CN101928459A - Method for preparing magnetic nanometer polypyrrole material - Google Patents
Method for preparing magnetic nanometer polypyrrole material Download PDFInfo
- Publication number
- CN101928459A CN101928459A CN2010102733899A CN201010273389A CN101928459A CN 101928459 A CN101928459 A CN 101928459A CN 2010102733899 A CN2010102733899 A CN 2010102733899A CN 201010273389 A CN201010273389 A CN 201010273389A CN 101928459 A CN101928459 A CN 101928459A
- Authority
- CN
- China
- Prior art keywords
- polypyrrole
- ionic liquid
- electrode
- magnetic nanometer
- synthesizing magnetic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
Abstract
The invention discloses a method for preparing a magnetic conductive polymer polypyrrole nanometer material, and in particular relates to a chemical polymerization or an electrochemical polymerization method for synthesizing the magnetic polypyrrole nanometer material by using ferric tetrachloride (BMIM[FeCl4]) of ionic liquid 1-butyl-3methylimidazole as an oxidant and a doping agent. The method has the advantages of no need of expensive instrument, simpleness and practicability.
Description
Technical field
The present invention relates to a kind of method for preparing magnetic conductive polyphosphazene polymer pyrroles nano material, be specifically related to titanium tetrachloride salt (BMIM[FeCl with ionic liquid 1-butyl-3 Methylimidazole
4]) as oxygenant and doping agent, utilize the method synthesizing magnetic polypyrrole nano material of chemical polymerization or electrochemical polymerization.
Background technology
Conductive polymers (Conducting Polymers, CPs) have special structure and good light, electronics, chemical property, having important use at aspects such as the energy, information storage, opto-electronic device, transmitter, military stealthy techniquies, is irreplaceable emerging functional materials.As the most common a kind of in the conducting polymer, polypyrrole is various with its synthetic method, building-up reactions simple, manufacturing cost is cheap relatively, conductivity range is big etc., and advantage receives much concern, and has broad application prospects.
In order further to increase the new and more applications approach of conducting polymer, the new character of conducting polymer constantly is developed and studies.If can give conducting polymer composite, then be expected to develop its application, thereby the research of the magnetic property of conducting polymer composite has caused investigator's very big interest at aspects such as electromagnetic shielding material, electromagnetic absorption agent with magnetic property.
In the high molecular preparation method of magnetic conductive, because the magnetic of conducting polymer/inorganic, metal oxide often derives from inorganic materials wherein, therefore, the investigator concentrates one's gaze on sight by doping techniques and prepares on the high molecular method of magnetic conductive.Formerly in the technology, utilize
Latter's magnetic property [A.Pron has been given in the doping of negatively charged ion in conducting polymer, I.Kulszewica, D.billand, J.Przyluski, J.Chem.Soc.Chem.Commun. (1981) 783//S.R.Vadera, N.Kumar, Frontiers of Polymer Research (Edited byP.N.Prasad, J.K.Nigan) p.443-447, Plenum Press.New York (1991). //M.X.Wan, Suzhen Li, JunchaoLi, Solid State Commun.97 (1996) 527-530. //J.Wang, M.X.Wan, Synth.Met.101 (1999) 846-847. //J.Wang, M.X.Wan, Synth.Met.101 (1999) 848-849], the power of this magnetic property depends on doping level.Yet above-mentioned work is all carried out in water solution system, because
May decompose in aqueous systems, simultaneously, conducting polymer may be because of O in the water or H in water solution system during polymerization
2The O molecule causes the reduction of its performance to the effect of conducting polymer.
