CN101492536A - Nano-polyaniline material with morphology inheritance and electrochemical preparation method - Google Patents
Nano-polyaniline material with morphology inheritance and electrochemical preparation method Download PDFInfo
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- CN101492536A CN101492536A CNA2008100208254A CN200810020825A CN101492536A CN 101492536 A CN101492536 A CN 101492536A CN A2008100208254 A CNA2008100208254 A CN A2008100208254A CN 200810020825 A CN200810020825 A CN 200810020825A CN 101492536 A CN101492536 A CN 101492536A
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Abstract
The invention discloses a nanometer polyaniline material with appearance hereditary potency and an electrochemistry preparation method thereof. The method comprises the following steps: aniline and doping acid I are added into water, stirred to form doping acid I solution of the aniline; in a three electrode system, the doping acid I solution of the aniline is added into an electrolytic cell; the electrochemical synthesis is carried out on a working electrode for obtaining the polyaniline material with nanometer structure doped with the doping acid I; after the electrochemical synthesis is finished, a polyaniline modified electrode doped with doping acid I is obtained; the modified electrode is used as the working electrode, put into water solution containing doping acid II, electrolyzed to a cyclic voltammetry graph by using cyclic voltammetry and stable to obtain the polyaniline material doped with doping acid II, the appearance of which is same to the polyaniline nanometer structure doped with the doping acid I obtained in the second step. The polyaniline material obtained in the invention only has difference in the chemical composition of doping ions and does not change the microscopic morphology of polyaniline. The appearance hereditary has important using value.
Description
Technical field
The invention belongs to the conducting polymer composite technology, particularly a kind of electrochemical preparation method with nano-polyaniline material of pattern heredity.
Background technology
Conducting polymers such as polyaniline are owing to have excellent electric performance and chemical property, especially also have advantages such as the stable and environmental friendliness of chemical property, be the conducting polymer composite that a class receives much concern, it has broad application prospects at ultracapacitor, chemical power source, antistatic, electrochromism, electromagnetic shielding and aspects such as biological and chemical sensor.
Recent years, along with the deep development in each field of nano science and technology, the conducting polymer of nanostructure such as polyaniline have caused investigator's very big interest.It has the chemico-physical properties of body electrically conductive polyaniline; The unique texture that has nano material again has good application prospects at numerous areas such as transmitter, opto-electronic device, molecular circuit, molecular memory equipment, modified electrode, advanced composite material, the energy and even life science and medicine sustained release.
Although nanostructure PANI has very big specific surface area and gas sensing property preferably, it does not obtain practical application on chemical sensor so far, and its research also only is in the fundamental research stage.
At present, nano structural conductive polyaniline synthetic has template and no template (as interfacial polymerization, self-assembly, electrospinning etc.).Though template is a main method commonly used both at home and abroad and effective synthesis of nano structure organic conductive macromolecule,, there is the preparation process complexity in these methods, the cost height, or template is removed deficiencies such as difficulty; Aspect modified electrode and sensor application, the polymkeric substance that these methods make is in the deposition step more complicated of electrode surface, and the control of film thickness and pattern has certain degree of difficulty, causes industrialized mass production to be difficult to realize.
Summary of the invention
The object of the present invention is to provide a kind of simple and easy, inexpensive synthetic pattern is controlled and have the pattern hereditary property nano-tube/polyaniline conductive material and electrochemical method thereof, promptly this method adopts any one electrochemical method, the control test parameter, the synthetic adulterated nano polyaniline of a kind of acid on working electrode, then this nano polyaniline modified electrode is immersed in the another kind of acid solution, carry out the doping and the dedoping process of dopant ion by the electrochemical method of cyclic voltammetry scan, can obtain another kind of sour adulterated polyaniline material, and pattern remains unchanged.
