CN104962945B - A kind of electrochemical method for synthesizing of sea urchin shape micrometer/nanometer structure polyaniline - Google Patents
A kind of electrochemical method for synthesizing of sea urchin shape micrometer/nanometer structure polyaniline Download PDFInfo
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- CN104962945B CN104962945B CN201510258303.8A CN201510258303A CN104962945B CN 104962945 B CN104962945 B CN 104962945B CN 201510258303 A CN201510258303 A CN 201510258303A CN 104962945 B CN104962945 B CN 104962945B
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- polyaniline
- sea urchin
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- urchin shape
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Abstract
The present invention relates to a kind of electrochemical method for synthesizing of sea urchin shape micrometer/nanometer structure polyaniline.The process of the synthetic method is summarized as follows：(1) electrolyte solution of aniline monomer and dopant acid is prepared；(2) three-electrode system is used, passes through cyclic voltammetry electrochemical polymerization aniline；(3) obtained polyaniline modified electrode is embathed with deionized water, dried in vacuum drying chamber, you can obtain blackish green polyaniline product, its pattern is in sea urchin shape nanostructured.The advantage of this method is that building-up process is simple and does not introduce impurity, and building-up process can be accomplished without wanting special low temperature environment under normal temperature environment, and obtained polyaniline structure is controllable.The polyaniline of prepared sea urchin shape nanostructured has good application prospect in sensor, capacitor, anti-corrosion and the field such as antifouling.
Description
Technical field
The invention belongs to polyaniline synthetic technology and nanostructured synthesis field, and in particular to a kind of nano junction of sea urchin shape
The electrochemical method for synthesizing of structure polyaniline.
Background technology
Later 1970s, Shirakawa, MacDiarmid, Heeger et al. have found doped polyacetylene
It is electric conductivity with metallic character, so as to open the gate of conducting polymer.Polyaniline as a kind of conducting polymer, due to
There are a variety of oxidation state in it, with electrical and optical activity, and aniline monomer is with low cost, oxidation/reduction invertibity and chemistry
The features such as stability, in rechargable power supplies, sensor, magnetic screen, electrochemical capacitor, anti-corrosion and the field such as antifouling by extensive
Concern and application.
In recent years, the polyaniline of nanostructured due to it shows excellent property in terms of electricity, optics and in section
Educational circles enjoys favor, and the research to its synthetic method and application is even more to emerge in an endless stream.Polyaniline nano structure includes nano wire, received
Rice rod, nanotube and nanofiber etc..The synthetic method of current micrometer/nanometer structure polyaniline includes template, self-assembly method, electrification
Method, phonochemistry polymerization, interfacial polymerization, electrostatic spinning etc..Wherein electrochemical method includes cyclic voltammetry, constant potential
Method, galvanostatic method etc..Qin Zongyi etc. [CN 103408754A] successfully synthesizes polyaniline nano using a kind of unique solwution method
Fiber.This method without using template, and react carried out in aqueous phase thus product postprocessing it is simple, can be used in extensive batch
Amount production.Wang Jixiao etc. [CN 101139440A] is prepared for the polyaniline with nanometer chip architecture using one-step method, and it prepares work
Skill process is simple, and the purity of polyaniline may be up to 100%.Kan Jinqing etc. uses electrochemical method, is prepared for Nano fiber polyaniline
Tie up [CN 1958854A], the characteristics of with uniform particle sizes, queueing discipline.Pan Mu etc. [CN 103255433A] uses two electrode bodies
The electrochemical method for synthesizing of Fast back-projection algorithm electrically conductive polyaniline under system, high current, obtains being in nano bar-shape structure, a diameter of 100-
350nm polyaniline.Although having there is the synthetic method of the polyaniline of many nanostructureds at present, novel nano knot is sought
The synthetic method of structure polyaniline still has great importance.
The content of the invention
The purpose of the present invention solves the deficiencies in the prior art, and there is provided a kind of sea urchin shape nanostructured of simple possible
The electrochemical method for synthesizing of polyaniline.
