CN104672445A - Method for preparing multiwalled carbon nanotube/polyaniline nano composite material - Google Patents
Method for preparing multiwalled carbon nanotube/polyaniline nano composite material Download PDFInfo
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- CN104672445A CN104672445A CN201510043008.0A CN201510043008A CN104672445A CN 104672445 A CN104672445 A CN 104672445A CN 201510043008 A CN201510043008 A CN 201510043008A CN 104672445 A CN104672445 A CN 104672445A
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Abstract
The invention relates to a method for preparing a multiwalled carbon nanotube/polyaniline nano composite material. The method comprises the steps of carrying out modification on the multiwalled carbon nanotube by using mixed acid consisting of concentrated sulfuric acid and concentrated nitric acid, and then preparing the multiwalled carbon nanotube/polyaniline nano composite material by taking the modified multiwalled carbon nanotube and aniline as main raw materials and adopting an in-situ oxidative polymerization method. The composite material obtained by the method has very high electrical conductivity, high strength and good heat stability and chemical stability. As the multiwalled carbon nanotube/polyaniline nano composite material has excellent electric properties and mechanical properties. The multiwalled carbon nanotube/polyaniline nano composite material has application potential in the aspects of photoelectric nanometer devices, super capacitors, field emission devices, sensors, anti-static electricity and electromagnetic shielding materials and the like.
Description
Technical field
The invention belongs to technical field of function materials, be specifically related to a kind of multi-walled carbon nano-tubes/polyaniline nano-composite material and preparation method thereof, be intended to the conductivity of the nano composite material that raising is prepared for raw material with multi-walled carbon nano-tubes, aniline.
Background technology
Conducting polymer composite refers to that specific conductivity is 10
-6the polymer materials of more than S/cm, the feature of the corrosion-resistant and easy processing of its existing macromolecular material, have again the advantages such as electroconductibility is good, other material can not be compared at present.
Carbon nanotube and conducting polymer compound, except improving except the specific conductivity of polymkeric substance, can also be improved its thermostability, mechanical property etc., therefore have very wide application prospect.At present, carbon nano tube/conducting polymer composite is applied to every field, as the manufacture of automobile conductive plastics component, the internal packing etc. of Anti-static device because of its good performance.In addition, it also can be used as electrode of super capacitor or electrochemical capacitor material.The preparation method of carbon nano tube/conducting polymer composite has any different because of the characteristic and performance difference of polymeric matrix, sums up and gets up to mainly contain two kinds of methods, as electrochemical in-situ polymerization and solution mixing method.[the Chen J H such as Chen, Huang Z P, Wang D Z, Appl. Phys. A, 2001,73 (2), 129-131] utilize electrochemical deposition method polypyrrole to be coated in coating and other metal or conductive polymers compound that carbon nano pipe array obtains, synthesize the nano composite material with multiple one-dimentional structure.[the Dalton A B such as Dalton, Stephan C, Coleman J N, J. Phys. Chem. B, 2000,104 (43), 10012-10016] MWCNTs joined a kind of conjugate light-emitting polymer with solution mixing method and gather metaphenylene ethene totally 2, in the toluene solution of the pungent alkoxyl group of 5-bis--to phenylene vinylene (PmPVDpPV), prepare MWCNTs/ PmPVDpPV nano composite material, compared with single PmPVDpPV, the conductivity of matrix material obviously strengthens.
Summary of the invention
The present invention is to provide a kind of method preparing multi-walled carbon nano-tubes/polyaniline nano-composite material, reaches the object improving nano composite material conductivity.
A kind of multi-walled carbon nano-tubes/polyaniline nano-composite material and preparation method thereof, is achieved through the following technical solutions:
Step (1): take 0.5 g multi-walled carbon nano-tubes in 250 mL there-necked flasks, slowly inject 80 mL nitration mixture, be then warming up to 80 oC, and mechanical stirring 2 h at this temperature.After reaction terminates, suction filtration is carried out to mixed solution, and repeatedly wash with distilled water until filtrate is in neutral.Finally by obtained filter cake dry 24 h under 60 oC, grinding obtains the multi-walled carbon nano-tubes of modification.
