CN105037718A - Method for preparing conductive polyaniline nano tube by taking D-tartaric acid as template - Google Patents
Method for preparing conductive polyaniline nano tube by taking D-tartaric acid as template Download PDFInfo
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- CN105037718A CN105037718A CN201510534026.9A CN201510534026A CN105037718A CN 105037718 A CN105037718 A CN 105037718A CN 201510534026 A CN201510534026 A CN 201510534026A CN 105037718 A CN105037718 A CN 105037718A
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Abstract
The invention discloses a method for preparing a conductive polyaniline nano tube by taking D-tartaric acid as a template. The method for preparing the conductive polyaniline nano tube by taking the D-tartaric acid as the template comprises the following steps: dispersing aniline into different aqueous solutions containing D-tartaric acid in different ratios, and fully stirring in ice-water bath, so that a uniform mixed solution is obtained; and then dropwise adding an oxidation initiating agent, namely ammonium persulphate for initiating polymerization of aniline, reacting for 12 hours while stirring, and then doping with a 2mL hydrochloric acid solution with the concentration of 1M, so that a conductive polyaniline material of a tubular structure is obtained. The method for preparing the conductive polyaniline nano tube by taking the D-tartaric acid as the template has the advantages that a preparation process is simple, environment-friendly and reliable, raw materials are available, and cost is low, so that the method disclosed by the invention is applicable to industrial production; and the obtained nano tubular conductive polyaniline has lower resistance and higher specific capacitance compared with pure polyaniline.
Description
Technical field
The invention belongs to conductive nanotube preparing technical field, particularly a kind of with the method for D-tartrate for Template preparation Preparation of conductive polyaniline nanotubes.The method with D-tartrate be template, aniline prepares the electrically conductive polyaniline with nano tubular structure by self-assembly and in-situ polymerization.
Background technology
Polyaniline is as a kind of common conductive polymers, because its preparation is simple, with low cost, and there is good environmental stability and unique physics and chemistry character, usually be used to ultracapacitor, battery, sensor and corrosion-resistant field, obtain the concern energetically of countries in the world researcher.Particularly there is the electrically conductive polyaniline of nanostructure, because its particle diameter is minimum, the character such as specific surface area is large, the electron transfer rate that is exceedingly fast, imparts nano-conductive polyaniline material and there are many special performances not available for conventional blocks.
Polyaniline nanotube, owing to can provide passage easily for the diffusion of electrolyte ion and movement, shortens the distance of ion transportation, thus improves the efficiency of ion and electrode generation redox reaction, receive concern and the research of researcher.For example prepare Preparation of conductive polyaniline nanotubes (Z.J.Gu, etal, Synthesisofpolyanilinenanotubeswithcontrolledrectangular orsquareporeshape.Mater.Lett.2014,121,12-14 with soft template method, H.J.Yin, etal, Synthesisofhigh-performanceone-dimensionalpolyanilinenan ostructuresusingdodecylbenzenesulfonicacidassofttemplate .Mater.Lett.2011,65,850-853, M.M.Sk, etal, Synthesisofpolyanilinenanotubesusingtheself-assemblybeha viorofvitaminC:amechanisticstudyandapplicationinelectroc hemicalsupercapacitors.J.Mater.Chem.A2014, 2, 2830-2838.) and without template synthesis Preparation of conductive polyaniline nanotubes (Z.Z.Huang, etal, Preparationofpolyanilinenanotubesbyatemplate-freeself-as semblymethod.Mater.Lett.2011, 65, 2015-2018.), polyaniline nanotube prepared by above-mentioned various soft template method has regular tubular structure and has good chemical property, but in suitability for industrialized production, there is certain difficulty.Without template synthesis polyaniline, there is environmental protection, the advantage such as simple, but the pipe diameter size of gained polyaniline nanotube cannot controlled and irregularity, have impact on the chemical property of polyaniline to a certain extent.
D-tartrate has good water-soluble, and wide material sources, cheap, especially its molecular chain exists a large amount of hydroxyls and carboxyl, can form a large amount of hydrogen bonds with aniline molecule, is suitable as that preparation is nanotube-shaped, the template of club-shaped material.Making Template preparation polyaniline nanotube with D-tartrate is a kind of simple and preparation method of environmental protection, gained polyaniline nano tubulose compound with regular structure and there is good chemical property, be a kind of desirable electrode material for super capacitor, be especially applicable to suitability for industrialized production.
Summary of the invention
The object of this invention is to provide and be a kind ofly template with D-tartrate, prepared the method for the Preparation of conductive polyaniline nanotubes with ordered structure by the method for self-assembling technique and in-situ polymerization.
Thinking of the present invention: utilize the hydroxyl on D-tartaric acid molecules and aniline molecule to form hydrogen bonding nano tubular structure polyaniline, for electrolyte ion diffusion and mobile provide good passage, ion is enable fully redox reaction to occur with electrode materials, thus increase the ratio capacitance of material, reduce its internal resistance.Gained nano tubular structure polyaniline has good chemical property, is a kind of desirable electrode material for super capacitor.
