CN101058417A - Electric polyaniline derivative surface modified water decentralized carbon nano-tube and preparation method - Google Patents
Electric polyaniline derivative surface modified water decentralized carbon nano-tube and preparation method Download PDFInfo
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Abstract
The invention discloses a water dispersing carbon nanometer pipe and making method of modified conductive polyaniline derivant surface, which is characterized by the following: dissolving the water-soluble phenylamine derivant monomer into inorganic acid solution; adding carbon nanometer pipe to be dispersed evenly through ultrasound; oxidizing and polymerizing to coat the water-soluble conductive phenylamine derivant on the carbon nanometer pipe surface evenly acted by oxidizer through original position chemistry; obtaining the product with simple and feasible method, strong controllability as well as good water dispersion and superior conductivity; fitting for making high-strength, antistatic and microwave-adsorbing material as mass transmitting and transferring carrier for special functional nanometer element and different systems; displaying wide applying prospect in the material science, nanometer technique and life science.
Description
Technical field
The present invention relates to a kind of water decentralized carbon nano-tube and preparation method thereof, particularly electric polyaniline derivative surface modified water decentralized carbon nano-tube and preparation method.
Background technology
Carbon nanotube (Carbon Nanotubes is called for short CNTs) is the hollow tube that is rolled into by the Graphene lamella that carbon atom forms.According to the quantity of its graphite flake layer, carbon nanotube be divided into Single Walled Carbon Nanotube (Single-wall Nanotube, SWNTs) and multi-walled carbon nano-tubes (Multi-wall Nanotube, MWNTs).
The structure uniqueness of carbon nanotube, performance are unusual, its theoretical tensile strength is 100 times of steel, and density only is 1/6 of steel, toughness is very high, electroconductibility is extremely strong, and field emission performance is good, and has good adsorption property, be called following " super fiber " by scientist, thereby caused that in the material field people greatly pay close attention to.Yet, since the growth characteristic of carbon nanotube to be many root balls poly-and tangle mutually, and surface characteristic and graphite-like are seemingly, cause having insolubility in organic solvent and water, difficult dispersiveness, this has limited its application at numerous areas greatly.From 1998, the surface treatment and the functionalization of carbon nanotube carried out [Science Vol.280,1253, (1998)] gradually.
In order to improve the dispersiveness of carbon nanotube in water, at present, the following technological method of main employing: (1) is that dispersion stabilizer carries out surface treatment [J.Colloid Interface Sci.Vol.260,89 (2003)] to carbon nanotube with the tensio-active agent; (2) surface grafting hydrophilic polymer [ZL200310121619.X]; (3) layer-by-layer pipe absocped with polyelectrolyte on surface [200610148005.4].Though aforesaid method has improved the water dispersible of carbon nanotube preferably, the carbon nano-tube conductive energy that reduces.Therefore, need provide a kind of new technology, overcome the defective that prior art exists.
Summary of the invention
The object of the present invention is to provide a kind of electric polyaniline derivative surface modified water decentralized carbon nano-tube and preparation method thereof, have the defective of low conductivity, satisfy the needs in different application field to overcome the carbon nanotube that prior art makes.
The objective of the invention is to be achieved through the following technical solutions:
By the supersound process technology carbon nanotube is dispersed in and is dissolved with in the monomeric aqueous solution of anils; Owing to exist π-πDian Zi effect between anils monomer and carbon nanotube, make the anils monomer be adsorbed on the carbon nano tube surface; Under the oxygenant effect, be adsorbed on the anils monomer generation in-situ oxidizing-polymerizing on the carbon nano tube surface, and on carbon nano tube surface, form the polyaniline derivative coating.Because polyaniline derivative contains-SO
3 -, one side has been improved the hydrophilicity of carbon nanotube, has increased the electrostatic repulsion between carbon nanotube on the other hand, thereby has obviously improved the dispersion stabilization of carbon nanotube in water.The surface-modified carbon nanotubes that makes is the system of two kinds of electrical conductor coexistences, and its current carrier is easily by carbon nanotube or the transmission of electric polyaniline derivative main chain, so its electroconductibility also is enhanced.
