CN101113199A - Method for preparing polyaniline nano thread - Google Patents
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Abstract
A preparation method of polyaniline nanometer line relates to a polymeric material, supplying a preparation method of polyaniline nanometer line based on the polymerization on suspended interface, the method is of gentle reaction conditions, high efficiency, and suitable for industrial production. A acidic aqueous solution containing 1mol/L hydrion concentration is added into a container to do external phase before water soluble dispersing agent is fed into and the water soluble dispersing agent concentration is 1 to 2 g/L in the terminal system; organic solution containing 0.1 to 1 mol/L aniline monomer is added into the acidic aqueous solution, then an acidic aqueous solution with the same mole of oxidant as aniline is added into the aqueous solution under the reaction temperature from 0 DEG C to room temperature, and the volume ration between organic phase and the acidic aqueous solution is 1/20 to 1/5; the product is filtrated after 2 to 48 hours of reaction, then the filtration is washed to neutral by distilled water, and washed with alcohol until the filtration is colorless and transparent; the product is baked under 40 to 60 DEG C, finally the polyaniline nanometer line with diameters between 40 to 90 nm is acquired.
Description
Technical field
The present invention relates to a kind of polymer materials, especially relate to a kind of preparation method of conductive polyaniline nano-wire.
Background technology
Because electrically conductive polyaniline has excellent environmental stability, thermostability and doping reversibility, and is easy to synthesize, therefore become one of conductive polymers (the Zhang D.H. of tool commercial application prospect, Wang Y.Y., MAT.SCI.E.B, 2006,134 (1): 9-19).Because the polyaniline nano material has the structure of nanoscale, thereby has possessed unexistent small-size effect of conventional conductive polymerization and quantum effect etc., gives its special physicals and chemical property.For example utilize the polyaniline nano-line of comparing the bigger specific surface that has with traditional polyaniline, high tens of times of (the Virji S. of its remolding sensitivity traditional sensors of the sensor material of making to ammonia in the environment, Huang J., Kaner R.B., Weiller B.H., NANO LETT., 2004,4 (3): 491-496).Polyaniline nano-line is dispersed among the PMMA,, can prepares transparent electrically-conductive film (Wang Y.Y, JingX.L.MAT.SCI.E.B, 2007,138 (1): 95-100) by evaporating film forming way.Utilize the electric transmission effect between polyaniline nano-line and the gold nano grain, can be used as (the Tseng R.J. such as element of memory for digits, Baker C.O., Shedd B., Huang J.X., KanerR.B., Ouyang J.Y., Yang Y., APPL.PHYS.LETT.2007,90 (5): 053101/1-053101/3).Along with the research of nano polyaniline deepened continuously a synthetic important research direction that has become conducting polymer materials of polyaniline nano-line.
The common method of synthesized polyaniline nano wire has following several at present:
1. template: template can be divided into " hard template " and " soft template " method, Martin (Martin C.R., Chem.Mater.1996,8 (8): 1739-1746) utilize porous-film, (Wu C.G., Bein T. such as Wu, Science 1994,264 1757-1759) utilize the porous zeolite to be the template synthesized polyaniline, template is removed can be obtained polyaniline nano-line again, this method is commonly referred to hard template method.Its advantage is that controllability is strong, can control the radius of the polyaniline nano-line of gained by the aperture of control template, and this is that additive method hardly matches; Shortcoming is exactly that preparation process is numerous and diverse, the cost height of template.Utilization adds additives such as tensio-active agent in reaction system, make aniline monomer polymerization in the microstructure that additive forms, and the method that forms micrometer/nanometer structure polyaniline is called soft template method.(Jang J.S., Yoon H.S., ADV.MATER. such as Jang for example, 2003,15 (24): 2088-2091) FeCl3 is joined in surfactant A OT and the isooctyl alcohol, utilize iron ion to reduce the characteristics of micelle-forming concentration, make the spontaneous formation columnar structure of AOT.Polyaniline polymerization and obtain polyaniline nano-line in these column micellas.The advantage of soft template method is a mild condition, prepares easy; Shortcoming is that the additive capacity that usually needs is big, consumption even greater than the amount of product, and cost is higher.
2. electrochemical process: obtain the method for polyaniline nano structure thereby electrochemical process is the various factors of control electrochemical reaction, as (Liang L. such as Liang, Liu J., Windisch C.F., Exarhos G.J., Lin Y.H., Angew.Chem.Int.Ed., 2002,41 (19): 3665-3668) utilize three steps control electric current, at 0.08mAcm
-2Current density under nucleation, reduce current density then to 0.04mAcm
-2, arrive 0.02mAcm at last
-2, utilize the nano polyaniline nuclear be deposited on the electrode, under less current density, form unified towards polyaniline nano-line.The advantage of electrochemical process is that controllability is better; Shortcoming is that output is lower, and Test Condition Requirements is higher, is not suitable for scale operation.
