CN103467740A - Method of preparing polyaniline nanometer tube with controllable pore diameter by taking beta-cyclodextrin as template - Google Patents
Method of preparing polyaniline nanometer tube with controllable pore diameter by taking beta-cyclodextrin as template Download PDFInfo
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- CN103467740A CN103467740A CN2013104077563A CN201310407756A CN103467740A CN 103467740 A CN103467740 A CN 103467740A CN 2013104077563 A CN2013104077563 A CN 2013104077563A CN 201310407756 A CN201310407756 A CN 201310407756A CN 103467740 A CN103467740 A CN 103467740A
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Abstract
The invention relates to a method of preparing a polyaniline nanometer tube with a controllable pore diameter by taking beta-cyclodextrin as a template. The method comprises the steps of: (1) mixing aniline, the beta-cyclodextrin and citric acid, adding deionized water into a mixture, and mixing to obtain a mixed solution; (2) dissolving ammonium persulfate in the deionized water to obtain an ammonium persulfate solution with the concentration of 0.4 mol/L; and (3) in thermostatic waterbath with the temperature of 0-10 DEG C, rapidly pouring the ammonium persulfate solution into the mixed solution to obtain a reaction solution, rapidly mixing for 1-2 minutes by virtue of a glass rod, then carrying out reaction under the stationary condition for 24 hours, and finally, washing and drying an obtained product to obtain the polyaniline nanometer tube. With the adoption of the method, the synthesis conditions are simple, the aftertreatment is easy, the pore diameter of the polyaniline nanometer tube is controllable, pore formation is effective, and the polyaniline nanometer tube has good application prospect in numerous fields of the antistatic field, the anticorrosive paint field, the electromagnetic shielding material field, the solar material field and the like.
Description
Technical field
The invention belongs to the polyaniline nanotube field, particularly a kind ofly take beta-cyclodextrin and prepare the method for the controlled polyaniline nanotube in aperture as template.
Background technology
Polyaniline is a kind of conducting function polymer.Have synthetic 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 the polyaniline nano material is as low-dimensional materials, the dimensional effect of nano material, quantum effect etc. are given its special physical and chemical performance, therefore the synthetic and applied research of polyaniline nano material has caused scientific research personnel's very big interest, has become one of focus of conducting function field of polymer technology.
Some researchs show, the regulatable polyaniline nanotube in development aperture is a focus in polyaniline research.
Beta-cyclodextrin is 7 D(+)-cyclic oligomer that glucopyranose forms, that its molecule is is wide at the top and narrow at the bottom, the tubular article of both ends open, hollow, and inside, chamber is relative hydrophobicity, and all hydroxyls are in the molecule outside.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind ofly take beta-cyclodextrin and prepares the method for the controlled polyaniline nanotube in aperture as template, and the method is simple to operate, and aftertreatment is easy, and the regulatable polyaniline nanotube pore-forming in prepared aperture is effective.
Of the present inventionly a kind ofly take beta-cyclodextrin as template prepares the method for the controlled polyaniline nanotube in aperture, comprising:
(1) add deionized water by aniline, beta-cyclodextrin and after citric acid mixes, magnetic agitation 0.5h, obtain mixing solutions at ambient temperature;
(2) ammonium persulphate is dissolved in deionized water, obtains the ammonium persulfate solution that concentration is 0.4mol/L;
(3) in 0-10 ℃ of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, obtained 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 the described reaction solution of step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 5: 1: 2: 5.
In the described reaction solution of step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 3.75: 0.75: 2: 5.
In the described reaction solution of 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 using acetone, more colourless to filtrate with deionized water wash.
Drying described in step (3) is at 40-60 ℃ 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 to be soft template with beta-cyclodextrin, and the aniline that concentration is changed in proportion and beta-cyclodextrin be ultrasonic mixing in citric acid solution, and aniline is attached on cyclodextrin internal chamber wall and outer chamber wall as far as possible.Under 0-10 ℃ of condition, with ammonium persulphate oxypolymerization, obtain.
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 descend 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 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%.Reduce monomer and template concentrations and be conducive to be hole.
Beneficial effect:
(1) synthesis condition of the present invention is simple, aftertreatment is easy;
(2) aperture of the prepared polyaniline nanotube of the present invention can regulate and control, and pore-forming is effective, and at antistatic, anticorrosive coating, electromagnetic shielding material, have good application prospect in the various fields such as solar energy materials.
The accompanying drawing explanation
The SEM figure that Fig. 1 is the polyaniline nanotube that obtains of embodiment 1;
The SEM figure that Fig. 2 is the polyaniline nanotube that obtains of embodiment 2;
The SEM figure that Fig. 3 is the polyaniline nanotube that obtains of embodiment 3;
The hole area that Fig. 4 is embodiment 1,2 and 3 gained polyaniline nanotubes accounts for the scale map of total cross-section.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only are not used in and limit the scope of the invention for the present invention is described.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
(1) by aniline and beta-cyclodextrin with add deionized water after citric acid mixes, magnetic agitation 0.5h, obtain mixing solutions at ambient temperature; 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 ℃ of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, after glass stick rapid stirring 1-2min, stop stirring, then standing and reacting 24h; Finally the product that obtains washing (first use acetone, more colourless to filtrate with deionized water wash), dry (at 40-60 ℃ of vacuum-drying 24h) are obtained to polyaniline nanotube.
