CN105131281A - Method for manufacturing conductive polyaniline nanotube by using xylitol as template - Google Patents
Method for manufacturing conductive polyaniline nanotube by using xylitol as template Download PDFInfo
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- CN105131281A CN105131281A CN201510647039.7A CN201510647039A CN105131281A CN 105131281 A CN105131281 A CN 105131281A CN 201510647039 A CN201510647039 A CN 201510647039A CN 105131281 A CN105131281 A CN 105131281A
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- xylitol
- aniline
- conductive polyaniline
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- deionized water
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Abstract
The invention discloses a method for manufacturing a conductive polyaniline nanotube by using xylitol as a template. The method comprises the steps that a certain amount of xylitol is sufficiently dissolved into deionized water, purified aniline and 10 mL of a 1 mol/M hydrochloric acid solution are added into an ice-water bath, an oxidative initiator of ammonium persulfate is added dropwise after sufficient stirring is performed so as to initiate polymerization of the aniline, and the reaction is performed for 12 h on the stirring condition to obtain a conductive polyaniline material of the tubular structure. The method is simple in preparation process, environmentally friendly, reliable, wide in raw material sources, low in cost and suitable for industrial production, the obtained conductive polyaniline nanotube has the higher specific capacitance and the larger current resistance compared with polyaniline prepared with no template, and the conductive polyaniline nanotube is an ideal supercapacitor electrode material.
Description
Technical field
The invention belongs to Preparation of conductive polyaniline nanotubes preparing technical field, in particular to a kind of take Xylitol as the method for Template preparation Preparation of conductive polyaniline nanotubes, the method take Xylitol as template, and 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 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, Wangetal, Polyanilinenanotubearraysashigh-performanceflexibleelect rodesforelectrochemicalenergystoragedevices.J.Mater.Chem., 2012,22,2401-2404, 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.
Xylitol mainly originates from China, is extensively present among various fruit, vegetables, cereal, has good water-soluble, and it is cheap, especially there is a large amount of hydroxyls in its molecular chain, a large amount of hydrogen bonds can be formed with aniline molecule, be suitable as the template preparing nanotube-shaped material.Making Template preparation polyaniline nanotube with Xylitol is a kind of simple and preparation method of environmental protection, the compound with regular structure of gained polyaniline nanotube and have good chemical property, is a kind of desirable electrode material for super capacitor, is especially applicable to suitability for industrialized production.
Summary of the invention
The object of this invention is to provide a kind of take Xylitol as template, prepare the method with ordered structure and high-specific capacitance super Preparation of conductive polyaniline nanotubes by the method for self-assembling technique and in-situ polymerization.
Concrete steps are:
(1) take raw material, Xylitol according to the ratio of following amount of substance: aniline: ammonium persulphate=1/6 ~ 1:1:1, wherein aniline is the aniline that 1mL has purified.
(2) Xylitol that step (1) takes is joined in the flask filling 30mL deionized water, after stirring at room temperature 0.5h, by flask transposition in ice-water bath, now, in flask, add aniline that step (1) takes and 10mL concentration is the hydrochloric acid soln of 1mol/L, under the condition of ice-water bath, stir 1h.
(3) ammonium persulphate that step (1) takes is dissolved in deionized water, obtained ammonium persulfate aqueous solution, then be dropwise added drop-wise in the obtained solution of step (2), under the condition of ice-water bath, stir 12h, after question response terminates, with deionized water reactant is washed, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, and grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
The inventive method preparation process is simple, environmental protection, reliable, raw material sources are extensive, with low cost, are applicable to suitability for industrialized production.The inventive method utilizes hydroxyls a large amount of in xylitol molecules and aniline molecule to form hydrogen bond to prepare the electrically conductive polyaniline with nano tubular structure, nano tubular structure can be the diffusion of electrolyte ion and mobile provides good passage, ion is enable fully redox reaction to occur with electrode materials, increase the ratio capacitance of material, reduce internal resistance, thus obtain the nano tubular structure polyaniline with good electrical chemical property, the polyaniline nanotube prepared of the inventive method is than the resistance to high-rate performance not using the polyaniline of Template preparation to have high specific capacitance to become reconciled, it is a kind of desirable electrode material for super capacitor.
Accompanying drawing explanation
Fig. 1 is the cyclic voltammetry curve figure of Preparation of conductive polyaniline nanotubes under different scanning speed prepared by the embodiment of the present invention 4.
Fig. 2 is the constant current charge-discharge graphic representation of Preparation of conductive polyaniline nanotubes under different current density that the embodiment of the present invention 4 obtains.
Embodiment
embodiment 1:
(1) take the Xylitol (Xylitol is 1:6 with the ratio of the amount of substance of aniline) of 0.278g, join in the flask filling 30mL deionized water, after stirring at room temperature 0.5h, by flask transposition in ice-water bath.Now, add to flask aniline that 1mL purified and 10mL concentration is the hydrochloric acid soln of 1mol/L, under the condition of ice-water bath, stir 1h.
(2) a certain amount of ammonium persulphate is dissolved in deionized water, obtained ammonium persulfate aqueous solution (ammonium persulphate is 1 with the ratio of the amount of substance of aniline), then be dropwise added drop-wise in the obtained solution of step (1), under the condition of ice-water bath, stir 12h, after question response terminates, with deionized water reactant is washed, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, and grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
embodiment 2:
(1) take the Xylitol (Xylitol is 1:5 with the ratio of the amount of substance of aniline) of 0.334g, join in the flask filling 30mL deionized water, after stirring at room temperature 0.5h, by flask transposition in ice-water bath.Now, add to flask aniline that 1mL purified and 10mL concentration is the hydrochloric acid soln of 1mol/L, under the condition of ice-water bath, stir 1h.