Summary of the invention
At above-mentioned situation, the present invention is intended to propose to be rich in a kind of
Non-aqueous system in the method for simple synthesizing magnetic nanometer polypyrrole, be specifically related to titanium tetrachloride (BMIM[FeCl with a kind of magnetic ion liquid 1-butyl-3-Methylimidazole
4]) as oxygenant and doping agent, use chemical oxidization method or electrochemical method synthesizing magnetic polypyrrole nano material, specifically comprise the steps:
According to pyrroles/ion liquid volume ratio smaller or equal to 3.5, measure the titanium tetrachloride (BMIM[FeCl of a certain amount of pyrrole monomer and ionic liquid 1-butyl-3-Methylimidazole
4], after thorough mixing is even, mixing solutions was left standstill chemical polymerization 24 hours in the dark, or a kind of with in Pt disc electrode, glass-carbon electrode (GC) or the conductive glass (ITO) as working electrode, the Pt silk is as counter electrode, the Ag/AgCl silk adopts the potentiodynamic technique polymerization as reference electrode, and the current potential upper limit is not higher than 0.75V
2. in above-mentioned chemistry or the electrochemical polymerization process, temperature should be controlled in 10-60 ℃, is preferably 15-30 ℃.
The method that the present invention adopts need not expensive instrument, and method is simple.
Description of drawings
Fig. 1 uses the scanning electron microscope picture of the polypyrrole material that chemical oxidization method obtains, and inserts figure: the Magnetic Measurement curve of this polypyrrole material
Embodiment
The present invention will be further described below in conjunction with embodiment, but protection scope of the present invention is not limited to this.
Embodiment 1
The pyrrole monomer of measuring 1ml is put in the 10ml beaker, and then to the ionic liquid that wherein adds 3.5ml, slowly is statically placed in the dark behind the stir about 10min, at 25 ℃ of reaction 24h.Question response finishes, and uses the ethanol cleaning and filtering, and dry 36h in 60 ℃ of vacuum drying ovens then obtains the powder of magnetic polypyrrole, and its SEM picture as shown in Figure 1.
Embodiment 2
The pyrrole monomer of measuring 1ml is put in the centrifuge tube of 5ml, measures the ionic liquid of about 3.5ml again, is placed in the three-electrode system electrolyzer after fully rocking 1min.Use the Pt disc electrode as working electrode, the Pt silk is as counter electrode, with Ag/AgCl as reference electrode, potential cycle scanning 2～4 circles at 0.3～0.75V, on the Pt disc electrode, generate the thin polypyrrole layer of one deck, use ethanol to clean back nitrogen and dry up, obtain the film of magnetic polypyrrole.
Embodiment 3
The pyrrole monomer of measuring 1ml is put in the centrifuge tube of 5ml, and the ionic liquid of measuring about 3.5ml again adds, and is placed in the three-electrode system electrolyzer after fully rocking 1min.Use conductive glass (ITO) as working electrode, the Pt silk is as counter electrode, with Ag/AgCl as reference electrode, potential cycle scanning 20～40 circles at 0.3～0.75V, film of poly pyrrole on the conductive glass is stripped in the centrifuge tube, after using ethanol fully to clean, 60 ℃ of dry 36h obtain the magnetic film of poly pyrrole in vacuum drying oven.
Embodiment 4
The pyrrole monomer of measuring 1ml is put in the 10ml beaker, and then to the ionic liquid that wherein adds 7.0ml, slowly is statically placed in the dark behind the stir about 10min, at 15 ℃ of reaction 24h.Question response finishes, and uses the ethanol cleaning and filtering, and dry 36h in 60 ℃ of vacuum drying ovens then obtains the powder of magnetic polypyrrole.
Embodiment 5
The pyrrole monomer of accurately measuring 1ml is put in the 10ml beaker, and then to the ionic liquid that wherein adds 3.5ml, slowly is statically placed in the dark behind the stir about 10min, at 60 ℃ of reaction 24h.Question response finishes, and uses the ethanol cleaning and filtering, and dry 36h in 60 ℃ of vacuum drying ovens then obtains the powder of magnetic polypyrrole.
Claims (4)
1. the method for a simple synthesizing magnetic nanometer polypyrrole is characterized in that: with ionic liquid BMIM[FeCl
4] as oxygenant and doping agent, use chemical polymerization or electrochemical polymerization synthesizing magnetic polypyrrole nanoparticle, it comprises the steps:
(1) accurately measures a certain amount of pyrrole monomer and ionic liquid;
(2) pyrroles and the ionic liquid that mixing step (1) is measured in reaction vessel, and be aided with stirring, treat both thorough mixing after, leave standstill and react 24h in the dark;
(3) pyrroles and the ionic liquid that mixing step (1) is measured in reaction vessel uses electrochemical method to generate the film of polypyrrole;
(4) product to (2), (3) filters or cleans, and dry in vacuum drying oven.