Of the present invention being achieved through the following technical solutions:
A kind of electric polyaniline derivative surface modified water decentralized carbon nano-tube, it is characterized in that, described carbon nano tube modified, its surperficial electric polyaniline derivative content is 3～60% of its total mass, wherein, a kind of in poly-ORTHO AMINO PHENOL SULPHONIC, poly-m-sulfanilic acid, the poly-N-propane sulfonic acid base aniline of said polyaniline derivative.
The present invention also provides its preparation method as follows:
The water-soluble anils monomer of 0.1-10wt% is dissolved in the inorganic acid aqueous solution of 0.1-3mol/L, carbon nanotube is joined in the above-mentioned aqueous solution again, through ultrasonication 0.5～2 hour, even carbon nanotube is disperseed, the slow then dropping oxidizing agent aqueous solution, 0-40 ℃ of down reaction 6～48 hours, after filtration, after the washing, drying, obtain electric polyaniline derivative surface modified water decentralized carbon nano-tube.
Wherein: the mass ratio of described water-soluble anils monomer and carbon nanotube is 0.1～5: 1; The mol ratio of water-soluble anils monomer and oxygenant is 0.5～2: 1;
Described water-soluble anils monomer is a kind of in ORTHO AMINO PHENOL SULPHONIC, m-sulfanilic acid, the N-propane sulfonic acid base aniline;
Described mineral acid is a kind of in hydrochloric acid, sulfuric acid, perchloric acid and the phosphoric acid;
Described oxygenant is a kind of in ammonium persulphate, Potassium Persulphate, Potcrate and the iron trichloride.
Compare with existing surface modification of carbon nanotube technology, the present invention has following advantage:
(1) preparation technology is simple, and polymeric coating is controlled easily; (2) the electric polyaniline derivative surface modified carbon nanotube that makes had both had good water dispersible, had excellent electroconductibility again; (3) the preparation process environmental pollution is little.
Description of drawings
Fig. 1. the infrared spectrogram of poly-ORTHO AMINO PHENOL SULPHONIC surface-modified carbon nanotubes
Fig. 2. the high-resolution-ration transmission electric-lens photo of poly-ORTHO AMINO PHENOL SULPHONIC surface-modified carbon nanotubes
Embodiment:
Following embodiment is that the invention will be further described, rather than limits protection scope of the present invention.
Embodiment 1
The ORTHO AMINO PHENOL SULPHONIC monomer of 1g is dissolved in the aqueous hydrochloric acid of 1mol/L, again 1g multi-walled carbon nano-tubes (its diameter is 10-20nm) is joined in the above-mentioned aqueous solution,, even carbon nanotube is disperseed through ultrasonication 2 hours; Get the 1.3g ammonium persulphate, be made into 10mL solution with deionized water, the mol ratio of control ORTHO AMINO PHENOL SULPHONIC and ammonium persulphate is 1: 1, then ammonium persulfate aqueous solution slowly is added drop-wise in the above-mentioned reaction system, reacted 24 hours down at 25 ℃, after filtration, after the washing, drying, obtain conducting electricity the water decentralized carbon nano-tube of poly-ORTHO AMINO PHENOL SULPHONIC surface modification.By ultimate analysis, determine that the poly-ORTHO AMINO PHENOL SULPHONIC content of modified carbon nano tube tube-surface is 36.8wt%.
Fig. 1 has provided the infrared analysis result of poly-ORTHO AMINO PHENOL SULPHONIC surface-modified carbon nanotubes, 1562cm
-1And 1082cm
-1Place's absorption peak is the characteristic peak of poly-ORTHO AMINO PHENOL SULPHONIC, has proved that poly-ORTHO AMINO PHENOL SULPHONIC exists.Fig. 2 has provided high-resolution-ration transmission electric-lens (HRTEM) photo, and as can be seen, the surface of modified carbon nano-tube presents dark and the poly-uniformly ORTHO AMINO PHENOL SULPHONIC layer of thickness, and thickness is about 4nm.