3. interfacial polymerization: interfacial polymerization is to utilize oxygenant and aniline monomer are dissolved in respectively in two kinds of immiscible media, make the polymerization of polyaniline occur in (Huang J. on the phase interface after again two media being mixed, Virji S., Weiller B.H., Kaner R.B., J.Am.Chem.Soc.2003,125 (2): 314-315).This is a kind of novel method, and the advantage of this method is to form the water-fast organic solvent at interface except using with water, need not add other auxiliary agents usually, and cost is low than additive method, and the polyaniline nano-line of preparation homogeneous comparatively; Shortcoming is that the organic solvent amount of this method use is very big, and monomeric concentration is lower.
Summary of the invention
Purpose of the present invention aims to provide a kind of reaction conditions gentleness, efficient height, the method for preparing polyaniline nano-line based on the suspended state interfacial polymerization of suitable suitability for industrialized production.
Concrete steps of the present invention are as follows:
1) adding hydrogen ion concentration in reaction vessel is that the acidic aqueous solution of 1mol/L is done external phase, adds water soluble dispersing agent again, and wherein the concentration of dispersant concentration in final system is 1～2g/L;
2) will contain the organic solution of 0.1～1mol/L aniline monomer, under agitation join in the acidic aqueous solution, add the acidic aqueous solution that contains with the equimolar oxygenant of aniline then, in this reaction system, temperature of reaction is 0 ℃ and arrives room temperature that the volume ratio of organic phase and acidic aqueous solution is 1/20～1/5;
3) behind reaction 2～48h,, be neutral, till continuing to be washed till filtrate and to be water white transparency, product can be obtained the polyaniline nano-line of diameter between 40～90nm 40～60 ℃ of following oven dry with ethanol with distilled water flushing to filtrate with the product suction filtration.
Described water soluble dispersing agent is polyvinyl alcohol, polyvinylpyrrolidone or sodium polyacrylate etc.Preparing the used solvent of described organic solution is tetracol phenixin, 1,2-ethylene dichloride, hexanaphthene or toluene etc.Described oxygenant is ammonium persulphate, hydrogen peroxide, potassium bichromate or iron(ic) chloride etc.Described acidic aqueous solution is a hydrochloric acid, the aqueous solution of sulfuric acid or perchloric acid, and described acidic aqueous solution is with a kind of aqueous acid, and hydrogen ion concentration is 1mol/L.
In step 3), the time of described reaction is preferably 4～24h.
The present invention has gathered interfacial polymerization can access more regular polyaniline nano-line, and the big characteristics of suspension polymerization specific surface area, is that a kind of efficient is higher, is more suitable for the method for suitability for industrialized production polyaniline nano-line; Its characteristics are: the specific surface of (1) polyaniline nano-line obtains increasing by the method for organic phase dispersant liquid drop that suspends, and has shortened the time of reacting required; (2) water/organic phase interface is subjected to the effect of shearing force, is in the state of continuous motion, has reduced the probability that nano wire is reunited, make the consumption of organic solvent greatly reduce, even only need 1/20 of water, and can make the polyaniline nano-line of homogeneous, reduce environmental pollution and cost consumption; (3) reaction conditions gentleness ℃ can prepare the polyaniline nano-line of rule in room temperature to 0.
Description of drawings
Fig. 1 is the SEM photo of the polyaniline nano-line of embodiment 1 preparation.
Fig. 2 is the XRD spectra of the polyaniline nano-line of embodiment 1 preparation.In Fig. 2, X-coordinate is 2 Θ/degree.
Fig. 3 is the FTIR spectrogram of the polyaniline nano-line of embodiment 1 preparation.In Fig. 3, X-coordinate is wave number Wavenumber/cm
-1
Specific implementation method
The invention will be further described below by embodiment.
Embodiment 1:1, in three-necked flask, add the aqueous hydrochloric acid 90ml of 1mol/L and dissolving is good in advance massfraction is 10% polyvinyl alcohol solution 2g, stir 20min.2, with aniline monomer 0.96g under condition of ice bath, be added in the 5ml tetracol phenixin to stir and make it to become uniform solution.3, the carbon tetrachloride solution with aniline under agitation drips to the aqueous phase that step 1 is prepared with dropping funnel, and solution drips off in 20min, is reflected in the ice bath to carry out; 4, the 2.28g ammonium persulphate is added to 10ml, concentration is in the aqueous hydrochloric acid of 1mol/L, wiring solution-forming.And this drips of solution is added in the solution of step 3, this oxidizing agent solution adds in 40min; 5, behind the reaction 4h, with the product suction filtration.It is neutral being washed till filtrate with distilled water, till continuing to be washed till filtrate and to be water white transparency with alcohol.6, product can be obtained the polyaniline nano-line of diameter between 40～90nm 50 ℃ of oven dry.
