CN101284908A - Polyaniline nano-fibre and method for preparing same - Google Patents
Polyaniline nano-fibre and method for preparing same Download PDFInfo
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- CN101284908A CN101284908A CNA200710300720XA CN200710300720A CN101284908A CN 101284908 A CN101284908 A CN 101284908A CN A200710300720X A CNA200710300720X A CN A200710300720XA CN 200710300720 A CN200710300720 A CN 200710300720A CN 101284908 A CN101284908 A CN 101284908A
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Abstract
The invention relates to a polyaniline nanofiber and a method for making the same. The technique is characterized in that polyethyleneglycol with ether link functional group is taken as a templating agent, a homogeneous system of water and water-solubility organic solvent is taken as a reacting medium, ammonium persulfate is taken as an oxidizer, hydrochloric acid is taken as doping acid; the compositions in mixture ratio are: 0.5 to 10.0g of polyethyleneglycol, 30 to 150 ml of the homogeneous system of water and water-solubility organic solvent and 5 to 20 ml of hydrochloric acid, 2.0 to 20.0g of ammonium persulfate, and 2 to 10 ml of aniline, wherein, the volume content of the water-solubility organic solvent is between 0 and 100 percent. The method for making the polyaniline nanofiber has little environmental pollution, simple technique and high productivity and is easy to produce industrially; the obtained polyaniline nanofiber has good electroconductibility and thermal stability. The polyaniline nanofiber synthesized by the method can be applied to the fields such as an antistatic material, an electromagnetic screen material, a sensor, a secondary battery, a camouflage material, an anti-rot material and a nano functional device.
Description
Technical field
The present invention relates to a kind of polyaniline nano fiber and preparation method thereof, with the polyoxyethylene glycol that contains ehter bond functional group is that template, hydrochloric acid are that the homogeneous system that doping agent, water and water-miscible organic solvent are formed is a reaction medium, utilizes chemical oxidization method to prepare by series of steps.
Background technology
Polyaniline one dimension Nano structure such as nano wire, nanotube, nanometer rod and nanofiber etc. have and are different from the random particulate performance of common polyaniline, are playing the part of important role at aspects such as making the nano functional device.When the characteristic dimension of material reaches nano-scale, noticeable change will take place with respect to bulk material in its performance.In recent years, the researchist is obtaining bigger progress aspect the preparation of polyaniline nano fiber, but the preparation of the controlled polyaniline nano fiber of size, pattern and performance remains and realizes their key in application technically.
The method that is used to prepare polyaniline nano fiber at present mainly is methods such as template, self-assembly method, interfacial polymerization, the following problem of these method ubiquities: the template that (1) aniline polymerization finishes to be adopted the back is difficult for removing; (2) problem of environmental pollution of oil phase organic solvent in the reaction medium; (3) production cost height; Problem such as (4) the pattern parameter of polyaniline nano fiber is restive.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes a kind of polyaniline nano fiber and preparation method thereof, with the polyoxyethylene glycol that contains ehter bond functional group is that the homogeneous system that template, water and water-miscible organic solvent are formed is a reaction medium, is that dopant acid prepares polyaniline nano fiber with hydrochloric acid by chemical oxidization method.
Technical scheme
Technical characterictic of the present invention is: be template, be that reaction medium, ammonium persulphate are that oxygenant, hydrochloric acid are dopant acid with the homogeneous system of water and water-miscible organic solvent with the polyoxyethylene glycol that contains ehter bond functional group; The ratio of each component is: polyoxyethylene glycol 0.5～10.0g; Homogeneous system 30～150ml that water and water-miscible organic solvent are formed, wherein the volume content of water-miscible organic solvent is 0～100%; Hydrochloric acid 5～20ml; Ammonium persulphate 2.0～20.0g; Aniline 2～10ml.
Described polyoxyethylene glycol number-average molecular weight is 500～30000.
Described water-miscible organic solvent is the organic solvent that alcohols, ketone can form homogeneous system with water.