Concrete steps are:
(1) take raw material, D-tartrate according to following amount of substance ratio: aniline=0.5 ~ 4:1, wherein aniline is 0.9mL.
(2) the D-tartrate that step (1) takes is joined in the flask filling 20ml deionized water, stirring at room temperature 10min, by flask transposition in ice-water bath, then in flask, aniline that step (1) takes is added and 2mL concentration is the hydrochloric acid soln of 1mol/L, 1h is stirred, obtained mixing solutions under ice bath.
(3) ammonium persulfate aqueous solution containing 2.3g ammonium persulphate is dropwise joined in the obtained mixing solutions of step (2), 12h is stirred under the condition of ice-water bath, the hydrochloric acid soln that 2mL concentration is 1mol/L is added again in mixing solutions, polyaniline is fully adulterated, then with deionized water carry out washing, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 60 DEG C, grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
Preparation process of the present invention is simple, environmental protection, reliable, raw material sources are extensive, with low cost, be applicable to suitability for industrialized production, and obtained nano tubular structure electrically conductive polyaniline have lower resistance, higher ratio capacitance than pure polyaniline.
Accompanying drawing explanation
Fig. 1 is the constant current charge-discharge graphic representation of Preparation of conductive polyaniline nanotubes when current density is 0.2A/g prepared by the embodiment of the present invention 1 ~ 5.
Fig. 2 is the constant current charge-discharge graphic representation of Preparation of conductive polyaniline nanotubes under different current density prepared by the embodiment of the present invention 2.
Fig. 3 is the constant current charge-discharge graphic representation of Preparation of conductive polyaniline nanotubes under different current density prepared by the embodiment of the present invention 3.
Fig. 4 is the constant current charge-discharge graphic representation of Preparation of conductive polyaniline nanotubes under different current density prepared by the embodiment of the present invention 4.
Wherein, the specific capacitance of embodiment 2 gained Preparation of conductive polyaniline nanotubes when current density is 0.2A/g, 0.5A/g, 0.7A/g and 1A/g is respectively 541.2F/g, 551.9F/g, 576.2F/g and 604.2F/g; The specific capacitance of embodiment 3 gained Preparation of conductive polyaniline nanotubes when current density is 0.2A/g, 0.5A/g, 0.7A/g and 1A/g is respectively 567.5F/g, 532.3F/g, 530.9F/g and 533.6F/g; The specific capacitance of embodiment 4 gained Preparation of conductive polyaniline nanotubes when current density is 0.2A/g, 0.5A/g, 0.7A/g and 1A/g is respectively 406.1F/g, 455.6F/g, 478.2F/g and 508.9F/g.
Fig. 5 is the electric capacity that prepared by the embodiment of the present invention 1 ~ 5, Preparation of conductive polyaniline nanotubes is tested when current density is 0.2A/g.
Embodiment
embodiment 1:
(1) take raw material, D-tartrate according to following amount of substance ratio: aniline=0:1, wherein aniline is 0.9mL.
(2) aniline step (1) taken and 2mL concentration are that the hydrochloric acid soln of 1mol/L joins in the flask filling 20ml deionized water, under ice bath, stir 1h, obtained mixing solutions.
(3) ammonium persulfate aqueous solution containing 2.3g ammonium persulphate is dropwise joined in the obtained mixing solutions of step (2), 12h is stirred under the condition of ice-water bath, the hydrochloric acid soln that 2mL concentration is 1mol/L is added again in mixing solutions, polyaniline is fully adulterated, then with deionized water carry out washing, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 60 DEG C, grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
embodiment 2:
(1) D-tartrate 0.74g and aniline 0.9mL is taken.
(2) the D-tartrate that step (1) takes is joined in the flask filling 20ml deionized water, stirring at room temperature 10min, by flask transposition in ice-water bath, then in flask, aniline that step (1) takes is added and 2mL concentration is the hydrochloric acid soln of 1mol/L, 1h is stirred, obtained mixing solutions under ice bath.
(3) ammonium persulfate aqueous solution containing 2.3g ammonium persulphate is dropwise joined in the obtained mixing solutions of step (2), 12h is stirred under the condition of ice-water bath, the hydrochloric acid soln that 2mL concentration is 1mol/L is added again in mixing solutions, polyaniline is fully adulterated, then with deionized water carry out washing, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 60 DEG C, grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
embodiment 3:
(1) D-tartrate 1.48g and aniline 0.9mL is taken.
(2) the D-tartrate that step (1) takes is joined in the flask filling 20ml deionized water, stirring at room temperature 10min, by flask transposition in ice-water bath, then in flask, aniline that step (1) takes is added and 2mL concentration is the hydrochloric acid soln of 1mol/L, 1h is stirred, obtained mixing solutions under ice bath.