In Fig. 1, the SEM photo of polyaniline nano-line shows that nanowire diameter is between 50～80nm, from the XRD spectra of Fig. 2 polyaniline nano-line, see a series of peaks between 18～26 ° be respectively the polyaniline crystallization in the reaction in crystal orientation of vertical and parallel polyaniline molecule chain, this result shows to compare with the polyaniline of traditional method preparation higher degree of crystallinity.1590cm in the FTIR spectrogram of Fig. 3
-1, 1499cm
-1The respectively absorption peak of corresponding quinoid structure (N=Q=N) and the charateristic avsorption band of benzene formula structure (N-B-N), 1310 and 1245cm
-1Be that aromatic amine Ar-N absorbs; 830cm
-1And 1135cm
-1The peak is respectively the outer and in-plane bending vibration characteristic absorption band of the face of contraposition phenyl ring, and these key bands have confirmed that synthetic is a polyaniline.
Embodiment 2:1, add the aqueous hydrochloric acid 90ml of 1mol/L in three-necked flask, adding the massfraction that dissolving is good in advance is 5% polyvinylpyrrolidonesolution solution 2g, stirs 20min.2, with aniline monomer 0.96g under condition of ice bath, be added in the 5ml tetracol phenixin, stir and to make it to become uniform solution.3, with the carbon tetrachloride solution dropping funnel of aniline in the step 2, under agitation be added drop-wise to step 1 aqueous phase, solution drips in 20min, is reflected in the ice bath and carries out; 4, the 2.28g potassium bichromate is joined 10ml, concentration is in the aqueous hydrochloric acid of 1mol/L, wiring solution-forming.And this drips of solution is added in the solution of step 3, this oxidizing agent solution adds in 40min; 5, behind the reaction 8h, with the product suction filtration.It is neutral being washed till filtrate with distilled water, till continuing to be washed till filtrate and to be water white transparency with alcohol.6, product can be obtained polyaniline nano-line 40 ℃ of oven dry.
Embodiment 3:1, add the aqueous sulfuric acid 90mi of 1mol/L in three-necked flask, adding the massfraction that dissolving is good in advance is 10% polyvinyl alcohol solution 2g, vigorous stirring 20min.2, with aniline monomer 0.96g under the condition of ice bath, join in the 5ml hexanaphthene, stir and to make it to become uniform solution.3, with the cyclohexane solution dropping funnel of aniline in the step 2, under agitation be added drop-wise to aqueous phase, solution drips in 20min, and reaction process is carried out in ice bath; 4, the 2.28g ammonium persulphate is joined 10ml, concentration is in the aqueous sulfuric acid of 1mol/L, wiring solution-forming.And this drips of solution is added in the solution of step 3, this oxidizing agent solution adds in 40min; 5, after the reaction 24h, with the product suction filtration.It is neutral being washed till filtrate with distilled water, till continuing to be washed till filtrate and to be water white transparency with alcohol.6, product can be obtained polyaniline nano-line 50 ℃ of oven dry.
Embodiment 4: add the aqueous hydrochloric acid 90ml of 1mol/L in three-necked flask, good massfraction is 10% polyvinyl alcohol solution 2g to add dissolving in advance, vigorous stirring 20min.Aniline monomer 0.96g under the condition of ice bath, is joined 10ml1, in the 2-ethylene dichloride, stir and make it to become uniform solution.With 1 of aniline, 2-dichloroethane solution dropping funnel under agitation is added drop-wise to aqueous phase, and solution drips in 20min; With the 2.28g ammonium persulphate join 10ml, concentration is in the aqueous hydrochloric acid of 1mol/L, wiring solution-forming, and this drips of solution is added in the above-mentioned solution, this oxidizing agent solution at room temperature adds in the 40min; After the reaction 24h, with the product suction filtration.It is neutral being washed till filtrate with distilled water, till continuing to be washed till filtrate and to be water white transparency with alcohol.Product can be obtained polyaniline nano-line 50 ℃ of oven dry.