Sample is pressed into the disk that diameter is 13mm, with four point probe instrument testing conductivity, the result is as follows: the specific conductivity of unmodified carbon nanotube is 4.7S/cm, and poly-ORTHO AMINO PHENOL SULPHONIC surface-modified carbon nanotubes specific conductivity is 19.5S/cm, this shows carbon nanotube after poly-ORTHO AMINO PHENOL SULPHONIC surface modification, and its specific conductivity is improved to some extent.
Water-dispersion stability adopts sedimentation experiment to estimate, and test result is as follows: unmodified carbon nanotube through ultra-sonic dispersion evenly after, sedimentation fully after 3 hours; And poly-ORTHO AMINO PHENOL SULPHONIC surface-modified carbon nanotubes can keep not sedimentation more than 500 hours.This shows carbon nanotube after poly-ORTHO AMINO PHENOL SULPHONIC surface modification, and its water-dispersion stability is improved greatly.
Embodiment 2
The ORTHO AMINO PHENOL SULPHONIC monomer of 0.1g is dissolved in the aqueous hydrochloric acid of 3mol/L, again 1g multi-walled carbon nano-tubes (its diameter is 10-20nm) is joined in the above-mentioned aqueous solution,, even carbon nanotube is disperseed through ultrasonication 1 hour; Get the 0.26g ammonium persulphate, be made into 5mL solution with deionized water, the mol ratio of control ORTHO AMINO PHENOL SULPHONIC and ammonium persulphate is 1: 2, then ammonium persulfate aqueous solution slowly is added drop-wise in the above-mentioned reaction system, reacted 48 hours down at 25 ℃, after filtration, after the washing, drying, obtain conducting electricity the water decentralized carbon nano-tube of poly-ORTHO AMINO PHENOL SULPHONIC surface modification.By ultimate analysis, determine that the poly-ORTHO AMINO PHENOL SULPHONIC content of modified carbon nano tube tube-surface is 4.2wt%.
Testing its specific conductivity with the four point probe instrument is 10.2S/cm.
Adopt sedimentation experiment to estimate water-dispersion stability, the result shows that this poly-ORTHO AMINO PHENOL SULPHONIC surface-modified carbon nanotubes keeps not precipitating more than 24 hours.
Embodiment 3
The ORTHO AMINO PHENOL SULPHONIC monomer of 5g is dissolved in the aqueous hydrochloric acid of 2mol/L, again 1g multi-walled carbon nano-tubes (its diameter is 10-20nm) is joined in the above-mentioned aqueous solution,, even carbon nanotube is disperseed through ultrasonication 1 hour; Get the 6.5g ammonium persulphate, be made into 50mL solution with deionized water, the mol ratio of control ORTHO AMINO PHENOL SULPHONIC and ammonium persulphate is 1: 1, then ammonium persulfate aqueous solution slowly is added drop-wise in the above-mentioned reaction system, reacted 24 hours down at 25 ℃, after filtration, after the washing, drying, obtain conducting electricity the water decentralized carbon nano-tube of poly-ORTHO AMINO PHENOL SULPHONIC surface modification.By ultimate analysis, determine that the poly-ORTHO AMINO PHENOL SULPHONIC content of modified carbon nano tube tube-surface is 56.2wt%.
Testing its specific conductivity with the four point probe instrument is 16.2S/cm.
Adopt sedimentation experiment to estimate water-dispersion stability, the result shows that this poly-ORTHO AMINO PHENOL SULPHONIC surface-modified carbon nanotubes keeps not precipitating more than 500 hours.