A kind of preparation method who prepares polyaniline nano fiber is characterized in that preparation process is as follows:
(1) 0.5～10.0g polyoxyethylene glycol is dissolved in the homogeneous system of 30～100ml water and water-miscible organic solvent composition;
(2) under agitation condition, hydrochloric acid 5～20ml is dissolved in the above-mentioned homogeneous system and forms hydrochloric acid soln;
(3) under agitation condition, add 2～10ml aniline and form component A;
(4) 2.0～20.0g oxygenant ammonium persulphate is dissolved in the homogeneous system that 20～50ml water and water-miscible organic solvent form and forms component B;
(5) under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 0.01～5.0ml/min; After dropwising, continue reaction 1～24 hour, temperature of reaction is controlled between 0 ℃～5 ℃;
(6) will use methyl alcohol, acetone and deionized water wash colourless respectively after the reaction product filtration to filtrate;
(7) carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5～4.0M, and the adulterated time is 0～48 hour;
(8) the washing final vacuum is drying to obtain polyaniline nano fiber, and the vacuum tightness during vacuum-drying is 0.1～0.9MPa, and the exsiccant temperature is 30～100 ℃.
Beneficial effect
The characteristics of polyaniline nano fiber of the present invention's development and preparation method thereof are: it is template that (1) the present invention adopts the polyoxyethylene glycol that contains the ehter bond structure of functional groups, to make aniline be template with the peg molecule in polymerization process by dropwise dripping ammonium persulfate solution, assembles in the mode of nanofiber to exist.With water-soluble polyoxyethylene glycol is that template helps after reaction finishes peg molecule being removed; (2) homogeneous system that forms with water and water-miscible organic solvent is reaction medium, has avoided the problem of environmental pollution of oil phase organic solvent in interfacial polymerization and the letex polymerization; (3) water-miscible organic solvent also is the good solvent of many polymkeric substance, and this just provides new research thinking for preparation polyaniline nano fiber conducing composite material, has bigger practical value.The homogeneous system that is template with the polyoxyethylene glycol, forms with water and water-miscible organic solvent is that the stereoscan photograph (SEM) of polyaniline nano fiber of reaction medium preparation and x-ray diffraction pattern (XRD) are as Fig. 1, Fig. 2, shown in Figure 3; The thermogravimetic analysis (TGA) (TGA) of the polyaniline of employing different methods preparation as shown in Figure 4.
Description of drawings
Fig. 1: with the polyoxyethylene glycol is that template, water are the stereoscan photograph (SEM) and the x-ray diffraction pattern (XRD) of the polyaniline nano fiber of reaction medium preparation.
Fig. 2: with the polyoxyethylene glycol is that the homogeneous system that template, water and water-miscible organic solvent form is the stereoscan photograph (SEM) and the x-ray diffraction pattern (XRD) of the polyaniline nano fiber of reaction medium preparation.
Fig. 3: with the polyoxyethylene glycol is that template, water-miscible organic solvent are the stereoscan photograph (SEM) and the x-ray diffraction pattern (XRD) of the polyaniline nano fiber of reaction medium preparation.
Fig. 4: the polyaniline thermogravimetic analysis (TGA) figure (TGA) of different methods preparation, wherein (a) no template, water are reaction medium; (b) be that template, water are reaction medium with the polyoxyethylene glycol; (c) be that the homogeneous system that template, water and water-miscible organic solvent form is a reaction medium with the polyoxyethylene glycol; (d) be that template, water-miscible organic solvent are reaction medium with the polyoxyethylene glycol.