2. the method for a kind of simple synthesizing magnetic nanometer polypyrrole according to claim 1 is characterized in that: pyrrole monomer and ion liquid volume ratio are not more than 1: 3.5.
3. the method for a kind of simple green synthesizing magnetic nanometer polypyrrole according to claim 1 is characterized in that: when step (2) uses chemical oxidization method to synthesize polypyrrole; Temperature should be controlled in 10-60 ℃, is preferably 15-30 ℃.
4. the method for a kind of simple synthesizing magnetic nanometer polypyrrole according to claim 1, it is characterized in that: when step (3) uses electrochemical method to synthesize polypyrrole, working electrode can be Pt disc electrode, glass-carbon electrode (GC) or conductive glass (ITO), counter electrode is the Pt silk, reference electrode is Ag/AgCl, and polymerization potential is not higher than 0.75V.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102733899A CN101928459A (en) | 2010-09-03 | 2010-09-03 | Method for preparing magnetic nanometer polypyrrole material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102733899A CN101928459A (en) | 2010-09-03 | 2010-09-03 | Method for preparing magnetic nanometer polypyrrole material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101928459A true CN101928459A (en) | 2010-12-29 |
Family
ID=43367907
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102733899A Pending CN101928459A (en) | 2010-09-03 | 2010-09-03 | Method for preparing magnetic nanometer polypyrrole material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101928459A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516538A (en) * | 2011-12-15 | 2012-06-27 | 河海大学 | Method for preparing fibrillar meshwork structure conducting polypyrrole film by interfacial polymerization |
| CN104164680A (en) * | 2013-11-04 | 2014-11-26 | 江苏大学 | Substrate support-free conductive polypyrrole film making method |
| CN105038143A (en) * | 2015-07-21 | 2015-11-11 | 菏泽学院 | Film made of nano material and doped with polypyrrole and preparation method of film |
| CN108182984A (en) * | 2018-01-22 | 2018-06-19 | 王旭 | A kind of ion liquid modified Polypyrrole Conducting Materials |
| CN110491892A (en) * | 2019-08-19 | 2019-11-22 | 德淮半导体有限公司 | Imaging sensor and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1995462A (en) * | 2006-01-06 | 2007-07-11 | 浙江工业大学 | Polypyrrole electrolytic synthesis method |
| CN101314639A (en) * | 2008-06-26 | 2008-12-03 | 华东理工大学 | Method for preparing poly-pyrrole with Fe(III) ion liquid as oxygenant |
-
2010
- 2010-09-03 CN CN2010102733899A patent/CN101928459A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1995462A (en) * | 2006-01-06 | 2007-07-11 | 浙江工业大学 | Polypyrrole electrolytic synthesis method |
| CN101314639A (en) * | 2008-06-26 | 2008-12-03 | 华东理工大学 | Method for preparing poly-pyrrole with Fe(III) ion liquid as oxygenant |
Non-Patent Citations (3)
| Title |
|---|
| 《Macromolecules》 20080320 Jin-Yeol Kim et al. Polypyrrole Nanostructures Self-Assembled in Magnetic Ionic Liquid as a Template 第2886-2889页 1-4 第41卷, 第8期 2 * |
| 《江苏技术师范学院学报（自然科学版）》 20080930 朱雯 导电聚合物的电化学聚合研究进展 第43-48页 1,4 第14卷, 第3期 2 * |
| 《高分子通报》 20061231 赵崇军等 离子液体在导电高分子中的应用 第8-12页 1-4 , 第12期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516538A (en) * | 2011-12-15 | 2012-06-27 | 河海大学 | Method for preparing fibrillar meshwork structure conducting polypyrrole film by interfacial polymerization |
| CN102516538B (en) * | 2011-12-15 | 2013-07-31 | 河海大学 | Method for preparing fibrillar meshwork structure conducting polypyrrole film by interfacial polymerization |
| CN104164680A (en) * | 2013-11-04 | 2014-11-26 | 江苏大学 | Substrate support-free conductive polypyrrole film making method |
| CN104164680B (en) * | 2013-11-04 | 2017-07-18 | 江苏大学 | A kind of preparation method of the Conductive Polypyrrole Film without substrate support |
