CN105801854A - Method for preparing conducting polypyrrole by using malic acid as template and doping agent - Google Patents
Method for preparing conducting polypyrrole by using malic acid as template and doping agent Download PDFInfo
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- CN105801854A CN105801854A CN201610246116.2A CN201610246116A CN105801854A CN 105801854 A CN105801854 A CN 105801854A CN 201610246116 A CN201610246116 A CN 201610246116A CN 105801854 A CN105801854 A CN 105801854A
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- malic acid
- ice
- polypyrrole
- water bath
- pyrroles
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0605—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0611—Polycondensates containing five-membered rings, not condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring, e.g. polypyrroles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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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 discloses a method for preparing conducting polypyrrole by using malic acid as a template and a doping agent. The method comprises the steps that a certain amount of pyrrole is dispersed into water solutions containing malic acid of different proportions, and sufficient stirring is performed in an ice-water bath to obtain an uniform mixed solution, then, an oxidative initiation agent-ammonium persulfate are added dropwisely, pyrrole polymerization is triggered, and a reaction is performed for 12 h under stirring in the ice-water bath; then, deionized water is used for performing washing and suction filtration on a prepared polypyrrole head product till the filtrate is neutral; finally, drying is performed for 24 h under the temperature of 50 DEG C, and grinding and collection are performed to obtain conducting polypyrrole. The method has the advantages that the preparation process is simple, environmentally friendly and reliable, raw materials are wide in source, low in cost and suitable for industrial production, and the obtained conducting polypyrrole has the electrochemical performances of low resistance, high specific capacitance, high energy density and the like.
Description
Technical field
The invention belongs to electric polypyrrole preparing technical field, particularly to a kind of method preparing electric polypyrrole for template and adulterant with malic acid.It particularly relates to one is with malic acid for template and adulterant, the method that pyrroles prepares the electric polypyrrole with outstanding chemical property by self assembly and chemical oxidising polymerisation.
Background technology
Polypyrrole is as the one of conductive high polymer, owing to it has higher electrical conductivity, the features such as the redox mechanism of good chemistry, environmental stability and uniqueness, are widely used in the field such as energy storage material of sensor, anti-corrosion material, advanced battery and ultracapacitor.Polypyrrole owing to having environmental protection, cost is low, synthesis is simple and the doping of high reversible/dedoping performance, is with a wide range of applications, and is one of the study hotspot in current ultracapacitor field.
The method of conventional synthesis polypyrrole mainly has electrochemical synthesis and chemical synthesis.Compared with the electrochemical method that synthetic quantity is relatively low, chemical synthesis has the advantage that cost is low, yield is high.At present, the ratio electric capacity of pure polypyrrole is generally kept in 200 ~ 400F/g.The polypyrrole that Yang etc. are synthesized by the method for interfacial polymerization, when sweep speed is 25mV/s, 261F/g(Q.Yang is reached than electric capacity, Z.Hou, T.Huang.Self-assembledpolypyrrolefilmbyinterfacialpolyme rizationforsupercapacitorapplications [J] .JournalofAppliedPolymerScience, 2015,132 (11) .).Xu etc. are by polypyrrole and sodium carboxymethyl cellulose compound, under the doping condition of hydrochloric acid, the electrode material of preparation, under the test condition that electric current density is 0.25A/g, it is 184F/g(Y.Xu than electric capacity, Y.Zhang.Synthesisofpolypyrrole/sodiumcarboxymethylcellul osenanosphereswithenhancedsupercapacitorperformance [J] .MaterialsLetters, 2015,139:145-148.).
Therefore adopt preparation process simple, reliable and the method synthesis electric polypyrrole material of environmental protection, for its application in electrochemical energy storage field, there is important and wide significance.Malic acid has good water solublity, and relative to any of the above method, there is wide material sources, the advantage such as cheap, especially there is substantial amounts of carboxyl and hydroxyl in its strand, substantial amounts of hydrogen bond can be formed with pyrroles's molecule, be suitable as the template preparing electric polypyrrole material；Meanwhile, malic acid can as the adulterant of polypyrrole, it is possible to be effectively improved the chemical property of polypyrrole.The present invention using malic acid be template and adulterant, Ammonium persulfate. is as oxidizing initiators, synthesize electric polypyrrole by the method for chemical oxidising polymerisation, it it is a kind of simple and environmental protection preparation method, gained electric polypyrrole material has good chemical property, it is a kind of desirably electrode material for super capacitor, is especially suitable for industrialized production.