Embodiment 4
The ORTHO AMINO PHENOL SULPHONIC monomer of 5g is dissolved in the aqueous sulfuric acid of 0.2mol/L, again 1g Single Walled Carbon Nanotube (its diameter is 1-2nm) is joined in the above-mentioned aqueous solution,, even carbon nanotube is disperseed through ultrasonication 2 hours; Get the 3.9g Potassium Persulphate, be made into 50mL solution with deionized water, the mol ratio of control ORTHO AMINO PHENOL SULPHONIC and Potassium Persulphate is 1: 0.5, then persulfate aqueous solution slowly is added drop-wise in the above-mentioned reaction system, reacted 24 hours down at 25 ℃, after filtration, after the washing, drying, obtain conducting electricity the water decentralized carbon nano-tube of poly-ORTHO AMINO PHENOL SULPHONIC surface modification.By ultimate analysis, determine that the poly-ORTHO AMINO PHENOL SULPHONIC content of modified carbon nano tube tube-surface is 28.5wt%.
Testing its specific conductivity with the four point probe instrument is 20.6S/cm.
Adopt sedimentation experiment to estimate water-dispersion stability, the result shows that this poly-ORTHO AMINO PHENOL SULPHONIC surface-modified carbon nanotubes keeps not precipitating more than 500 hours.
Embodiment 5
The ORTHO AMINO PHENOL SULPHONIC monomer of 0.5g is dissolved among the high chloro acid solution of 1mol/L, again 1g multi-walled carbon nano-tubes (its diameter is 10-20nm) is joined in the above-mentioned aqueous solution,, even carbon nanotube is disperseed through ultrasonication 0.5 hour; Get 0.36g Potcrate, be made into 10mL solution with deionized water, the mol ratio of control ORTHO AMINO PHENOL SULPHONIC and Potcrate is 1: 1, then the Potcrate aqueous solution slowly is added drop-wise in the above-mentioned reaction system, reacted 6 hours down at 40 ℃, after filtration, after the washing, drying, obtain conducting electricity the water decentralized carbon nano-tube of poly-ORTHO AMINO PHENOL SULPHONIC surface modification.By ultimate analysis, determine that the poly-ORTHO AMINO PHENOL SULPHONIC content of modified carbon nano tube tube-surface is 26.6wt%.
Testing its specific conductivity with the four point probe instrument is 12.3S/cm.
Adopt sedimentation experiment to estimate water-dispersion stability, the result shows that this poly-ORTHO AMINO PHENOL SULPHONIC surface-modified carbon nanotubes keeps not precipitating more than 500 hours.
Embodiment 6
The ORTHO AMINO PHENOL SULPHONIC monomer of 0.5g is dissolved in the phosphate aqueous solution of 2mol/L, again 1g multi-walled carbon nano-tubes (its diameter is 10-20nm) is joined in the above-mentioned aqueous solution,, even carbon nanotube is disperseed through ultrasonication 1 hour; Get the 0.47g iron trichloride, be made into 10mL solution with deionized water, the mol ratio of control ORTHO AMINO PHENOL SULPHONIC and iron trichloride is 1: 1, then ferric chloride aqueous solutions slowly is added drop-wise in the above-mentioned reaction system, reacted 24 hours down at 25 ℃, after filtration, after the washing, drying, obtain conducting electricity the water decentralized carbon nano-tube of poly-ORTHO AMINO PHENOL SULPHONIC surface modification.By ultimate analysis, determine that the poly-ORTHO AMINO PHENOL SULPHONIC content of modified carbon nano tube tube-surface is 22.7wt%.
Testing its specific conductivity with the four point probe instrument is 11.5S/cm.
Adopt sedimentation experiment to estimate water-dispersion stability, the result shows that this poly-ORTHO AMINO PHENOL SULPHONIC surface-modified carbon nanotubes keeps not precipitating more than 500 hours.
