CN110105549A - A kind of MnO2Load the synthetic method of poly- 3- alkylthrophene - Google Patents
A kind of MnO2Load the synthetic method of poly- 3- alkylthrophene Download PDFInfo
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- CN110105549A CN110105549A CN201910379129.0A CN201910379129A CN110105549A CN 110105549 A CN110105549 A CN 110105549A CN 201910379129 A CN201910379129 A CN 201910379129A CN 110105549 A CN110105549 A CN 110105549A
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- alkylthrophene
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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
- C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G61/12—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule
- C08G61/122—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides
- C08G61/123—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds
- C08G61/126—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds with a five-membered ring containing one sulfur atom in the ring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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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- 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
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/10—Definition of the polymer structure
- C08G2261/11—Homopolymers
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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
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
- C08G2261/32—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain
- C08G2261/322—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed
- C08G2261/3223—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed containing one or more sulfur atoms as the only heteroatom, e.g. thiophene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2262—Oxides; Hydroxides of metals of manganese
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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
The present invention provides a kind of MnO2Load the synthetic method of poly- 3- alkylthrophene, which comprises the following steps: 3- alkylthrophene monomer is added in deionized water, KI and MnI is added2, it is stirred by ultrasonic and forms emulsion；Ferric chloride aqueous solutions are slowly added in first part of solution, are persistently stirred in adition process, room temperature~50 DEG C are precipitated after standing reaction 12~24 hours, dry to obtain MnO through filtration washing2Load poly- 3- alkylthrophene powder.All raw materials of the present invention are common cheap chemicals, and using friendly process one-step synthesis, situ study synthesizes MnO under room temperature2Load I2Poly- 3- alkylthrophene is adulterated, is uniformly dispersed, the structure and morphology of material, which controls, to be stablized, and can be used for the electrode material of supercapacitor.
Description
Technical field
The invention belongs to material chemistry technical fields, are related to a kind of MnO2Load the synthetic method of poly- 3- alkylthrophene.
Background technique
Polythiophene is a kind of typical conjugated conductive high molecular material, can be used for electrochromism, secondary cell, electrochemical capacitance etc.
Field.By replacing to alkyl on the position thiphene ring 3-, the stability of derivative is enhanced, can be with for super capacitor material
Obtain preferable cycle performance.The poly- 3- alkylthrophene conductivity of eigenstate is very low, leads to lower specific capacity and power capacity, leads to
Conductivity can significantly be promoted by crossing I2 doping.In chemical capacitor the performance of conductive polymer electrodes can by with metal oxygen
The mode of compound nano-particles reinforcement is improved.Manganese oxide has cheap, naturally environmentally friendly, the advantages such as specific capacitance height.It is existing
There is the nano-particle modified polymer material of technology synthesis oxide to realize usually using two-step method: i.e. first synthesis oxide nanometer
Particle, then oxide nano particles are dispersed in in-situ polymerization in polymer monomer.One-step synthesis method MnO2It is poly- to load I2 doping
3- alkylthrophene and realize technique currently without report.
Summary of the invention
The purpose of the present invention is to provide a kind of MnO2Load the synthetic method of poly- 3- alkylthrophene, which is characterized in that packet
It includes following steps: 3- alkylthrophene monomer is added in deionized water, KI and MnI is added2, it is stirred by ultrasonic and forms emulsion；It will
Ferric chloride aqueous solutions are slowly added in first part of solution, are persistently stirred in adition process, and room temperature~50 DEG C standing reaction 12~
It is precipitated after 24 hours, dries to obtain MnO through filtration washing2Load poly- 3- alkylthrophene powder.
The 3- alkylthrophene include 3 methyl thiophene, 3- ethylthiophene, 3- hexyl thiophene, in 3- dodecylthiophene
One kind, concentration of the monomer in reaction solution are 0.05~0.1mol/L.
Concentration of the potassium iodide in reaction solution is 10~20gL-1, MnI2Concentration in reaction solution is 1~
5gL-1。
Ferric trichloride concentration in reaction solution is 0.8~1mol/L.
The washing is alternately washed with deionized water and ethyl alcohol, is used centrifuge to precipitate or filter each time after washing and is set
Standby to be filtered, filtration product is dispersed in deionized water or ethyl alcohol again, and repeated filtration is 7 until filtrate pH value, last
It is secondary to use ethanol washing with convenient and dry；The drying is dried in 50~80 DEG C of vacuum drying ovens, and vacuum drying condition is true
Reciprocal of duty cycle < 133Pa.