Embodiment
Now in conjunction with the accompanying drawings the present invention is further described:
Embodiment 1:
(1) the 0.5g polyoxyethylene glycol is dissolved in the 30ml water;
(2) under agitation condition with the 5ml dissolving with hydrochloric acid in above-mentioned solution;
(3) under agitation condition, add 2ml aniline and form component A;
(4) the 2.0g ammonium persulphate is dissolved in formation component B in the 20ml water;
(5) under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 0.01ml/min, after dropwising, continues reaction 10 hours, and temperature of reaction is controlled between 3 ℃;
(6) will use methyl alcohol, acetone and deionized water wash colourless respectively after the reaction product filtration to filtrate;
(7) carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5～4.0M, and the adulterated time is 10 hours;
(8) the washing final vacuum is drying to obtain polyaniline nano fiber, and the vacuum tightness during vacuum-drying is 0.1～0.9MPa, and the exsiccant temperature is 30 ℃.
Embodiment 2:
(1) water and 1: 1 by volume mixed of water-miscible organic solvent are formed the homogeneous system of 100ml;
(2) the 10.0g polyoxyethylene glycol is dissolved in the above-mentioned system;
(3) under stirring condition with the 20ml dissolving with hydrochloric acid in above-mentioned solution;
(4) under agitation condition, add 10ml aniline and form component A;
(5) the 20.0g ammonium persulphate is dissolved in the 50ml homogeneous system that water and 1: 1 by volume mixed of water-miscible organic solvent generate and forms component B;
(6) under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 5.0ml/min; After dropwising, continue reaction 24 hours, temperature of reaction is controlled between 5 ℃;
(7) will use methyl alcohol, acetone and deionized water wash colourless respectively after the reaction product filtration to filtrate;
(8) carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5～4.0M, and the adulterated time is 48 hours;
(9) the washing final vacuum is drying to obtain polyaniline nano fiber, and the vacuum tightness during vacuum-drying is 0.1～0.9MPa, and the exsiccant temperature is 100 ℃.
Embodiment 3:
(1) the 5.0g polyoxyethylene glycol is dissolved in the 60ml water-miscible organic solvent;
(2) under stirring condition with the 12ml dissolving with hydrochloric acid in above-mentioned solution;
(3) under agitation condition, add 5ml aniline and form component A;
(4) the 10.0g ammonium persulphate is dissolved in formation component B in the 400ml water-miscible organic solvent;
(5) under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 0.01～5.0ml/min; After dropwising, continue reaction 1～24 hour, temperature of reaction is controlled between 0 ℃～5 ℃;
(6) will use methyl alcohol, acetone and deionized water wash colourless respectively after the reaction product filtration to filtrate;
(7) carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5～4.0M, and the adulterated time is 0～48 hour;
(8) the washing final vacuum is drying to obtain polyaniline nano fiber, and the vacuum tightness during vacuum-drying is 0.1～0.9MPa, and the exsiccant temperature is 30～100 ℃.
The present invention is a template with the polyoxyethylene glycol that contains ehter bond functional group, the homogeneous system that water and water-miscible organic solvent are formed is a reaction medium, by chemical oxidization method is that dopant acid prepares polyaniline nano fiber with hydrochloric acid, so both helped utilizing ehter bond functional group the synthesizing in the polyoxyethylene glycol as the template-directed polyaniline nano fiber, and to adopt water and water-miscible organic solvent be reaction system, avoided the problem of environmental pollution of oil phase organic solvent in interfacial polymerization and the letex polymerization, water-miscible organic solvent also is the good solvent of many polymkeric substance in addition, this just provides new research thinking for preparation polyaniline nano fiber conducing composite material, has bigger practical value.By the homogeneous system that is template with the polyoxyethylene glycol, forms with water and water-miscible organic solvent provided by the invention is reaction medium synthetic polyaniline nano fiber, and its pattern parameter can be controlled by change template agent, the volume content of water-miscible organic solvent, the reaction parameters such as concentration, reaction times and temperature of reaction of dopant acid.
Claims (4)
1. polyaniline nano fiber is characterized in that: be template, be that reaction medium, ammonium persulphate are that oxygenant, hydrochloric acid are dopant acid with the homogeneous system of water and water-miscible organic solvent with the polyoxyethylene glycol that contains ehter bond functional group; The ratio of each component is: polyoxyethylene glycol 0.5～10.0g; Homogeneous system 30～150ml that water and water-miscible organic solvent are formed, wherein the volume content of water-miscible organic solvent is 0～100%; Hydrochloric acid 5～20ml; Ammonium persulphate 2.0～20.0g; Aniline 2～10ml.