Summary of the invention
It is an object of the invention to provide a kind of with malic acid be template and adulterant, method by self-assembling technique and the chemical oxidising polymerisation method of preparing the electric polypyrrole with outstanding chemical property.
Concretely comprise the following steps:
Weigh malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add the pyrroles of 0.5mL, ice-water bath stirs 0.5h, prepare mixed liquor, it is added dropwise over Ammonium persulfate. with in backward mixed liquor, and continue continuous stirring 12h in ice-water bath, finally with deionized water product is washed, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely prepare electric polypyrrole.
The ratio of described malic acid and the amount of substance of pyrroles is 0.25 ~ 4:1；The ratio of described Ammonium persulfate. and the amount of substance of pyrroles is 1:1.
The inventive method has the advantage that
It is simple and environmentally-friendly, reliable that the inventive method has preparation process, and raw material sources are extensive, with low cost, is suitable for industrialized production, and the electric polypyrrole prepared has that resistance is relatively low, higher than electric capacity and the chemical property such as energy density.
The inventive method utilizes the hydroxyl on malic acid molecule and carboxyl and pyrroles's molecule form hydrogen bond and prepare the electric polypyrrole material with outstanding chemical property with malic acid for adulterant, the polypyrrole material of preparation has bigger specific surface area, substantial amounts of reactivity point can be provided for redox reaction, improve the effective rate of utilization of electrode material, thus obtaining the electric polypyrrole material with outstanding chemical property, it it is a kind of desirably electrode material for super capacitor.
Accompanying drawing explanation
Fig. 1 is the electric polypyrrole for preparing of the embodiment of the present invention 1 cyclic voltammogram under different scanning speed.
Fig. 2 is the electric polypyrrole for preparing of the embodiment of the present invention 1 constant current charge-discharge figure under different electric current densities.
Detailed description of the invention
Embodiment 1:
Weigh 3.865g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add the pyrroles of 0.5mL, ice-water bath stirs 0.5h, prepare mixed liquor, it is added dropwise over Ammonium persulfate. with in backward mixed liquor, and continue continuous stirring 12h in ice-water bath, finally with deionized water product is washed, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely prepare electric polypyrrole.
The ratio of described malic acid and the amount of substance of pyrroles is 4:1；The ratio of described Ammonium persulfate. and the amount of substance of pyrroles is 1:1.
Embodiment 2:
Weigh 2.899g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add the pyrroles of 0.5mL, ice-water bath stirs 0.5h, prepare mixed liquor, it is added dropwise over Ammonium persulfate. with in backward mixed liquor, and continue continuous stirring 12h in ice-water bath, finally with deionized water product is washed, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely prepare electric polypyrrole.
The ratio of described malic acid and the amount of substance of pyrroles is 3:1；The ratio of described Ammonium persulfate. and the amount of substance of pyrroles is 1:1.
Embodiment 3:
Weigh 1.933g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add the pyrroles of 0.5mL, ice-water bath stirs 0.5h, prepare mixed liquor, it is added dropwise over Ammonium persulfate. with in backward mixed liquor, and continue continuous stirring 12h in ice-water bath, finally with deionized water product is washed, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely prepare electric polypyrrole.
The ratio of described malic acid and the amount of substance of pyrroles is 2:1；The ratio of described Ammonium persulfate. and the amount of substance of pyrroles is 1:1.
Embodiment 4:
Weigh 0.966g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add the pyrroles of 0.5mL, ice-water bath stirs 0.5h, prepare mixed liquor, it is added dropwise over Ammonium persulfate. with in backward mixed liquor, and continue continuous stirring 12h in ice-water bath, finally with deionized water product is washed, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely prepare electric polypyrrole.
The ratio of described malic acid and the amount of substance of pyrroles is 1:1；The ratio of described Ammonium persulfate. and the amount of substance of pyrroles is 1:1.
