CN103467740B - Take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture - Google Patents
Take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture Download PDFInfo
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- CN103467740B CN103467740B CN201310407756.3A CN201310407756A CN103467740B CN 103467740 B CN103467740 B CN 103467740B CN 201310407756 A CN201310407756 A CN 201310407756A CN 103467740 B CN103467740 B CN 103467740B
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Abstract
The present invention relates to a kind of take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture, comprising: (1) adds deionized water after aniline, beta-cyclodextrin being mixed with citric acid, stirs and obtain mixing solutions; (2) ammonium persulphate is dissolved in deionized water, obtains the ammonium persulfate solution that concentration is 0.4mol/L; (3) in 0-10 DEG C of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, obtains reaction solution, stop after glass stick rapid stirring 1-2min stirring, then standing and reacting 24h; Finally the product obtained is washed, is drying to obtain polyaniline nanotube.Synthesis condition of the present invention is simple, aftertreatment is easy; The aperture controllable of the polyaniline nanotube prepared by the present invention, pore-forming is effective, and at antistatic, anticorrosive coating, electromagnetic shielding material, has good application prospect in the various fields such as solar energy materials.
Description
Technical field
The invention belongs to polyaniline nanotube field, particularly a kind of take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture.
Background technology
Polyaniline is a kind of conducting function polymer.Have that synthesis is easy, cost is low, thermal conductivity good and the advantage such as environmental stability and be used to antistatic, anticorrosive coating, electromagnetic shielding material, the various fields such as solar energy materials.And polyaniline nano material is as low-dimensional materials, the dimensional effect, quantum effect etc. of nano material give its special physical and chemical performance, therefore the synthesis of polyaniline nano material and applied research have caused the great interest of scientific research personnel, have become one of focus of conducting function field of polymer technology.
Some researchs show, the polyaniline nanotube of development aperture controllable is a focus in polyaniline research.
Beta-cyclodextrin is 7 D(+) cyclic oligomer of-glucopyranose composition, its molecule be wide at the top and narrow at the bottom, both ends open, hollow tubular article, and inside, chamber is in relative hydrophobicity, and all hydroxyls are then in molecule outside.
Summary of the invention
It take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture that technical problem to be solved by this invention is to provide a kind of, and the method is simple to operate, and aftertreatment is easy, and the polyaniline nanotube pore-forming of prepared aperture controllable is effective.
Of the present invention a kind of take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture, comprising:
(1) add deionized water after aniline, beta-cyclodextrin being mixed with citric acid, magnetic agitation 0.5h at ambient temperature, obtains mixing solutions;
(2) ammonium persulphate is dissolved in deionized water, obtains the ammonium persulfate solution that concentration is 0.4mol/L;
(3) in 0-10 DEG C of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, obtains reaction solution, stop after glass stick rapid stirring 1-2min stirring, then standing and reacting 24h; Finally the product obtained is washed, is drying to obtain polyaniline nanotube.
The pH value of the mixing solutions that step (1) obtains is 2-6.
In reaction solution described in step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 5: 1: 2: 5.
In reaction solution described in step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 3.75: 0.75: 2: 5.
In reaction solution described in step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 2.5: 0.5: 2: 5.
The speed of the rapid stirring described in step (3) is 200-500rpm.
Washing described in step (3) is for first to use acetone, more colourless to filtrate with deionized water wash.
Drying described in step (3) is at 40-60 DEG C of vacuum-drying 24h.
The ratio that the hole area of the polyaniline nanotube section that step (3) obtains accounts for the total area is 11.8%, 33.5% and 36.5%.
Polyaniline nanotube of the present invention is soft template with beta-cyclodextrin, and aniline concentration changed in proportion and beta-cyclodextrin be ultrasonic mixing in citric acid solution, and aniline is attached in cyclodextrin internal chamber wall and outer chamber wall as far as possible.Under 0-10 DEG C of condition, obtain with ammonium persulphate oxypolymerization.
Of the present invention is the technology of the regulatable polyaniline nanotube of a kind of easy synthetic aperture.The mode that the present invention adopts aniline and beta-cyclodextrin concentration to decline in proportion obtains the polyaniline nanotube of corresponding different pore size size.
The present invention's citric acid amount used is dopant acid, and it act as and controls solution ph is 2-6.
The section of three kinds of polyaniline nanotubes of the present invention, the ratio that hole area accounts for the total area is respectively 11.8%, 33.5% and 36.5%.Reduction monomer and template concentrations are conducive in hole.
Beneficial effect:
(1) synthesis condition of the present invention is simple, aftertreatment is easy;
(2) aperture controllable of the polyaniline nanotube prepared by the present invention, pore-forming is effective, and at antistatic, anticorrosive coating, electromagnetic shielding material, has good application prospect in the various fields such as solar energy materials.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the polyaniline nanotube that embodiment 1 obtains;
Fig. 2 is the SEM figure of the polyaniline nanotube that embodiment 2 obtains;
Fig. 3 is the SEM figure of the polyaniline nanotube that embodiment 3 obtains;
Fig. 4 is the scale map that the hole area of embodiment 1,2 and 3 gained polyaniline nanotube accounts for total cross-section.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) add deionized water after aniline and beta-cyclodextrin being mixed with citric acid, magnetic agitation 0.5h at ambient temperature, obtains mixing solutions; The pH value of described mixing solutions is 2-6;
(2) ammonium persulphate is dissolved in deionized water, obtains the ammonium persulfate solution that concentration is 0.4mol/L;
(3) in 0-10 DEG C of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, stop after glass stick rapid stirring 1-2min stirring, then standing and reacting 24h; Finally the product obtained is washed (first use acetone, more colourless to filtrate with deionized water wash), dry (at 40-60 DEG C of vacuum-drying 24h) namely obtains polyaniline nanotube.