In the described system of 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%.
(1) by aniline and beta-cyclodextrin with add deionized water after citric acid mixes, magnetic agitation 0.5h, obtain mixing solutions at ambient temperature; 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 ℃ of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, after glass stick rapid stirring 1-2min, stop stirring, then standing and reacting 24h; Finally the product that obtains washing (first use acetone, more colourless to filtrate with deionized water wash), dry (at 40-60 ℃ of vacuum-drying 24h) are obtained to polyaniline nanotube.
In the described system of 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%.
(1) by aniline and beta-cyclodextrin with add deionized water after citric acid mixes, magnetic agitation 0.5h, obtain mixing solutions at ambient temperature; 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 ℃ of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, after glass stick rapid stirring 1-2min, stop stirring, then standing and reacting 24h; Finally the product that obtains washing (first use acetone, more colourless to filtrate with deionized water wash), dry (at 40-60 ℃ of vacuum-drying 24h) are obtained to polyaniline nanotube.
In the described system of 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 (9)
1. take beta-cyclodextrin as template prepares the method for the controlled polyaniline nanotube in aperture for one kind, comprising:
(1) add deionized water by aniline, beta-cyclodextrin and after citric acid mixes, magnetic agitation 0.5h, obtain mixing solutions at ambient temperature;
(2) ammonium persulphate is dissolved in deionized water, obtains the ammonium persulfate solution that concentration is 0.4mol/L;
(3) in 0-10 ℃ of water bath with thermostatic control, above-mentioned ammonium persulfate solution is poured into rapidly in above-mentioned mixing solutions, obtained 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.
2. according to claim 1ly a kind ofly take beta-cyclodextrin as template prepares the method for the controlled polyaniline nanotube in aperture, it is characterized in that: the pH value of the mixing solutions that step (1) obtains is 2-6.
3. according to claim 1ly a kind ofly take beta-cyclodextrin and prepare the method for the controlled polyaniline nanotube in aperture as template, it is characterized in that: in the described reaction solution of step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 5: 1: 2: 5.
4. according to claim 1ly a kind ofly take beta-cyclodextrin and prepare the method for the controlled polyaniline nanotube in aperture as template, it is characterized in that: in the described reaction solution of step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 3.75: 0.75: 2: 5.
5. according to claim 1ly a kind ofly take beta-cyclodextrin and prepare the method for the controlled polyaniline nanotube in aperture as template, it is characterized in that: in the described reaction solution of step (3), the molar concentration rate of aniline, beta-cyclodextrin, citric acid and ammonium persulphate is 2.5: 0.5: 2: 5.
6. according to claim 1ly a kind ofly take beta-cyclodextrin and prepare the method for the controlled polyaniline nanotube in aperture as template, it is characterized in that: the speed of the rapid stirring described in step (3) is 200-500rpm.
7. according to claim 1ly a kind ofly take beta-cyclodextrin as template prepares the method for the controlled polyaniline nanotube in aperture, it is characterized in that: the washing described in step (3) is for first using acetone, more colourless to filtrate with deionized water wash.
8. according to claim 1ly a kind ofly take beta-cyclodextrin as template prepares the method for the controlled polyaniline nanotube in aperture, it is characterized in that: the drying described in step (3) is at 40-60 ℃ of vacuum-drying 24h.
9. describedly a kind ofly take beta-cyclodextrin and prepare the method for the controlled polyaniline nanotube in aperture as template according to claim 3,4 or 5, 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936983A (en) * | 2014-04-10 | 2014-07-23 | 东华大学 | Method for preparing polyaniline micron/nano structure by using polylactic acid regulation and control |
| CN104371138A (en) * | 2014-11-13 | 2015-02-25 | 吉林大学 | Method for preparing polyarylether microporous membrane with adjustable 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 |
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| 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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| 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)
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| MIRCEA GRIGORAS,ET AL: "Chemical oxidative polymerization of β-cyclodextrin/aniline inclusion complex", 《JOURNAL OF INCLUSION PHENOMENA AND MACROCYCLIC CHEMISTRY》, vol. 54, no. 12, 1 February 2006 (2006-02-01), pages 101 - 107, XP019248856 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936983A (en) * | 2014-04-10 | 2014-07-23 | 东华大学 | Method for preparing polyaniline micron/nano structure by using polylactic acid regulation and control |
| CN104371138A (en) * | 2014-11-13 | 2015-02-25 | 吉林大学 | Method for preparing polyarylether microporous membrane with adjustable aperture |
| 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 |
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