Embodiment 5:
Weigh 0.483g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add the pyrroles of 0.5mL, ice-water bath stirs 0.5h, prepare mixed liquor, it is added dropwise over Ammonium persulfate. with in backward mixed liquor, and continue continuous stirring 12h in ice-water bath, finally with deionized water product is washed, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely prepare electric polypyrrole.
The ratio of described malic acid and the amount of substance of pyrroles is 0.5:1；The ratio of described Ammonium persulfate. and the amount of substance of pyrroles is 1:1.
Embodiment 6:
Weigh 0.322g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add the pyrroles of 0.5mL, ice-water bath stirs 0.5h, prepare mixed liquor, it is added dropwise over Ammonium persulfate. with in backward mixed liquor, and continue continuous stirring 12h in ice-water bath, finally with deionized water product is washed, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely prepare electric polypyrrole.
The ratio of described malic acid and the amount of substance of pyrroles is 1:3；The ratio of described Ammonium persulfate. and the amount of substance of pyrroles is 1:1.
Embodiment 7:
Weigh 0.242g malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add the pyrroles of 0.5mL, ice-water bath stirs 0.5h, prepare mixed liquor, it is added dropwise over Ammonium persulfate. with in backward mixed liquor, and continue continuous stirring 12h in ice-water bath, finally with deionized water product is washed, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely prepare electric polypyrrole.
The ratio of described malic acid and the amount of substance of pyrroles is 0.25:1；The ratio of described Ammonium persulfate. and the amount of substance of pyrroles is 1:1.
Claims (1)
1. the method preparing electric polypyrrole for template and adulterant with malic acid, it is characterised in that concretely comprise the following steps:
Weigh malic acid and join in the flask filling 30mL deionized water, after 0.5h is stirred at room temperature, by flask transposition in ice-water bath, then in flask, add the pyrroles of 0.5mL, ice-water bath stirs 0.5h, prepare mixed liquor, it is added dropwise over Ammonium persulfate. with in backward mixed liquor, and continue continuous stirring 12h in ice-water bath, finally with deionized water product is washed, sucking filtration, until filtrate is in neutrality, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, grind and collect, namely prepare electric polypyrrole；
The ratio of described malic acid and the amount of substance of pyrroles is 0.25 ~ 4:1；The ratio of described Ammonium persulfate. and the amount of substance of pyrroles is 1:1.
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| CN201610246116.2A CN105801854A (en) | 2016-04-20 | 2016-04-20 | Method for preparing conducting polypyrrole by using malic acid as template and doping agent |
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| CN201610246116.2A CN105801854A (en) | 2016-04-20 | 2016-04-20 | Method for preparing conducting polypyrrole by using malic acid as template and doping agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106449177A (en) * | 2016-11-24 | 2017-02-22 | 桂林理工大学 | Method for preparing conducting polypyrrole nanotube by using abietic acid as template and dopant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781520A (en) * | 2010-02-08 | 2010-07-21 | 北京航空航天大学 | Water-based conducting polymer/metal composite nano-coating for porous wall board and preparation method thereof |
| CN104064358A (en) * | 2014-06-25 | 2014-09-24 | 福建国光电子科技股份有限公司 | Electrochemical polymerization solution for preparing solid electrolyte layer for solid electrolytic capacitor |
| CN104672447A (en) * | 2015-02-21 | 2015-06-03 | 桂林理工大学 | Preparation method of polypyrrole with high specific capacitance |
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2016
- 2016-04-20 CN CN201610246116.2A patent/CN105801854A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781520A (en) * | 2010-02-08 | 2010-07-21 | 北京航空航天大学 | Water-based conducting polymer/metal composite nano-coating for porous wall board and preparation method thereof |
| CN104064358A (en) * | 2014-06-25 | 2014-09-24 | 福建国光电子科技股份有限公司 | Electrochemical polymerization solution for preparing solid electrolyte layer for solid electrolytic capacitor |
| CN104672447A (en) * | 2015-02-21 | 2015-06-03 | 桂林理工大学 | Preparation method of polypyrrole with high specific capacitance |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106449177A (en) * | 2016-11-24 | 2017-02-22 | 桂林理工大学 | Method for preparing conducting polypyrrole nanotube by using abietic acid as template and dopant |
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Application publication date: 20160727 |