In system described in step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 5: 1: 2: 5.
The ratio that the hole area of the polyaniline nanotube section that step (3) obtains accounts for the total area is 11.8%.
Embodiment 2
(1) add deionized water after aniline and beta-cyclodextrin being mixed with citric acid, magnetic agitation 0.5h at ambient temperature, obtains mixing solutions; The pH value of described mixing solutions is 2-6;
(2) ammonium persulphate is dissolved in deionized water, obtains the ammonium persulfate solution that concentration is 0.4mol/L;
(3) in 0-10 DEG C of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, stop after glass stick rapid stirring 1-2min stirring, then standing and reacting 24h; Finally the product obtained is washed (first use acetone, more colourless to filtrate with deionized water wash), dry (at 40-60 DEG C of vacuum-drying 24h) namely obtains polyaniline nanotube.
In system described in step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 3.75: 0.75: 2: 5.
The ratio that the hole area of the polyaniline nanotube section that step (3) obtains accounts for the total area is 33.5%.
Embodiment 3
(1) add deionized water after aniline and beta-cyclodextrin being mixed with citric acid, magnetic agitation 0.5h at ambient temperature, obtains mixing solutions; The pH value of described mixing solutions is 2-6;
(2) ammonium persulphate is dissolved in deionized water, obtains the ammonium persulfate solution that concentration is 0.4mol/L;
(3) in 0-10 DEG C of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, stop after glass stick rapid stirring 1-2min stirring, then standing and reacting 24h; Finally the product obtained is washed (first use acetone, more colourless to filtrate with deionized water wash), dry (at 40-60 DEG C of vacuum-drying 24h) namely obtains polyaniline nanotube.
In system described in step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 2.5: 0.5: 2: 5.
The ratio that the hole area of the polyaniline nanotube section that step (3) obtains accounts for the total area is 36.5%.
Claims (6)
1. be a method for the controlled polyaniline nanotube in Template preparation aperture with beta-cyclodextrin, comprise:
(1) add deionized water after aniline, beta-cyclodextrin being mixed with citric acid, magnetic agitation 0.5h at ambient temperature, obtains mixing solutions;
(2) ammonium persulphate is dissolved in deionized water, obtains the ammonium persulfate solution that concentration is 0.4mol/L;
(3) in 0-10 DEG C of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, obtains reaction solution, stop after glass stick rapid stirring 1-2min stirring, then standing and reacting 24h; Finally the product obtained is washed, is drying to obtain polyaniline nanotube; Wherein in reaction solution the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate be 5: 1: 2: 5 or reaction solution in the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate be 3.75: 0.75: 2: 5 or reaction solution in the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate be 2.5: 0.5: 2: 5.
2. according to claim 1 a kind of take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture, it is characterized in that: the pH value of the mixing solutions that step (1) obtains is 2-6.
3. according to claim 1 a kind of take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture, it is characterized in that: the speed of the rapid stirring described in step (3) is 200-500rpm.
4. according to claim 1 a kind of take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture, it is characterized in that: the washing described in step (3) is for first to use acetone, more colourless to filtrate with deionized water wash.
5. according to claim 1 a kind of take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture, it is characterized in that: the drying described in step (3) is at 40-60 DEG C of vacuum-drying 24h.
6. according to claim 1 a kind of take beta-cyclodextrin as the method for the controlled polyaniline nanotube in Template preparation aperture, it is characterized in that: the ratio that the hole area of the polyaniline nanotube section that step (3) obtains accounts for the total area is followed successively by 11.8%, 33.5% and 36.5%.
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| CN103936983B (en) * | 2014-04-10 | 2017-06-06 | 东华大学 | A kind of method that application PLA regulation and control prepare polyaniline micro/nano structure |
| CN104371138B (en) * | 2014-11-13 | 2017-10-10 | 吉林大学 | A kind of preparation method of the adjustable polyarylether class microporous barrier in aperture |
| CN105037717A (en) * | 2015-08-27 | 2015-11-11 | 桂林理工大学 | Method for preparing conductive polyaniline nanotube by taking glucose as template |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850880A (en) * | 2006-05-26 | 2006-10-25 | 华东理工大学 | Method for preparing self-dispersion nano-level conducting polyaniline |
| CN101125895A (en) * | 2007-07-16 | 2008-02-20 | 南开大学 | Full-methylated cyclodextrinaniline nano supermolecule conducting polymer and its preparation method and use |
| CN103242524A (en) * | 2013-05-16 | 2013-08-14 | 东华大学 | Method of preparing polyaniline nanotube by utilizing cyclodextrin as template |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850880A (en) * | 2006-05-26 | 2006-10-25 | 华东理工大学 | Method for preparing self-dispersion nano-level conducting polyaniline |
| CN101125895A (en) * | 2007-07-16 | 2008-02-20 | 南开大学 | Full-methylated cyclodextrinaniline nano supermolecule conducting polymer and its preparation method and use |
| CN103242524A (en) * | 2013-05-16 | 2013-08-14 | 东华大学 | Method of preparing polyaniline nanotube by utilizing cyclodextrin as template |
Non-Patent Citations (1)
| Title |
|---|
| Chemical oxidative polymerization of β-cyclodextrin/aniline inclusion complex;MIRCEA GRIGORAS,et al;《Journal of Inclusion Phenomena and Macrocyclic Chemistry》;Springer;20060201;第54卷(第1-2期);第101-107页 * |
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