All raw materials of the present invention are common cheap chemicals, using friendly process one-step synthesis, a step in situ under room temperature
Method synthesizes MnO2Load I2Poly- 3- alkylthrophene is adulterated, is uniformly dispersed, the structure and morphology of material, which controls, to be stablized, and can be used for super electricity
The electrode material of container.
The contents of the present invention and feature have revealed that as above, however the present invention that describes of front only briefly or pertains only to this
The specific part of invention, feature of the invention may be more than what content disclosed herein was related to.Therefore, protection model of the invention
The revealed content of embodiment should be not limited to by enclosing, and should include the combination of all the elements embodied in different piece, with
And it is various without departing substantially from replacement and modification of the invention, and covered by claims of the present invention.
Detailed description of the invention
Fig. 1 is to synthesize MnO using (embodiment 1) of the invention2The scanning electron microscope for loading poly- 3- alkylthrophene micromorphology is shone
Piece.
Specific embodiment
Embodiment 1
The 3 methyl thiophene monomer of 0.1mol/L is added in 50mL deionized water, 20gL is added-1KI and 2gL-1MnI2, surpass
Sound stirs to form emulsion；50mL 1.6mol/L ferric chloride aqueous solutions are slowly added in first part of solution, in adition process
Lasting stirring, is precipitated after being stored at room temperature reaction 12 hours, dries to obtain MnO as shown in Figure 1 through filtration washing2Load is poly-
3- alkylthrophene powder.Using the powder of preparation use PVDF as adhesive coated on a pet film, then uniformly coating one layer of PVA/
H3PO4Gel electrolyte is cut into the identical 2 5cm × 8cm sheet materials of size, respectively as positive and negative electrode, above two electrodes
Electrolyte when being in leather hard, 2 electrodes faces are sticked together, drying obtains all solid state symmetric form super capacitor
Device, specific capacity 431Fg-1。
Embodiment 2
The 3- hexyl thiophene monomer of 0.2mol/L is added in 50mL deionized water, 40gL is added-1KI and 10gL-1MnI2,
Ultrasonic agitation forms emulsion；50mL 2mol/L ferric chloride aqueous solutions are slowly added in first part of solution, in adition process
Lasting stirring, 50 DEG C of standings are precipitated after reacting 12 hours, dry to obtain MnO through filtration washing2Load poly- 3- alkylthrophene
Powder.Using the powder of preparation use PVDF as adhesive coated on a pet film, then uniformly coating one layer of PVA/H3PO4Gel electrolyte
Matter is cut into the identical 2 5cm × 8cm sheet materials of size and is in respectively as positive and negative electrode to the electrolyte above two electrodes
When leather hard, 2 electrodes faces are sticked together, drying obtains all solid state symmetric form supercapacitor, and specific capacity is
420Fg-1。
Embodiment 3
The 3- dodecylthiophene monomer of 0.1mol/L is added in 50mL deionized water, 30gL is added-1KI and 5gL- 1MnI2, it is stirred by ultrasonic and forms emulsion；50mL 1.8mol/L ferric chloride aqueous solutions are slowly added in first part of solution, are added
Lasting stirring, is precipitated after being stored at room temperature reaction 24 hours, dries to obtain MnO through filtration washing during entering2Load poly- 3-
Alkylthrophene powder.Using the powder of preparation use PVDF as adhesive coated on a pet film, then uniformly coating one layer of PVA/H3PO4
Gel electrolyte is cut into the identical 2 5cm × 8cm sheet materials of size, respectively as positive and negative electrode, to the electricity above two electrodes
When solution matter is in leather hard, 2 electrodes faces are sticked together, drying obtains all solid state symmetric form supercapacitor, than
Capacity is 479Fg-1。
Claims (6)
1. a kind of MnO2Load the synthetic method of poly- 3- alkylthrophene, which comprises the following steps: by 3- alkylthrophene
Monomer is added in deionized water, and KI and MnI is added2, it is stirred by ultrasonic and forms emulsion；Ferric chloride aqueous solutions are slowly added to
It in a solution, is persistently stirred in adition process, room temperature~50 DEG C are precipitated after standing reaction 12~24 hours, by diafiltration
It washs drying and obtains MnO2Load poly- 3- alkylthrophene powder.