Step (2): get a certain amount of modified multiwalled carbon nanotube, 100 mL1 mol/L hydrochloric acid in the there-necked flask of 250 mL, pipetting 0.5 g aniline with transfer pipet adds in said mixture, then above-mentioned multi-walled carbon nano-tubes, hydrochloric acid soln, aniline mixture are placed in ultrasonic 30 min of ultrasonic cleaner, then to be placed in ice-water bath and in addition mechanic whirl-nett reaction, to control at certain rotating speed.After reacting 30 min, drip ammonium persulfate solution (a certain amount of ammonium persulphate is dissolved in the hydrochloric acid of 20 mL1 mol/L) gradually, the speed regulation of dropping is in certain scope.After reaction for some time, suction filtration is carried out to gained polymerisate, and repeatedly wash with dehydrated alcohol, to guarantee to remove the impurity such as unreacted aniline and oxygenant, subsequently filter cake is placed on dry 24 h in 60 oC baking ovens, finally grinding obtains multi-walled carbon nano-tubes/polyaniline nano-composite material.
In aforesaid method, the nitration mixture described in step (1) is made up of the vitriol oil and concentrated nitric acid, and the volume ratio of the vitriol oil and concentrated nitric acid is 1:1.
In aforesaid method, the content adding modified multiwalled carbon nanotube described in step (2) is 0 ~ 80 wt%(relative to the total amount of multi-walled carbon nano-tubes and aniline).
In aforesaid method, the mixture of the multi-walled carbon nano-tubes described in step (2), hydrochloric acid soln, aniline composition, in ice-water bath, in addition churned mechanically rotating speed controls at 450 rpm.In addition, ammonium persulfate solution rate of addition regulation and control every 3 seconds 1.
In aforesaid method, the ammonium persulphate consumption described in step (2) is 0.125 ~ 0.875 g.
In aforesaid method, the reaction times dripped in step (2) after ammonium persulfate solution is 1 ~ 8 h.
The present invention first carries out modification with the nitration mixture that the vitriol oil and concentrated nitric acid form to multi-walled carbon nano-tubes.Then with modified multiwalled carbon nanotube, aniline is main raw material, adopts the method for in-situ oxidizing-polymerizing to prepare multi-walled carbon nano-tubes/polyaniline nano-composite material, and evaluates the conductivity of gained matrix material.
Beneficial effect of the present invention: the present invention is before this with the nitration mixture modified multiwalled carbon nanotube that the vitriol oil and concentrated nitric acid form, and modified multi-wall carbon nano-tube tube-surface introduces more carboxyl and oh group, and dispersion stabilization significantly improves.Therefore energy is good and polyaniline carries out compound, thus the conductivity of nano composite material can be improved.
Accompanying drawing explanation
The content of Fig. 1 multi-walled carbon nano-tubes is on the impact of multi-walled carbon nano-tubes/polyaniline nano-composite material conductivity;
The consumption of Fig. 2 ammonium persulphate is on the impact of multi-walled carbon nano-tubes/polyaniline nano-composite material conductivity;
Fig. 3 polymerization time is on the impact of multi-walled carbon nano-tubes/polyaniline nano-composite material conductivity;
The transmission electron microscope picture of Fig. 4 multi-walled carbon nano-tubes/polyaniline nano-composite material.
Embodiment
Below in conjunction with embodiment, the present invention is described further, but the scope of protection of present invention is not limited to the scope that embodiment is expressed.Except as otherwise noted, embodiment mid-score and per-cent are all with dry weight basis.
Embodiment 1
A kind of multi-walled carbon nano-tubes/polyaniline nano-composite material and preparation method thereof.First, take 0.5 g multi-walled carbon nano-tubes in 250 mL there-necked flasks, slowly inject 80 mL nitration mixture, be then warming up to 80 oC, and mechanical stirring 2 h at this temperature.After reaction terminates, suction filtration is carried out to mixed solution, and repeatedly wash with distilled water until filtrate is in neutral.Finally by obtained filter cake dry 24 h under 60 oC, grinding obtains the multi-walled carbon nano-tubes of modification.Secondly, get respectively modified multiwalled carbon nanotube that content is 0,20,40,60,80 wt%, 100 mL1 mol/L hydrochloric acid in the there-necked flask of 250 mL, pipetting 0.5 g aniline with transfer pipet adds in said mixture, then above-mentioned multi-walled carbon nano-tubes, hydrochloric acid soln, aniline mixture are placed in ultrasonic 30 min of ultrasonic cleaner, then to be placed in ice-water bath and in addition mechanic whirl-nett reaction, stirring velocity controls at 450 rpm.After reacting 30 min, drip ammonium persulfate solution (0.375 g ammonium persulphate is dissolved in the hydrochloric acid of 20 mL1 mol/L) gradually, the speed regulation of dropping every 3 seconds 1.After reacting 6 h, suction filtration is carried out to gained polymerisate, and repeatedly wash with dehydrated alcohol, to guarantee to remove the impurity such as unreacted aniline and oxygenant, subsequently filter cake is placed on dry 24 h in 60 oC baking ovens, finally grinding obtains multi-walled carbon nano-tubes/polyaniline nano-composite material.Record the specific conductivity of gained matrix material under different multi-walled carbon nano-tubes content as shown in Figure 1.