(3) ammonium persulfate aqueous solution containing 2.3g ammonium persulphate is dropwise joined in the obtained mixing solutions of step (2), 12h is stirred under the condition of ice-water bath, the hydrochloric acid soln that 2mL concentration is 1mol/L is added again in mixing solutions, polyaniline is fully adulterated, then with deionized water carry out washing, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 60 DEG C, grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
embodiment 4:
(1) D-tartrate 2.96g and aniline 0.9mL is taken.
(2) the D-tartrate that step (1) takes is joined in the flask filling 20ml deionized water, stirring at room temperature 10min, by flask transposition in ice-water bath, then in flask, aniline that step (1) takes is added and 2mL concentration is the hydrochloric acid soln of 1mol/L, 1h is stirred, obtained mixing solutions under ice bath.
(3) ammonium persulfate aqueous solution containing 2.3g ammonium persulphate is dropwise joined in the obtained mixing solutions of step (2), 12h is stirred under the condition of ice-water bath, the hydrochloric acid soln that 2mL concentration is 1mol/L is added again in mixing solutions, polyaniline is fully adulterated, then with deionized water carry out washing, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 60 DEG C, grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
embodiment 5:
(1) D-tartrate 5.93g and aniline 0.9mL is taken.
(2) the D-tartrate that step (1) takes is joined in the flask filling 20ml deionized water, stirring at room temperature 10min, by flask transposition in ice-water bath, then in flask, aniline that step (1) takes is added and 2mL concentration is the hydrochloric acid soln of 1mol/L, 1h is stirred, obtained mixing solutions under ice bath.
(3) ammonium persulfate aqueous solution containing 2.3g ammonium persulphate is dropwise joined in the obtained mixing solutions of step (2), 12h is stirred under the condition of ice-water bath, the hydrochloric acid soln that 2mL concentration is 1mol/L is added again in mixing solutions, polyaniline is fully adulterated, then with deionized water carry out washing, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 60 DEG C, grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
Claims (1)
1., with the method for D-tartrate for Template preparation Preparation of conductive polyaniline nanotubes, it is characterized in that concrete steps are:
(1) take raw material, D-tartrate according to following amount of substance ratio: aniline=0.5 ~ 4:1, wherein aniline is 0.9mL;
(2) the D-tartrate that step (1) takes is joined in the flask filling 20ml deionized water, stirring at room temperature 10min, by flask transposition in ice-water bath, then in flask, aniline that step (1) takes is added and 2mL concentration is the hydrochloric acid soln of 1mol/L, 1h is stirred, obtained mixing solutions under ice bath;
(3) ammonium persulfate aqueous solution containing 2.3g ammonium persulphate is dropwise joined in the obtained mixing solutions of step (2), 12h is stirred under the condition of ice-water bath, the hydrochloric acid soln that 2mL concentration is 1mol/L is added again in mixing solutions, polyaniline is fully adulterated, then with deionized water carry out washing, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 60 DEG C, grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754093A (en) * | 2016-04-20 | 2016-07-13 | 桂林理工大学 | Method for preparing conductive polyaniline nano-rod by using malic acid as template and dopant |
| CN106920971A (en) * | 2017-02-16 | 2017-07-04 | 江苏大学 | A kind of cluster polyaniline nano fiber composite carbon electrode and preparation method and purposes |
| 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 |
| CN107221457A (en) * | 2017-05-16 | 2017-09-29 | 常州大学 | A kind of preparation method of D winestones acid doped polyaniline electrode |
| CN110819106A (en) * | 2018-08-09 | 2020-02-21 | 中国科学院大连化学物理研究所 | Preparation of PANI/BaTiO3Method (2) |
-
2015
- 2015-08-27 CN CN201510534026.9A patent/CN105037718A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| JINGJING MU, ET AL: ""Facile fabrication of self-assembled polyaniline nanotubes doped with D-tartaric acid for high-performance supercapacitors"", 《JOURNAL OF POWER SOURCES》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105754093A (en) * | 2016-04-20 | 2016-07-13 | 桂林理工大学 | Method for preparing conductive polyaniline nano-rod by using malic acid as template and dopant |
| CN106920971A (en) * | 2017-02-16 | 2017-07-04 | 江苏大学 | A kind of cluster polyaniline nano fiber composite carbon electrode and preparation method and purposes |
| CN106920971B (en) * | 2017-02-16 | 2019-12-31 | 江苏大学 | Clustered polyaniline nanofiber composite carbon electrode and preparation method and application 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 |
| CN107221457A (en) * | 2017-05-16 | 2017-09-29 | 常州大学 | A kind of preparation method of D winestones acid doped polyaniline electrode |
| CN110819106A (en) * | 2018-08-09 | 2020-02-21 | 中国科学院大连化学物理研究所 | Preparation of PANI/BaTiO3Method (2) |
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