The technical solution that realizes the object of the invention is: a kind of nano-polyaniline material with pattern hereditary potency, get by following electrochemical production: the first step, aniline and dopant acid I are added in the water, stir the dopant acid I solution of the aniline that forms homogeneous transparent;
Second step, electrochemical synthesis: in three-electrode system, the dopant acid I solution of aniline is added in the electrolyzer, on working electrode, carry out the synthetic polyaniline material for preparing the adulterated nanostructure of dopant acid I of electrochemical method, electrochemical synthesis finishes, a large amount of water flushings, the reactant of removal surface attachment obtains the adulterated polyaniline modified electrode of dopant acid I;
The 3rd step as working electrode, was placed on above-mentioned modified electrode in the aqueous solution that fills dopant acid II, adopted the cyclic voltammetry electrolysis stable to the cyclic voltammetric figure, and final reaction stops at+0.3V (with respect to saturated calomel electrode);
The 4th step, wash above-mentioned electrode, promptly get pattern and the same adulterated polyaniline material of dopant acid II of the second step adulterated polyaniline nano structure of gained dopant acid I.
The present invention compared with prior art, its remarkable advantage: first kind of adulterated polyaniline of acid that (1) goes out by electrochemical production can possess the pattern of any nanostructure, subsequently by changing different acid solutions, doping and dedoping by the cyclic voltammetry scan process, realize that second kind of acid ion is doped to the polyaniline skeleton and substitutes first kind of acid ion, the polyaniline material that this method obtains only there are differences on the chemical ingredients of dopant ion, and can't change the microscopic appearance of polyaniline, application in various fields has important value for this material in this " pattern heredity " truly, as not only doing the contribution that makes new advances in the application of sensor field, can also make the PANI modified electrode of the nanostructure that is used for chemistry and bioelectrochemistry analysis for the conduction PANI film of nanostructure.(2) preparation method of dopant acid I doped polyaniline can be any electrochemical method, can obtain the different dopant acid I doped polyaniline of pattern by the control electrochemical parameter.(3) as long as change different dopant acid II, need not the existence of monomer aniline, can prepare the different sour adulterated polyaniline material of a series of consistent appearance, operating process is easy, cost is low.(4) realized that really pattern is controlled.(5) compare with chemical synthesis process, electrochemical method for synthesizing has characteristics such as product is pure, the controllable thickness of product film, environmental friendliness.(6) polyaniline of application the present invention preparation can have application promise in clinical practice and economic benefit in fields such as super capacitance electrode material, transmitter, environment, life sciences.
Below in conjunction with accompanying drawing the present invention is described in further detail.
Description of drawings
Fig. 1 is the schematic flow sheet that the present invention has the nano-polyaniline material electrochemical preparation method of pattern hereditary potency.
Fig. 2 is dopant acid I, the dopant acid II doped polyaniline nano material sem photograph (polyaniline nano fiber of the doped hydrochloride that obtains after the exchange of adulterated polyaniline of gained camphorsulfonic acid and hydrochloric acid among the embodiment 2) of gained.
Embodiment
In conjunction with Fig. 1, the present invention has the nano-polyaniline material of pattern hereditary potency, gets by following electrochemical production: the first step, aniline and dopant acid I are added in the water, and stir the dopant acid I solution of the aniline that forms homogeneous transparent.Wherein, aniline monomer concentration is 0.1～0.5mol/L; The concentration of dopant acid I and II is 0.5～2mol/L; The mol ratio of aniline and dopant acid I is 1: 1～1: 10.
Second step, electrochemical synthesis: in three-electrode system, the dopant acid I solution of aniline is added in the electrolyzer, on working electrode, carry out the synthetic polyaniline material for preparing the adulterated nanostructure of dopant acid I of electrochemical method, electrochemical synthesis finishes, a large amount of water flushings, the reactant of removal surface attachment obtains the adulterated polyaniline modified electrode of dopant acid I.Electrochemical cell is a three-electrode system, and conductive glass, stainless steel substrates, platinum electrode or gold electrode are as working electrode, and platinized platinum or platinum filament are as counter electrode, and saturated calomel electrode or silver, silver chloride electrode are reference electrode.For the electrochemical method for synthesizing of dopant acid I doped polyaniline is in continuous current, constant potential, pulsed current and the cyclic voltammetry polymerization any, and in the described galvanostatic method polymerization, current density is controlled at 0.01～1.5mA/cm
2In the potentiostatic method polymerization, control of Electric potentials is at 0.6～1.0V; In the cyclic voltammetry, potential range-0.2～1.1V, scanning speed is controlled at 50～150mV/s; In the pulse current method, break make ratio was controlled at 1: 1～10: 1; All current potentials are for saturated calomel electrode.The electro-chemical test temperature is 5～30 ℃.