2. polyaniline nano fiber according to claim 1 is characterized in that: described polyoxyethylene glycol number-average molecular weight is 500～30000.
3. polyaniline nano fiber according to claim 1 is characterized in that: described water-miscible organic solvent is the organic solvent that alcohols, ketone can form homogeneous system with water.
4. preparation method who prepares the described polyaniline nano fiber of claim 1～3 is characterized in that preparation process is as follows:
(1) 0.5～10.0g polyoxyethylene glycol is dissolved in the homogeneous system of 30～100ml water and water-miscible organic solvent composition;
(2) under agitation condition, hydrochloric acid 5～20ml is dissolved in the above-mentioned homogeneous system and forms hydrochloric acid soln;
(3) under agitation condition, add 2～10ml aniline and form component A;
(4) 2.0～20.0g oxygenant ammonium persulphate is dissolved in the homogeneous system that 20～50ml water and water-miscible organic solvent form and forms component B;
(5) under agitation condition component B dropwise is added drop-wise among the component A continuously, rate of addition is 0.01～5.0ml/min; After dropwising, continue reaction 1～24 hour, temperature of reaction is controlled between 0 ℃～5 ℃;
(6) will use methyl alcohol, acetone and deionized water wash colourless respectively after the reaction product filtration to filtrate;
(7) carry out secondary doping with aqueous hydrochloric acid, the concentration of hydrochloric acid that secondary doping is used is 0.5～4.0M, and the adulterated time is 0～48 hour;
(8) the washing final vacuum is drying to obtain polyaniline nano fiber, and the vacuum tightness during vacuum-drying is 0.1～0.9MPa, and the exsiccant temperature is 30～100 ℃.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212210A (en) * | 2011-04-29 | 2011-10-12 | 南京理工大学 | Method for preparing polyaniline-coated bacteria cellulose nano conductive composite by in-situ polymerization |
| CN102243203A (en) * | 2011-06-13 | 2011-11-16 | 暨南大学 | Anti-oxidation sensor and preparation method hereof |
| CN102702920A (en) * | 2012-06-12 | 2012-10-03 | 中国科学院长春应用化学研究所 | Aqueous polyaniline anti-corrosive paint and preparation method thereof |
| CN103819667A (en) * | 2014-03-07 | 2014-05-28 | 青岛科技大学 | Method for preparing secondarily-doped polyaniline nanofiber material through total liquid phase method |
-
2007
- 2007-12-21 CN CNA200710300720XA patent/CN101284908A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212210A (en) * | 2011-04-29 | 2011-10-12 | 南京理工大学 | Method for preparing polyaniline-coated bacteria cellulose nano conductive composite by in-situ polymerization |
| CN102212210B (en) * | 2011-04-29 | 2014-06-11 | 南京理工大学 | Method for preparing polyaniline-coated bacteria cellulose nano conductive composite by in-situ polymerization |
| CN102243203A (en) * | 2011-06-13 | 2011-11-16 | 暨南大学 | Anti-oxidation sensor and preparation method hereof |
| CN102702920A (en) * | 2012-06-12 | 2012-10-03 | 中国科学院长春应用化学研究所 | Aqueous polyaniline anti-corrosive paint and preparation method thereof |
| CN102702920B (en) * | 2012-06-12 | 2015-07-22 | 中国科学院长春应用化学研究所 | Aqueous polyaniline anti-corrosive paint and preparation method thereof |
| CN103819667A (en) * | 2014-03-07 | 2014-05-28 | 青岛科技大学 | Method for preparing secondarily-doped polyaniline nanofiber material through total liquid phase method |
| CN103819667B (en) * | 2014-03-07 | 2017-01-18 | 青岛科技大学 | Method for preparing secondarily-doped polyaniline nanofiber material through total liquid phase method |
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