| CN105038143A (en) * | 2015-07-21 | 2015-11-11 | 菏泽学院 | Film made of nano material and doped with polypyrrole and preparation method of film |
| CN105038143B (en) * | 2015-07-21 | 2017-05-24 | 菏泽学院 | Film made of nano material and doped with polypyrrole and preparation method of film |
| CN108182984A (en) * | 2018-01-22 | 2018-06-19 | 王旭 | A kind of ion liquid modified Polypyrrole Conducting Materials |
| CN110491892A (en) * | 2019-08-19 | 2019-11-22 | 德淮半导体有限公司 | Imaging sensor and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US11530331B2 (en) | Functional ink suitable for 3D printing and preparation method thereof | |
| Zhang et al. | Graphene–polypyrrole nanocomposite as a highly efficient and low cost electrically switched ion exchanger for removing ClO4–from wastewater | |
| Gao et al. | General method of manipulating formation, composition, and morphology of solid-electrolyte interphases for stable Li-alloy anodes | |
| Naseri et al. | Novel electroactive nanocomposite of POAP for highly efficient energy storage and electrocatalyst: electrosynthesis and electrochemical performance | |
| Szeifert et al. | Ultrasmall titania nanocrystals and their direct assembly into mesoporous structures showing fast lithium insertion | |
| Qi et al. | Size control of polypyrrole particles | |
| Li et al. | Synthesis of spherical PANI particles via chemical polymerization in ionic liquid for high-performance supercapacitors | |
| Ahmed et al. | An innovative method for preparation of nanometal hydroxide superabsorbent hydrogel | |
| Menon et al. | Investigation of molecular and supermolecular structure in template-synthesized polypyrrole tubules and fibrils | |
| Lu et al. | Water dispersed conducting polyaniline nanofibers for high-capacity rechargeable lithium–oxygen battery | |
| Zhang et al. | Electrochemical performance and surface properties of bare and TiO2-coated cathode materials in lithium-ion batteries | |
| CN101928459A (en) | Method for preparing magnetic nanometer polypyrrole material | |
| Hosseini et al. | Electrochemical behavior of a Nafion‐membrane‐based solid‐state supercapacitor with a graphene oxide—multiwalled carbon nanotube—polypyrrole nanocomposite | |
| Li et al. | NiO/Cu-TCPP hybrid nanosheets as an efficient substrate for supercapacitor and sensing applications | |
| O’Meara et al. | Nickel–salen-type polymer as conducting agent and binder for carbon-free cathodes in lithium-ion batteries | |
| CN102206342A (en) | Electric conduction polymer and synthesis method thereof and electroactive electrode with surface covered with electric conduction polymer | |
| JPWO2011108254A1 (en) | Polymerization solution and production method thereof, transparent film and transparent electrode obtained from this polymerization solution | |
| Olivetti et al. | Sol− gel synthesis of vanadium oxide within a block copolymer matrix | |
| Bendrea et al. | Polythiophene-g-poly (ethylene glycol) graft copolymers for electroactive scaffolds | |
| Chen et al. | Structural and electrochemical study of polypyrrole/ZnO nanocomposites coating on nickel sheet synthesized by electrochemical method | |
| Liao et al. | Synergistic effect of polyaniline-modified Pd/C catalysts on formic acid oxidation in a weak acid medium (NH4) 2SO4 | |
| CN105405671A (en) | Oxidized graphene/pure graphene/polyaniline ternary conductive composite material and preparation method thereof | |
| Krishnan et al. | Nanostructure-dependent electrochemical properties of Nb2O5 for long-life Li-ion batteries | |
| Chen et al. | Ordered conducting polypyrrole doped with sulfopropyl ether of β-cyclodextrin | |
| CN104672447B (en) | A kind of preparation method of high specific capacitance polypyrrole |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20101229 |