The electrochemical method for synthesizing of the polyaniline of sea urchin shape nanostructured is to use cyclic voltammetry, in three-electrode system
Interior, the electrochemical polymerization aniline in the mixed electrolytic solution that aniline and proton dopant acid are constituted, polymerization terminates to repair on rear working electrode
The product of decorations is polyaniline, and its pattern is in sea urchin shape nanostructured.
The electrochemical method for synthesizing of the polyaniline of sea urchin shape nanostructured is comprised the following steps that：
(1) aniline that will be greater than the chromatographic grade equal to 99.98% is added to concentration for 0.8 ~ 1 molL-1Proton doping
In acid solution, stir, the concentration of aniline is controlled in 0.1 ~ 0.45molL-1, obtained mixed solution is molten as electrolyte
Liquid, it is stand-by；
(2) it is injected into mixed solution as electrolyte solution in electrolytic cell, using saturated calomel electrode as reference electrode,
It is electric by work of a diameter of 1 mm platinum filament using a diameter of 2 mm platinum disk electrode or a diameter of 1 mm platinum filament as to electrode
Pole, the length of working electrode is 6 ~ 8 cm, and the length for the platinum filament being immersed in electrolyte is 1 ~ 3 cm, and magnetic agitation, magneton turns
Speed is 120 ~ 150 rmin-1；
(3) cyclic voltammetry electrochemical polymerization aniline at 10 ~ 30 DEG C is used, the parameter of cyclic voltammetry is set to：Electricity
Pressure scope is -0.1 ~ 1 V vs. SCE, and sweep speed is 5 ~ 20mv s-1, scanning times are 2 ~ 25 times；
(4) after the completion of polymerizeing, the platinum filament for being modified with polyaniline is taken out from electrolyte, embathed with deionized water, removed
The proton dopant acid of polyaniline surface attachment；
(5) platinum filament for being modified with polyaniline is dried in vacuo 40 ~ 50h in 30 ~ 35 DEG C of vacuum drying chamber, you can
To the polyaniline of sea urchin shape nanostructured.
Described proton dopant acid is hydrochloric acid, phosphoric acid or perchloric acid.The polyaniline of described sea urchin shape nanostructured is ink
The polyaniline of green sea urchin shape nanostructured.
The present invention has the advantage that compared with prior art：
(1) electrolyte composition is simple.Electrolyte used in the method for the present invention is the mixed solution of aniline and inorganic acid,
Therefore the product obtained is the polyaniline of acid doping, and without other miscellaneous as initiator, oxidant or surfactant
Matter.
(2) polymerizing condition is simple.The present invention uses cyclic voltammetry electrochemical polymerization aniline, and the polymerisation is in room temperature
Under can carry out, without provide low temperature environment.
(3) product postprocessing is simple.As described in (1), the product that polyaniline obtains is prepared using the method for the present invention straight
It is connected in the polyaniline of acid doping, therefore product postprocessing process need to only be dried in vacuo and eliminate the cumbersome of the removal of impurity and purification
Process.
(4) structure-controllable of polyaniline.Under the experiment condition of the present invention, obtained polyaniline is the sea urchin of acid doping
The blackish green polyaniline of shape nanostructured.
The polyaniline of sea urchin shape nanostructured prepared by the present invention is expected in sensor, capacitor, anti-corrosion of metal, biology
The field such as antifouling obtains wide application prospect.
Brief description of the drawings
Fig. 1 is the scanning electron microscopic picture (SEM) for the sea urchin shape micrometer/nanometer structure polyaniline that the present invention is obtained.
Embodiment
The electrochemical method for synthesizing of the polyaniline of sea urchin shape nanostructured is to use cyclic voltammetry, in three-electrode system
Interior, the electrochemical polymerization aniline in the mixed electrolytic solution that aniline and proton dopant acid are constituted, polymerization terminates to repair on rear working electrode
The product of decorations is polyaniline, and its pattern is in sea urchin shape nanostructured.
