not only overcome the expansion and contraction of polyaniline in the charging and discharging processes, but also form good protection to manganese dioxide, thereby improving the stability of the electrode material; and all the raw materials, such as polyvinyl alcohol, aniline hydrochloride, a cross-linking agent, an oxidizing agent and the like, are added into the system in sequence, uniformly mixed and then kept stand for reaction. During the standing reaction, polyaniline is formed by oxidative polymerization, and at the same time, the oxidizing agent is reduced to manganese dioxide. The preparation method is simple and easy to implement.
Drawings
FIG. 1 is a scanning electron micrograph of the polyaniline/manganese dioxide electrode material prepared in example 1.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
Example 1
Completely dissolving 1.0g of polyvinyl alcohol in 20mL of deionized water under the heating condition, and naturally cooling for later use. And (2) placing the prepared polyvinyl alcohol aqueous solution in an ice water bath, stirring, sequentially adding 2.07g of aniline hydrochloride, 0.05g of boric acid and 1.27g of potassium permanganate, uniformly stirring, and standing at room temperature for reaction for a certain time. And (3) purifying and balancing the reaction product in a large amount of deionized water to remove oligomers and inorganic matters, thus obtaining the polyaniline/manganese dioxide electrode material.
Example 2
1.0g of polyvinyl alcohol is completely dissolved in 20mL of deionized water at 90 ℃, and the solution is naturally cooled for later use. And (2) placing the prepared polyvinyl alcohol aqueous solution in an ice water bath, stirring, sequentially adding 1.65g of aniline hydrochloride, 0.05g of boric acid and 1.27g of potassium permanganate, uniformly stirring, and standing at room temperature for reaction for a certain time. And (3) purifying and balancing the reaction product in a large amount of deionized water to remove oligomers and inorganic matters, thus obtaining the polyaniline/manganese dioxide electrode material.
Example 3
1.0g of polyvinyl alcohol is completely dissolved in 20mL of deionized water at 90 ℃, and the solution is naturally cooled for later use. Placing the prepared polyvinyl alcohol aqueous solution in an ice water bath, stirring, sequentially adding 2.07g of aniline hydrochloride, 0.05g of boric acid, 1.27g of potassium permanganate and 1.82g of ammonium persulfate, uniformly stirring, and standing at room temperature for reaction for a certain time. And (3) purifying and balancing the reaction product in a large amount of deionized water to remove oligomers and inorganic matters, thus obtaining the polyaniline/manganese dioxide electrode material.
Example 4
1.0g of polyvinyl alcohol is completely dissolved in 20mL of deionized water at 90 ℃, and the solution is naturally cooled for later use. And (2) placing the prepared polyvinyl alcohol aqueous solution in an ice water bath, stirring, sequentially adding 2.07g of aniline hydrochloride, 0.05g of boric acid, 1.27g of potassium permanganate and 1.29g of ferric chloride, uniformly stirring, and standing at room temperature for reaction for a certain time. And (3) purifying and balancing the reaction product in a large amount of deionized water to remove oligomers and inorganic matters, thus obtaining the polyaniline/manganese dioxide electrode material.
Example 5
1.0g of polyvinyl alcohol is completely dissolved in 20mL of deionized water at 90 ℃, and the solution is naturally cooled for later use. Placing the prepared polyvinyl alcohol aqueous solution in an ice water bath, stirring, sequentially adding 2.07g of aniline hydrochloride, 0.05g of boric acid, 1.27g of potassium permanganate and 1.93g of ferric nitrate, uniformly stirring, and standing at room temperature for reaction for a certain time. And (3) purifying and balancing the reaction product in a large amount of deionized water to remove oligomers and inorganic matters, thus obtaining the polyaniline/manganese dioxide electrode material.
Example 6
0.5g of polyvinyl alcohol is completely dissolved in 20mL of deionized water at 85 ℃, and the solution is naturally cooled for later use. Placing the prepared polyvinyl alcohol aqueous solution in an ice water bath, stirring, sequentially adding 2.07g of aniline hydrochloride, 0.025g of boric acid, 1.27g of potassium permanganate and 1.82g of ammonium persulfate, uniformly stirring, and standing at room temperature for reaction for a certain time. And (3) purifying and balancing the reaction product in a large amount of deionized water to remove oligomers and inorganic matters, thus obtaining the polyaniline/manganese dioxide electrode material.
Example 7
1.0g of polyvinyl alcohol is completely dissolved in 20mL of deionized water at 85 ℃, and the solution is naturally cooled for later use. And (2) placing the prepared polyvinyl alcohol aqueous solution in an ice water bath, stirring, sequentially adding 2.07g of aniline hydrochloride, 0.05g of borax and 1.27g of potassium permanganate, uniformly stirring, and standing at room temperature for reaction for a certain time. And (3) purifying and balancing the reaction product in a large amount of deionized water to remove oligomers and inorganic matters, thus obtaining the polyaniline/manganese dioxide electrode material.
Referring to the drawings, fig. 1 is a scanning electron micrograph of the polyaniline/manganese dioxide electrode material prepared in example 1: (a) low magnification and (b) high magnification. As is apparent from the figure, the prepared electrode material has a typical three-dimensional interlaced network structure, and polyaniline and manganese dioxide active materials are uniformly loaded in the network structure. The polyaniline/manganese dioxide electrode material prepared by the preparation method disclosed by the invention has the advantages of enhanced three-dimensional network structure, simple preparation method and the like, and has great application prospects in the field of high-performance supercapacitor electrode materials.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (9)
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| CN103413689B (en) * | 2013-07-19 | 2016-08-10 | 北京科技大学 | Prepare graphene aerogel and the method for graphene/metal oxide aeroge |
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| Chemical crosslinking engineered nitrogen-doped carbon aerogels from polyaniline-boric acid-polyvinyl alcohol gels for high-performance electrochemical capacitors;Xianjun Wei, et al;《Carbon》;20170731;第471-480页 * |
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