The 3rd step as working electrode, was placed on above-mentioned modified electrode in the aqueous solution that fills dopant acid II, adopted the cyclic voltammetry electrolysis stable to the cyclic voltammetric figure, and final reaction stops at+0.3V (with respect to saturated calomel electrode).Dopant acid-II doped polyaniline for pattern heredity is obtained by cyclic voltammetry, electric potential scanning scope-0.2～1.0V (with respect to saturated calomel electrode), and scanning speed is controlled at 5～200mV/s.
The 4th step, wash above-mentioned electrode, promptly get pattern and the same adulterated polyaniline material of dopant acid II of the second step adulterated polyaniline nano structure of gained dopant acid I.
Above-mentioned dopant acid I and II are inorganic or organic acid, and the negatively charged ion radius of dopant acid I is bigger than dopant acid II's.Wherein, mineral acid is hydrochloric acid, sulfuric acid or phosphoric acid etc.Organic acid is camphorsulfonic acid, tosic acid or poly-organic acid etc.
Embodiment 1: the present invention has the nano-polyaniline material electrochemical preparation method of pattern hereditary potency, may further comprise the steps:
The first step is added to 5mmol aniline and 25mmol sulfuric acid in the water, stirs, and is made into the transparent mixing solutions of 50ml, and aniline concentration is 0.1mol/L, and sulfuric acid is 0.5mol/L;
Second step was a working electrode with the conductive glass, and platinized platinum is a counter electrode, and saturated calomel electrode is that reference electrode carries out electrochemical synthesis: the above-mentioned solution of 20ml is added in the electrolyzer, adopts potentiostatic method, polymerization is 10 minutes under 1.0V, and experimental temperature is 10 ℃.Finish a large amount of water flushings, the reactant of removal surface attachment;
The 3rd step, above-mentioned modified electrode as working electrode, is placed on and fills in the 20ml 1.0mol/L aqueous solution of hydrochloric acid employing cyclic voltammetry, electrolysis is stable to the CV figure in-0.2V～1.0V potential range, and final reaction stops at+0.3V (with respect to saturated calomel electrode);
The 4th step, wash above-mentioned electrode, promptly get the polyaniline material of the pattern doped hydrochloride the same with the adulterated polyaniline nano fiber of the second step gained sulfuric acid.
Embodiment 2: the present invention has the nano-polyaniline material electrochemical preparation method of pattern hereditary potency, may further comprise the steps:
The first step is added to 5mmol aniline and 50mmol camphorsulfonic acid (CSA) in the water, stirs, and is made into the transparent mixing solutions of 50ml, and aniline concentration is 0.1mol/L, and CSA is 1.0mol/L;
Second step was a working electrode with the gold electrode, and platinized platinum is a counter electrode, and saturated calomel electrode is that reference electrode carries out electrochemical synthesis: the above-mentioned solution of 20ml is added in the electrolyzer, adopts potentiostatic method, polymerization is 10 minutes under 0.8V, and experimental temperature is 20 ℃.Finish a large amount of water flushings, the reactant of removal surface attachment;
The 3rd step is with step 3 in the example 1;
The 4th step, wash above-mentioned electrode, promptly get the polyaniline material of the pattern doped hydrochloride the same with the adulterated polyaniline nano fiber of the 4th step gained camphorsulfonic acid.
The second, the scanning electron microscope diagram sheet of the polyaniline material of four step gained is seen Fig. 2.The result shows that the adulterated polyaniline of CSA is a nanofiber, and the polyaniline behind the doped hydrochloride still is a nanofiber, and mean diameter does not change, and is tens nanometers.