Embodiment 1：
The electrochemical method for synthesizing of the polyaniline of sea urchin shape nanostructured comprises the following steps that in the present embodiment：
(1) aniline that will be greater than the chromatographic grade equal to 99.98% is added to concentration for 1 molL-1Hydrochloric acid solution in,
Stir, the concentration of aniline is controlled in 0.1molL-1, obtained mixed solution is stand-by as electrolyte solution；
(2) it is injected into mixed solution as electrolyte solution in electrolytic cell, using saturated calomel electrode as reference electrode,
Using a diameter of 2 mm platinum disk electrode as to electrode, the platinum filament using a diameter of 1 mm is working electrode, and the length of working electrode is 6
Cm, the length for the platinum filament being immersed in electrolyte is 1 cm, and magnetic agitation, magneton rotating speed is 120 rmin-1；
(3) cyclic voltammetry electrochemical polymerization aniline at 10 DEG C is used, the parameter of cyclic voltammetry is set to：Voltage
Scope is -0.1 ~ 1 V vs. SCE, and sweep speed is 5 mv s-1, scanning times are 25 times；
(4) after the completion of polymerizeing, the platinum filament for being modified with polyaniline is taken out from electrolyte, embathed with deionized water, removed
The hydrochloric acid of polyaniline surface attachment；
(5) platinum filament for being modified with polyaniline is dried in vacuo 40 h in 30 DEG C of vacuum drying chamber, you can obtain sea
The polyaniline of courage shape nanostructured.
Embodiment 2：
The electrochemical method for synthesizing of the polyaniline of sea urchin shape nanostructured comprises the following steps that in the present embodiment：
(1) aniline that will be greater than the chromatographic grade equal to 99.98% is added to concentration for 0.8 molL-1Phosphoric acid solution
In, stir, the concentration of aniline is controlled in 0.45molL-1, obtained mixed solution is stand-by as electrolyte solution；
(2) it is injected into mixed solution as electrolyte solution in electrolytic cell, using saturated calomel electrode as reference electrode,
Using a diameter of 1 mm platinum filament as to electrode, the platinum filament using a diameter of 1 mm is working electrode, and the length of working electrode is 8 cm,
The length for the platinum filament being immersed in electrolyte is 3 cm, and magnetic agitation, magneton rotating speed is 150 rmin-1；
(3) cyclic voltammetry electrochemical polymerization aniline at 30 DEG C is used, the parameter of cyclic voltammetry is set to：Voltage model
Enclose for -0.1 ~ 1 V vs. SCE, sweep speed is 20mv s-1, scanning times are 2 times；
(4) after the completion of polymerizeing, the platinum filament for being modified with polyaniline is taken out from electrolyte, embathed with deionized water, removed
The phosphoric acid of polyaniline surface attachment；
(5) platinum filament for being modified with polyaniline is dried in vacuo 50h in 35 DEG C of vacuum drying chamber, you can obtain sea urchin
The polyaniline of shape nanostructured.
Embodiment 3：
The electrochemical method for synthesizing of the polyaniline of sea urchin shape nanostructured comprises the following steps that in the present embodiment：
(1) aniline that will be greater than the chromatographic grade equal to 99.98% is added to concentration for 1 molL-1Perchloric acid solution
In, stir, the concentration of aniline is controlled in 0.15molL-1, obtained mixed solution is stand-by as electrolyte solution；
(2) it is injected into mixed solution as electrolyte solution in electrolytic cell, using saturated calomel electrode as reference electrode,
Using a diameter of 1 mm platinum filament as to electrode, the platinum filament using a diameter of 1 mm is working electrode, and the length of working electrode is 7 cm,
The length for the platinum filament being immersed in electrolyte is 2 cm, and magnetic agitation, magneton rotating speed is 130 rmin-1；
(3) cyclic voltammetry electrochemical polymerization aniline at 30 DEG C is used, the parameter of cyclic voltammetry is set to：Voltage model
Enclose for -0.1 ~ 1 V vs. SCE, sweep speed is 5 mv s-1, scanning times are 20 times；
(4) after the completion of polymerizeing, the platinum filament for being modified with polyaniline is taken out from electrolyte, embathed with deionized water, removed
The perchloric acid of polyaniline surface attachment；
(5) platinum filament for being modified with polyaniline is dried in vacuo 48 h in 30 DEG C of vacuum drying chamber, you can obtain sea urchin
The polyaniline of shape nanostructured.