Embodiment 5:1, add the aqueous hydrochloric acid 90ml of 1mol/L in three-necked flask, adding the massfraction that dissolving is good in advance is 10% polyvinyl alcohol solution 2g, vigorous stirring 20min.2, with aniline monomer 0.96g under the condition of ice bath, join in the 20ml toluene, stir and to make it to become uniform solution.3, with the toluene solution dropping funnel of aniline in the step 2, under agitation be added drop-wise to aqueous phase, solution drips in 20min.4, the 2.28g ammonium persulphate is joined 10ml, concentration is in the aqueous hydrochloric acid of 1mol/L, wiring solution-forming.And this drips of solution is added in the solution of step 3, this oxidizing agent solution at room temperature adds in the 40min.5, after the reaction 2h, with the product suction filtration.It is neutral being washed till filtrate with distilled water, till continuing to be washed till filtrate and to be water white transparency with alcohol.6, product can be obtained polyaniline nano-line 50 ℃ of oven dry.
Embodiment 6: identical with the reactions steps of embodiment 5, only replace polyvinyl alcohol with 5% polyvinylpyrrolidonesolution solution, and replace ammonium persulphate as oxygenant with potassium bichromate.After reaction finishes with product 60 ℃ of oven dry get final product polyaniline nano-line.
Embodiment 7:1, add the aqueous sulfuric acid 90ml of 1mol/L in three-necked flask, adding the massfraction that dissolving is good in advance is 5% polyvinylpyrrolidonesolution solution 2g, vigorous stirring 20min.2, with aniline monomer 0.96g under the condition of ice bath, join in the 20ml toluene, stir and to make it to become uniform solution.3, with the toluene solution dropping funnel of aniline in the step 2, under agitation be added drop-wise to aqueous phase, solution drips in 20min.4, with H
2O
2/ FeCl
2((m[H wherein
2O
2]/m[FeCl
2]=500: 1, H
2O
2With moles such as aniline) join 10ml, concentration is in the aqueous sulfuric acid of 1mol/L, wiring solution-forming.And this drips of solution is added in the solution of step 3, this oxidizing agent solution at room temperature adds in the 40min.5, after the reaction 48h, with the product suction filtration.It is neutral being washed till filtrate with distilled water, till continuing to be washed till filtrate and to be water white transparency with alcohol.6, product can be obtained polyaniline nano-line 50 ℃ of oven dry.
Embodiment 8: with the reactions steps among the embodiment 1, dispersion agent replaces polyvinyl alcohol with 10% sodium polyacrylate solution, and acidic aqueous solution replaces hydrochloric acid with perchloric acid.Oxygenant replaces ammonium persulphate with FeCl3, after 20 hours reaction times product can be obtained polyaniline nano-line 60 ℃ of oven dry.
Claims (6)
1. a method for preparing polyaniline nano-line is characterized in that the steps include:
1) adding hydrogen ion concentration in reaction vessel is that the acidic aqueous solution of 1mol/L is done external phase, adds water soluble dispersing agent again, and wherein the concentration of dispersant concentration in final system is 1～2g/L;
2) will contain the organic solution of 0.1～1mol/L aniline monomer, under agitation join in the acidic aqueous solution, add the acidic aqueous solution that contains with the equimolar oxygenant of aniline then, in this reaction system, temperature of reaction is 0 ℃ and arrives room temperature that the volume ratio of organic phase and acidic aqueous solution is 1/20～1/5;
3) behind reaction 2～48h,, be neutral, till continuing to be washed till filtrate and to be water white transparency, product can be obtained the polyaniline nano-line of diameter between 40～90nm 40～60 ℃ of following oven dry with ethanol with distilled water flushing to filtrate with the product suction filtration.
2. a kind of method for preparing polyaniline nano-line as claimed in claim 1 is characterized in that described water soluble dispersing agent is polyvinyl alcohol, polyvinylpyrrolidone or sodium polyacrylate.
3. a kind of method for preparing polyaniline nano-line as claimed in claim 1, the used solvent of organic solution that it is characterized in that preparing aniline monomer is a tetracol phenixin, 1,2-ethylene dichloride, hexanaphthene or toluene.
4. a kind of method for preparing polyaniline nano-line as claimed in claim 1 is characterized in that described oxygenant is ammonium persulphate, hydrogen peroxide, potassium bichromate or iron(ic) chloride.
5. a kind of method for preparing polyaniline nano-line as claimed in claim 1 is characterized in that described acidic aqueous solution is that concentration is the hydrochloric acid of 1mol/L, the aqueous solution of sulfuric acid or perchloric acid.
6. a kind of method for preparing polyaniline nano-line as claimed in claim 1 is characterized in that in step 3) the time of described reaction is 4～24h.
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