Embodiment 3: the present invention has the nano-polyaniline material electrochemical preparation method of pattern hereditary potency, may further comprise the steps:
The first step is added to 10mmol aniline and 50mmol tosic acid (TSA) in the water, stirs, and is made into transparent mixing solutions, and aniline concentration is 0.2mol/L, and TSA is 1.0mol/L;
Second step was a working electrode with the gold electrode, and platinized platinum is a counter electrode, and saturated calomel electrode is that reference electrode carries out electrochemical synthesis: the above-mentioned solution of 20ml is added in the electrolyzer, adopts galvanostatic method, at 0.5mAcm
-2Polymerization is 5 minutes under the current density, and experimental temperature is 20 ℃.Finish a large amount of water flushings, the reactant of removal surface attachment;
The 3rd step, with above-mentioned modified electrode as working electrode, be placed on and fill in the 20ml 0.5mol/L vitriolic aqueous solution, adopt cyclic voltammetry, electrolysis is stable to the CV figure in-0.2V～1.0V potential range, final reaction stops at+0.3V (with respect to saturated calomel electrode), sweeps speed and is 100mV/s;
The 4th step, wash above-mentioned electrode, promptly get pattern and the same adulterated polyaniline material of sulfuric acid of the second step adulterated nano polyaniline of gained TSA.
Embodiment 4: the present invention has the nano-polyaniline material electrochemical preparation method of pattern hereditary potency, may further comprise the steps:
The first step is added to 5mmol aniline and 25mmol phosphoric acid in the water, stirs, and is made into the transparent mixing solutions of 50ml, and aniline concentration is 0.1mol/L, and phosphoric acid is 0.5mol/L;
Second step was a working electrode with the platinum electrode, and platinized platinum is a counter electrode, and saturated calomel electrode is that reference electrode carries out electrochemical synthesis: the above-mentioned solution of 20ml is added in the electrolyzer, adopts galvanostatic method, at 0.2mAcm
-2Polymerization is 10 minutes under the current density, and experimental temperature is 20 ℃.Finish a large amount of water flushings, the reactant of removal surface attachment;
The 3rd step, above-mentioned modified electrode as working electrode, is placed on and fills in the 20ml 2.0mol/L aqueous solution of hydrochloric acid employing cyclic voltammetry, electrolysis is stable to the CV figure in-0.2V～1.0V potential range, and final reaction stops at+0.3V (with respect to saturated calomel electrode);
The 4th step, wash above-mentioned electrode, promptly get the polyaniline material that pattern and second goes on foot the same doped hydrochloride of the phosphate-doped nano polyaniline of gained.
Embodiment 5: the present invention has the nano-polyaniline material electrochemical preparation method of pattern hereditary potency, may further comprise the steps:
The first step is added to 5mmol aniline and 30mmol polyvinyl sulfonic acid in the water, stirs, and is made into the transparent mixing solutions of 50ml, and aniline concentration is 0.1mol/L, and polyvinyl sulfonic acid is 0.6mol/L;
Second step was a working electrode with the platinum electrode, and platinized platinum is a counter electrode, and saturated calomel electrode is that reference electrode carries out electrochemical synthesis: the above-mentioned solution of 20ml is added in the electrolyzer, adopts galvanostatic method, at 0.2mAcm
-2Polymerization is 10 minutes under the current density, and experimental temperature is 20 ℃.Finish a large amount of water flushings, the reactant of removal surface attachment;
The 3rd step is with step 3 in the example 3;
The 4th step, wash above-mentioned electrode, promptly get pattern and the same adulterated polyaniline material of sulfuric acid of the second step adulterated nano polyaniline of gained polyvinyl sulfonic acid.