Embodiment 7
The m-sulfanilic acid monomer of 1g is dissolved in the aqueous hydrochloric acid of 1mol/L, again 1g multi-walled carbon nano-tubes (its diameter is 10-20nm) is joined in the above-mentioned aqueous solution,, even carbon nanotube is disperseed through ultrasonication 2 hours; Get the 1.3g ammonium persulphate, be made into 10mL solution with deionized water, the mol ratio of control m-sulfanilic acid and ammonium persulphate is 1: 1, then ammonium persulfate aqueous solution slowly is added drop-wise in the above-mentioned reaction system, reacted 48 hours down at 25 ℃, after filtration, after the washing, drying, the water decentralized carbon nano-tube of poly-aniline sulfonic acid surface modification between obtaining conducting electricity.By ultimate analysis, determine that the poly-m-sulfanilic acid content of modified carbon nano tube tube-surface is 12.6wt%.
Testing its specific conductivity with the four point probe instrument is 13.1S/cm.
Adopt sedimentation experiment to estimate water-dispersion stability, the result shows that this poly-m-sulfanilic acid surface-modified carbon nanotubes keeps not precipitating more than 500 hours.
Embodiment 8
The N-propane sulfonic acid base aniline monomer of 1.2g is dissolved in the aqueous hydrochloric acid of 1mol/L, again 1g multi-walled carbon nano-tubes (its diameter is 10-20nm) is joined in the above-mentioned aqueous solution,, even carbon nanotube is disperseed through ultrasonication 2 hours; Get the 1.27g ammonium persulphate, be made into 10mL solution with deionized water, the mol ratio of control N-propane sulfonic acid base aniline and ammonium persulphate is 1: 1, then ammonium persulfate aqueous solution slowly is added drop-wise in the above-mentioned reaction system, reacted 24 hours down at 25 ℃, after filtration, after the washing, drying, obtain conducting electricity the water decentralized carbon nano-tube of poly-N-propane sulfonic acid base aniline surface modification.By ultimate analysis, determine that the poly-N-propane sulfonic acid base aniline content of modified carbon nano tube tube-surface is 24.8wt%.
Testing its specific conductivity with the four point probe instrument is 14.8S/cm.
Adopt sedimentation experiment to estimate water-dispersion stability, the result shows that this poly-N-propane sulfonic acid base aniline surface-modified carbon nanotubes keeps not precipitating more than 500 hours.
Claims (2)
1, a kind of electric polyaniline derivative surface modified water decentralized carbon nano-tube, it is characterized in that, described carbon nano tube modified, its surperficial electric polyaniline derivative content is 3～60% of its total mass, wherein, a kind of in poly-ORTHO AMINO PHENOL SULPHONIC, poly-m-sulfanilic acid, the poly-N-propane sulfonic acid base aniline of said polyaniline derivative.
2, a kind of preparation method of electric polyaniline derivative surface modified water decentralized carbon nano-tube, it is characterized in that, said method comprising the steps of: the water-soluble anils monomer of 0.1-10wt% is dissolved in the inorganic acid aqueous solution of 0.1-3mol/L, carbon nanotube is joined in the above-mentioned aqueous solution again, through ultrasonication 0.5～2 hour, even carbon nanotube is disperseed, the slow then dropping oxidizing agent aqueous solution, reacted 6～48 hours down at 0-40 ℃, after filtration, washing, after the drying, obtain electric polyaniline derivative surface modified water decentralized carbon nano-tube;
Wherein: the mass ratio of described water-soluble anils monomer and carbon nanotube is 0.1～5: 1; The mol ratio of water-soluble anils monomer and oxygenant is 0.5～2: 1;
Described water-soluble anils monomer is a kind of in ORTHO AMINO PHENOL SULPHONIC, m-sulfanilic acid, the N-propane sulfonic acid base aniline;
Described mineral acid is a kind of in hydrochloric acid, sulfuric acid, perchloric acid and the phosphoric acid;
Described oxygenant is a kind of in ammonium persulphate, Potassium Persulphate, Potcrate and the iron trichloride.
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