(2) a certain amount of ammonium persulphate is dissolved in deionized water, obtained ammonium persulfate aqueous solution (ammonium persulphate is 1 with the ratio of the amount of substance of aniline), then be dropwise added drop-wise in the obtained solution of step (1), under the condition of ice-water bath, stir 12h, after question response terminates, with deionized water reactant is washed, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, and grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
embodiment 3:
(1) take the Xylitol (Xylitol is 1:3 with the ratio of the amount of substance of aniline) of 0.556g, join in the flask filling 30mL deionized water, after stirring at room temperature 0.5h, by flask transposition in ice-water bath.Now, add to flask aniline that 1mL purified and 10mL concentration is the hydrochloric acid soln of 1mol/L, under the condition of ice-water bath, stir 1h.
(2) a certain amount of ammonium persulphate is dissolved in deionized water, obtained ammonium persulfate aqueous solution (ammonium persulphate is 1 with the ratio of the amount of substance of aniline), then be dropwise added drop-wise in the obtained solution of step (1), under the condition of ice-water bath, stir 12h, after question response terminates, with deionized water reactant is washed, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, and grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
embodiment 4:
(1) take the Xylitol (Xylitol is 1:2 with the ratio of the amount of substance of aniline) of 0.835g, join in the flask filling 30mL deionized water, after stirring at room temperature 0.5h, by flask transposition in ice-water bath.Now, add to flask aniline that 1mL purified and 10mL concentration is the hydrochloric acid soln of 1mol/L, under the condition of ice-water bath, stir 1h.
(2) a certain amount of ammonium persulphate is dissolved in deionized water, obtained ammonium persulfate aqueous solution (ammonium persulphate is 1 with the ratio of the amount of substance of aniline), then be dropwise added drop-wise in the obtained solution of step (1), under the condition of ice-water bath, stir 12h, after question response terminates, with deionized water reactant is washed, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, and grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
embodiment 5:
(1) take the Xylitol (Xylitol is 3:5 with the ratio of the amount of substance of aniline) of 1.001g, join in the flask filling 30mL deionized water, after stirring at room temperature 0.5h, by flask transposition in ice-water bath.Now, add to flask aniline that 1mL purified and 10mL concentration is the hydrochloric acid soln of 1mol/L, under the condition of ice-water bath, stir 1h.
(2) a certain amount of ammonium persulphate is dissolved in deionized water, obtained ammonium persulfate aqueous solution (ammonium persulphate is 1 with the ratio of the amount of substance of aniline), then be dropwise added drop-wise in the obtained solution of step (1), under the condition of ice-water bath, stir 12h, after question response terminates, with deionized water reactant is washed, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, and grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
embodiment 6:
(1) take the Xylitol (Xylitol is 1:1 with the ratio of the amount of substance of aniline) of 1.669g, join in the flask filling 30mL deionized water, after stirring at room temperature 0.5h, by flask transposition in ice-water bath.Now, add to flask aniline that 1mL purified and 10mL concentration is the hydrochloric acid soln of 1mol/L, under the condition of ice-water bath, stir 1h.
(2) a certain amount of ammonium persulphate is dissolved in deionized water, obtained ammonium persulfate aqueous solution (ammonium persulphate is 1 with the ratio of the amount of substance of aniline), then be dropwise added drop-wise in the obtained solution of step (1), under the condition of ice-water bath, stir 12h, after question response terminates, with deionized water reactant is washed, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, and grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
Claims (1)
1. be a method for Template preparation Preparation of conductive polyaniline nanotubes with Xylitol, it is characterized in that concrete steps are:
(1) take raw material, Xylitol according to the ratio of following amount of substance: aniline: ammonium persulphate=1/6 ~ 1:1:1, wherein aniline is the aniline that 1mL has purified;
(2) Xylitol that step (1) takes is joined in the flask filling 30mL deionized water, after stirring at room temperature 0.5h, by flask transposition in ice-water bath, now, in flask, add aniline that step (1) takes and 10mL concentration is the hydrochloric acid soln of 1mol/L, under the condition of ice-water bath, stir 1h;
(3) ammonium persulphate that step (1) takes is dissolved in deionized water, obtained ammonium persulfate aqueous solution, then be dropwise added drop-wise in the obtained solution of step (2), under the condition of ice-water bath, stir 12h, after question response terminates, with deionized water reactant is washed, suction filtration, until filtrate is in neutral, gained filter cake is dry 24h in the vacuum drying oven of 50 DEG C, and grinding is collected, i.e. obtained Preparation of conductive polyaniline nanotubes.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103282457A (en) * | 2010-11-19 | 2013-09-04 | 汉高公司 | Adhesive compositions and use thereof |
| CN104119530A (en) * | 2014-08-02 | 2014-10-29 | 桂林理工大学 | Method for preparing conducting polyaniline nanotube |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103282457A (en) * | 2010-11-19 | 2013-09-04 | 汉高公司 | Adhesive compositions and use thereof |
| CN104119530A (en) * | 2014-08-02 | 2014-10-29 | 桂林理工大学 | Method for preparing conducting polyaniline nanotube |
Non-Patent Citations (1)
| Title |
|---|
| 王学智等: "模板法合成聚苯胺的研究进展", 《材料导报》 * |
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Application publication date: 20151209 |