2. a kind of MnO according to claim 12Load the synthetic method of poly- 3- alkylthrophene, it is characterised in that: the 3- alkane
Base thiophene includes one of 3 methyl thiophene, 3- ethylthiophene, 3- hexyl thiophene, 3- dodecylthiophene, and monomer is reacting
Concentration in solution is 0.05~0.1mol/L.
3. a kind of MnO according to claim 12Load the synthetic method of poly- 3- alkylthrophene, it is characterised in that: the iodate
Concentration of the potassium in reaction solution is 10~20gL-1, MnI2Concentration in reaction solution is 1~5gL-1。
4. a kind of MnO according to claim 12Load the synthetic method of poly- 3- alkylthrophene, it is characterised in that: the trichlorine
Changing iron concentration in reaction solution is 0.8~1mol/L.
5. a kind of MnO according to claim 12Load the synthetic method of poly- 3- alkylthrophene, it is characterised in that: described washes
Washing alternately is washed with deionized water and ethyl alcohol, is filtered, is filtered using centrifuge precipitating or pumping and filtering device each time after washing
Product disperses in deionized water or ethyl alcohol again, and repeated filtration is 7 until filtrate pH value, for the last time with ethanol washing with side
Just it dries；The drying is dried in 50~80 DEG C of vacuum drying ovens, and vacuum drying condition is vacuum degree < 133Pa.
6. a kind of MnO as claimed in any one of claims 1 to 5, wherein2Prepared by the synthetic method for loading poly- 3- alkylthrophene
MnO2Load poly- 3- alkylthrophene.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910379129.0A CN110105549A (en) | 2019-04-23 | 2019-04-23 | A kind of MnO2Load the synthetic method of poly- 3- alkylthrophene |
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| CN201910379129.0A CN110105549A (en) | 2019-04-23 | 2019-04-23 | A kind of MnO2Load the synthetic method of poly- 3- alkylthrophene |
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| CN201910379129.0A Withdrawn CN110105549A (en) | 2019-04-23 | 2019-04-23 | A kind of MnO2Load the synthetic method of poly- 3- alkylthrophene |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070109940A (en) * | 2006-05-12 | 2007-11-15 | 주식회사 엘지화학 | Highly electron conductive polymer and electrochemical energy storgage device with high capacity and high power using the same |
| CN102453309A (en) * | 2010-10-26 | 2012-05-16 | 南开大学 | Preparation and application of organic/inorganic composite gas sensing material for NO2 detection at room temperature |
| US9922775B2 (en) * | 2015-10-13 | 2018-03-20 | Nanotek Instruments, Inc. | Continuous process for producing electrodes for supercapacitors having high energy densities |
| CN108774320A (en) * | 2018-07-02 | 2018-11-09 | 合肥萃励新材料科技有限公司 | A kind of synthetic method of nickel oxide loaded polyaniline |
| CN108948330A (en) * | 2018-07-05 | 2018-12-07 | 合肥萃励新材料科技有限公司 | A kind of synthetic method aoxidizing tungsten load polythiophene |
| CN109239281A (en) * | 2018-11-08 | 2019-01-18 | 上海萃励电子科技有限公司 | A kind of MnO2Load the synthetic method of poly- fluoroaniline |
-
2019
- 2019-04-23 CN CN201910379129.0A patent/CN110105549A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20070109940A (en) * | 2006-05-12 | 2007-11-15 | 주식회사 엘지화학 | Highly electron conductive polymer and electrochemical energy storgage device with high capacity and high power using the same |
| CN102453309A (en) * | 2010-10-26 | 2012-05-16 | 南开大学 | Preparation and application of organic/inorganic composite gas sensing material for NO2 detection at room temperature |
| US9922775B2 (en) * | 2015-10-13 | 2018-03-20 | Nanotek Instruments, Inc. | Continuous process for producing electrodes for supercapacitors having high energy densities |
| CN108774320A (en) * | 2018-07-02 | 2018-11-09 | 合肥萃励新材料科技有限公司 | A kind of synthetic method of nickel oxide loaded polyaniline |
| CN108948330A (en) * | 2018-07-05 | 2018-12-07 | 合肥萃励新材料科技有限公司 | A kind of synthetic method aoxidizing tungsten load polythiophene |
| CN109239281A (en) * | 2018-11-08 | 2019-01-18 | 上海萃励电子科技有限公司 | A kind of MnO2Load the synthetic method of poly- fluoroaniline |
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