The polyaniline of described obtained sea urchin shape nanostructured is the polyaniline of blackish green sea urchin shape nanostructured.
Claims (3)
1. a kind of electrochemical method for synthesizing of the polyaniline of sea urchin shape nanostructured, it is characterised in that comprise the following steps that：
(1) aniline that will be greater than the chromatographic grade equal to 99.98% is added to concentration for 0.8 ~ 1 molL-1Proton dopant acid it is molten
In liquid, stir, the concentration of aniline is controlled in 0.1 ~ 0.45molL-1, obtained mixed solution treats as electrolyte solution
With；
(2) it is injected into mixed solution as electrolyte solution in electrolytic cell, using saturated calomel electrode as reference electrode, with straight
The platinum disk electrode or a diameter of 1 mm platinum filament that footpath is 2 mm are that, to electrode, the platinum filament using a diameter of 1 mm is working electrode, work
The length for making electrode is 6 ~ 8 cm, and the length of the platinum filament being immersed in electrolyte is 1 ~ 3 cm, magnetic agitation, and magneton rotating speed is
120~150 r·min-1；
(3) cyclic voltammetry electrochemical polymerization aniline at 10 ~ 30 DEG C is used, the parameter of cyclic voltammetry is set to：Voltage model
Enclose for -0.1 ~ 1 V vs. SCE, sweep speed is 5 ~ 20mv s-1, scanning times are 2 ~ 25 times；
(4) after the completion of polymerizeing, the platinum filament for being modified with polyaniline is taken out from electrolyte, embathed with deionized water, remove polyphenyl
The proton dopant acid of amine surface attachment；
(5) platinum filament for being modified with polyaniline is dried in vacuo 40 ~ 50h in 30 ~ 35 DEG C of vacuum drying chamber, you can obtain sea
The polyaniline of courage shape nanostructured.
2. according to the method described in claim 1, it is characterised in that described proton dopant acid is hydrochloric acid, phosphoric acid or perchloric acid.
3. according to the method described in claim 1, it is characterised in that the polyaniline of described sea urchin shape nanostructured is blackish green
The polyaniline of sea urchin shape nanostructured.
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| CN105461920B (en) * | 2015-12-16 | 2018-02-23 | 华南师范大学 | Method and the application of one pot process sea urchin shape golden nanometer particle and spherical polyaniline |
| CN111272842B (en) * | 2020-02-25 | 2022-09-30 | 衡阳师范学院 | Polyaniline modified electrode capable of quantitatively detecting estrone and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03173787A (en) * | 1989-11-30 | 1991-07-29 | Central Glass Co Ltd | Production of polyaniline |
| CN102505130A (en) * | 2011-12-01 | 2012-06-20 | 昆明理工大学 | Polyaniline-coated Al-based Pb-WC composite anode and preparation method thereof |
| CN102516764A (en) * | 2011-11-17 | 2012-06-27 | 华东理工大学 | Polyaniline nanowire/ graded porous carbon composite material as well as preparation method and application thereof |
| CN103063722A (en) * | 2012-12-13 | 2013-04-24 | 浙江大学 | Solid calcium ion electrode based on conductive polyaniline and preparing method thereof |
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| US7255924B2 (en) * | 2004-01-13 | 2007-08-14 | The United States Of America As Represented By The Secretary Of The Navy | Carbon nanoarchitectures with ultrathin, conformal polymer coatings for electrochemical capacitors |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03173787A (en) * | 1989-11-30 | 1991-07-29 | Central Glass Co Ltd | Production of polyaniline |
| CN102516764A (en) * | 2011-11-17 | 2012-06-27 | 华东理工大学 | Polyaniline nanowire/ graded porous carbon composite material as well as preparation method and application thereof |
| CN102505130A (en) * | 2011-12-01 | 2012-06-20 | 昆明理工大学 | Polyaniline-coated Al-based Pb-WC composite anode and preparation method thereof |
| CN103063722A (en) * | 2012-12-13 | 2013-04-24 | 浙江大学 | Solid calcium ion electrode based on conductive polyaniline and preparing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 苯胺的电聚合研究;孙东豪等;《苏州丝绸工学院学报》;19991231;第19卷(第3期);第21-23页 * |
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