Embodiment 6: the present invention has the nano-polyaniline material electrochemical preparation method of pattern hereditary potency, may further comprise the steps:
The first step is added to 10mmol aniline and 50mmol sulfuric acid in the water, stirs, and is made into the transparent mixing solutions of 50ml, and aniline concentration is 0.2mol/L, and sulfuric acid is 1.0mol/L;
Second step was a working electrode with the conductive glass, and platinized platinum is a counter electrode, saturated calomel electrode is that reference electrode carries out electrochemical synthesis: the above-mentioned solution of 20ml is added in the electrolyzer, adopt pulse current method polymerization 10min, break make ratio was controlled at 1: 10～10: 1, and pulse current density is 1mA/cm
2, experimental temperature is 10 ℃.Finish a large amount of water flushings, the reactant of removal surface attachment;
The 3rd step is with step 3 in the example 1;
The 4th step, wash above-mentioned electrode, promptly get the polyaniline material of the pattern doped hydrochloride the same with the adulterated polyaniline nano fiber of the second step gained sulfuric acid.
Claims (10)
1, a kind of nano-polyaniline material with pattern hereditary potency is characterized in that getting by following electrochemical production: the first step, aniline and dopant acid I are added in the water, and stir the dopant acid I solution of the aniline that forms homogeneous transparent;
Second step, electrochemical synthesis: in three-electrode system, the dopant acid I solution of aniline is added in the electrolyzer, on working electrode, carry out the synthetic polyaniline material for preparing the adulterated nanostructure of dopant acid I of electrochemical method, electrochemical synthesis finishes, a large amount of water flushings, the reactant of removal surface attachment obtains the adulterated polyaniline modified electrode of dopant acid I;
The 3rd step as working electrode, was placed on above-mentioned modified electrode in the aqueous solution that fills dopant acid II, adopted the cyclic voltammetry electrolysis stable to the cyclic voltammetric figure, and final reaction stops at+0.3V (with respect to saturated calomel electrode);
The 4th step, wash above-mentioned electrode, promptly get pattern and the same adulterated polyaniline material of dopant acid II of the second step adulterated polyaniline nano structure of gained dopant acid I.
2, a kind of electrochemical preparation method with nano-polyaniline material of pattern hereditary potency is characterized in that step is as follows: the first step, aniline and dopant acid I are added in the water, and stir the dopant acid I solution of the aniline that forms homogeneous transparent;
Second step, electrochemical synthesis: in three-electrode system, the dopant acid I solution of aniline is added in the electrolyzer, on working electrode, carry out the synthetic polyaniline material for preparing the adulterated nanostructure of dopant acid I of electrochemical method, electrochemical synthesis finishes, a large amount of water flushings, the reactant of removal surface attachment obtains the adulterated polyaniline modified electrode of dopant acid I;
The 3rd step as working electrode, was placed on above-mentioned modified electrode in the aqueous solution that fills dopant acid II, adopted the cyclic voltammetry electrolysis stable to the cyclic voltammetric figure, and final reaction stops at+0.3V (with respect to saturated calomel electrode);
The 4th step, wash above-mentioned electrode, promptly get pattern and the same adulterated polyaniline material of dopant acid II of the second step adulterated polyaniline nano structure of gained dopant acid I.
3, the electrochemical preparation method with nano-polyaniline material of pattern hereditary potency according to claim 2 is characterized in that: aniline monomer concentration is 0.1～0.5mol/L; The concentration of dopant acid I and II is 0.5～2mol/L; The mol ratio of aniline and dopant acid I is 1: 1～1: 10.
4, according to claim 2 or 3 described electrochemical preparing methods with nano-polyaniline material of pattern hereditary potency, it is characterized in that: dopant acid I and II are inorganic or organic acid, and the negatively charged ion radius of dopant acid I is bigger than dopant acid II's.
5, the electrochemical preparation method with nano-polyaniline material of pattern hereditary potency according to claim 4 is characterized in that: mineral acid is hydrochloric acid, sulfuric acid or phosphoric acid.
6, the electrochemical preparation method with nano-polyaniline material of pattern hereditary potency according to claim 4 is characterized in that: organic acid is camphorsulfonic acid, tosic acid or poly-organic acid.