Embodiment 2
A kind of multi-walled carbon nano-tubes/polyaniline nano-composite material and preparation method thereof, first, takes 0.5 g multi-walled carbon nano-tubes in 250 mL there-necked flasks, slowly injects 80 mL nitration mixture, be then warming up to 80 oC, and mechanical stirring 2 h at this temperature.After reaction terminates, suction filtration is carried out to mixed solution, and repeatedly wash with distilled water until filtrate is in neutral.Finally by obtained filter cake dry 24 h under 60 oC, grinding obtains the multi-walled carbon nano-tubes of modification.Secondly, get 0.5 g modified multiwalled carbon nanotube, 100 mL1 mol/L hydrochloric acid in the there-necked flask of 250 mL, pipetting 0.5 g aniline with transfer pipet adds in said mixture, then above-mentioned multi-walled carbon nano-tubes, hydrochloric acid soln, aniline mixture are placed in ultrasonic 30 min of ultrasonic cleaner, then to be placed in ice-water bath and in addition mechanic whirl-nett reaction, stirring velocity controls at 450 rpm.After reacting 30 min, drip ammonium persulfate solution (getting the hydrochloric acid that 0.125,0.25,0.375,0.5,0.625,0.75,0.875 g ammonium persulphate is dissolved in 20 mL1 mol/L respectively) gradually, the speed regulation of dropping every 3 seconds 1.After reacting 6 h, suction filtration is carried out to gained polymerisate, and repeatedly wash with dehydrated alcohol, to guarantee to remove the impurity such as unreacted aniline and oxygenant, subsequently filter cake is placed on dry 24 h in 60 oC baking ovens, finally grinding obtains multi-walled carbon nano-tubes/polyaniline nano-composite material.Record the specific conductivity of gained matrix material under different ammonium persulphate consumption as shown in Figure 2.
Embodiment 3
A kind of multi-walled carbon nano-tubes/polyaniline nano-composite material and preparation method thereof, first, takes 0.5 g multi-walled carbon nano-tubes in 250 mL there-necked flasks, slowly injects 80 mL nitration mixture, be then warming up to 80 oC, and mechanical stirring 2 h at this temperature.After reaction terminates, suction filtration is carried out to mixed solution, and repeatedly wash with distilled water until filtrate is in neutral.Finally by obtained filter cake dry 24 h under 60 oC, grinding obtains the multi-walled carbon nano-tubes of modification.Secondly, get 0.5 g modified multiwalled carbon nanotube, 100 mL1 mol/L hydrochloric acid in the there-necked flask of 250 mL, pipetting 0.5 g aniline with transfer pipet adds in said mixture, then above-mentioned multi-walled carbon nano-tubes, hydrochloric acid soln, aniline mixture are placed in ultrasonic 30 min of ultrasonic cleaner, then to be placed in ice-water bath and in addition mechanic whirl-nett reaction, stirring velocity controls at 450 rpm.After reacting 30 min, drip ammonium persulfate solution (getting the hydrochloric acid that 0.625 g ammonium persulphate is dissolved in 20 mL1 mol/L) gradually, the speed regulation of dropping every 3 seconds 1.After reacting 1,2,4,6,8 h respectively, suction filtration is carried out to gained polymerisate, and repeatedly wash with dehydrated alcohol, to guarantee to remove the impurity such as unreacted aniline and oxygenant, subsequently filter cake is placed on dry 24 h in 60 oC baking ovens, finally grinding obtains multi-walled carbon nano-tubes/polyaniline nano-composite material.Record the specific conductivity of gained matrix material under the differential responses time as shown in Figure 3.In addition, the microscopic appearance of the nano composite material that 6 h obtain is reacted as shown in Figure 4.