7, the electrochemical preparation method with nano-polyaniline material of pattern hereditary potency according to claim 2, it is characterized in that: electrochemical cell is a three-electrode system, conductive glass, stainless steel substrates, platinum electrode or gold electrode are as working electrode, platinized platinum or platinum filament are as counter electrode, and saturated calomel electrode or silver, silver chloride electrode are reference electrode.
8, according to claim 2 or 3 described electrochemical preparing methods with nano-polyaniline material of pattern hereditary potency, it is characterized in that: the electrochemical method for synthesizing of dopant acid I doped polyaniline is any in continuous current, constant potential, pulsed current and the cyclic voltammetry polymerization, in the described galvanostatic method polymerization, current density is controlled at 0.01～1.5mA/cm
2In the potentiostatic method polymerization, control of Electric potentials is at 0.6～1.0V; In the cyclic voltammetry, potential range-0.2～1.1V, scanning speed is controlled at 50～150mV/s; In the pulse current method, break make ratio was controlled at 1: 1～10: 1; All current potentials are for saturated calomel electrode.
9, according to claim 2 or 3 described electrochemical preparing methods with nano-polyaniline material of pattern hereditary potency, it is characterized in that: the dopant acid of pattern heredity-II doped polyaniline is obtained by cyclic voltammetry, electric potential scanning scope-0.2～1.0V (with respect to saturated calomel electrode), scanning speed is controlled at 5～200mV/s.
10, the electrochemical preparation method with nano-polyaniline material of pattern hereditary potency according to claim 2 is characterized in that: the electro-chemical test temperature is 5～30 ℃.
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Cited By (6)
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| CN103936984A (en) * | 2014-04-10 | 2014-07-23 | 东华大学 | Method for preparing polyaniline nanofiber by applying electric field regulation |
| CN104498986A (en) * | 2014-12-22 | 2015-04-08 | 安徽理工大学 | Polyaniline single crystal film with long-term stable existence in atmospheric environment |
| CN105482106A (en) * | 2015-12-07 | 2016-04-13 | 温州大学 | Preparation method of heteropoly acid-inorganic acid mixed acid doped polyaniline / silver composite |
| CN105606678A (en) * | 2015-09-08 | 2016-05-25 | 浙江大学 | Doped polyaniline based solid acid radical electrode and preparation method thereof |
| CN106928434A (en) * | 2017-03-07 | 2017-07-07 | 常州大学 | A kind of method and its application by the tartrate ion synthesis of chiral conducting polymer that adulterates |
| CN108225966A (en) * | 2018-01-31 | 2018-06-29 | 浙江大学 | QCM gas sensors of polyaniline nano-line modification and preparation method and application |
Family Cites Families (1)
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| CN100358937C (en) * | 2006-03-02 | 2008-01-02 | 扬州大学 | Electrochemical synthesis method for producing homogeneous and odered aniline nanometer particles |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103936984A (en) * | 2014-04-10 | 2014-07-23 | 东华大学 | Method for preparing polyaniline nanofiber by applying electric field regulation |
| CN103936984B (en) * | 2014-04-10 | 2016-06-08 | 东华大学 | The method of polyaniline nano fiber is prepared in the regulation and control of a kind of using electric field |
| CN104498986A (en) * | 2014-12-22 | 2015-04-08 | 安徽理工大学 | Polyaniline single crystal film with long-term stable existence in atmospheric environment |
| CN105606678A (en) * | 2015-09-08 | 2016-05-25 | 浙江大学 | Doped polyaniline based solid acid radical electrode and preparation method thereof |
| CN105482106A (en) * | 2015-12-07 | 2016-04-13 | 温州大学 | Preparation method of heteropoly acid-inorganic acid mixed acid doped polyaniline / silver composite |
| CN106928434A (en) * | 2017-03-07 | 2017-07-07 | 常州大学 | A kind of method and its application by the tartrate ion synthesis of chiral conducting polymer that adulterates |
| CN108225966A (en) * | 2018-01-31 | 2018-06-29 | 浙江大学 | QCM gas sensors of polyaniline nano-line modification and preparation method and application |
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