The present invention take aniline as monomer, ammonium persulphate is oxygenant, deposit in case at modified multiwalled carbon nanotube, adopt the method for in situ chemical oxidative polymerization successfully to prepare hud typed multi-walled carbon nano-tubes/polyaniline nano-composite material, the purer polyaniline of specific conductivity of gained matrix material obviously strengthens.
Claims (6)
1. multi-walled carbon nano-tubes/polyaniline nano-composite material preparation method, is characterized in that comprising the steps:
Step (1): take 0.5 g multi-walled carbon nano-tubes in 250 mL there-necked flasks, slowly inject 80 mL nitration mixture, be then warming up to 80 oC, and mechanical stirring 2 h at this temperature; After reaction terminates, suction filtration is carried out to mixed solution, and repeatedly wash with distilled water until filtrate is in neutral; Finally by obtained filter cake dry 24 h under 60 oC, grinding obtains the multi-walled carbon nano-tubes of modification;
Step (2): get a certain amount of modified multiwalled carbon nanotube, 100 mL1 mol/L hydrochloric acid in the there-necked flask of 250 mL, pipetting 0.5 g aniline with transfer pipet adds in said mixture, then above-mentioned multi-walled carbon nano-tubes, hydrochloric acid soln, aniline mixture are placed in ultrasonic 30 min of ultrasonic cleaner, then to be placed in ice-water bath and in addition mechanic whirl-nett reaction, to control at certain rotating speed; After reacting 30 min, drip ammonium persulfate solution gradually, the speed regulation of dropping is in certain scope; After reaction for some time, suction filtration is carried out to gained polymerisate, and repeatedly wash with dehydrated alcohol, to guarantee to remove unreacted aniline and oxygenant, subsequently filter cake is placed on dry 24 h in 60 oC baking ovens, finally grinding obtains multi-walled carbon nano-tubes/polyaniline nano-composite material.
2. method according to claim 1, is characterized in that: the nitration mixture described in step (1) is made up of the vitriol oil and concentrated nitric acid, and the volume ratio of the vitriol oil and concentrated nitric acid is 1:1.
3. method according to claim 1, is characterized in that: the content adding modified multiwalled carbon nanotube described in step (2) is 0 ~ 80 wt%, relative to the total amount of multi-walled carbon nano-tubes and aniline.
4. method according to claim 1, is characterized in that: the mixture of the multi-walled carbon nano-tubes described in step (2), hydrochloric acid soln, aniline composition, and in ice-water bath, in addition churned mechanically rotating speed controls at 450 rpm; In addition, ammonium persulfate solution rate of addition regulation and control every 3 seconds 1.
5. method according to claim 1, is characterized in that: the ammonium persulphate consumption described in step (2) is 0.125 ~ 0.875 g.
6. method according to claim 1, is characterized in that: the reaction times dripped in step (2) after ammonium persulfate solution is 1 ~ 8 h.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105200848A (en) * | 2015-08-09 | 2015-12-30 | 浙江理工大学 | Nanometer composite conductive paint and preparation method thereof |
| CN105801850A (en) * | 2016-03-30 | 2016-07-27 | 重庆金固特新材料科技有限公司 | Synthesis method of conductive polyaniline and carbon nanotube compound |
| CN107337926A (en) * | 2017-07-17 | 2017-11-10 | 徐州乐泰机电科技有限公司 | A kind of preparation method of butadiene Polymerization of Polyaniline/carbon Nanotube anti-static material |
| CN107344996A (en) * | 2017-07-05 | 2017-11-14 | 安徽中威光电材料有限公司 | A kind of compound-type conducting heat conduction particle of polyaniline packaged silicon carbide multi-walled carbon nanotube and preparation method thereof |
| CN108410084A (en) * | 2018-02-12 | 2018-08-17 | 北京理工大学珠海学院 | A kind of preparation method of multi-walled carbon nanotube/polyvinylidene fluoride composite material |
| CN108490051A (en) * | 2018-05-21 | 2018-09-04 | 吉林大学 | A kind of flexible miniature is from driving gas at normal temperature sensor and preparation method thereof |
| WO2018157401A1 (en) * | 2017-03-03 | 2018-09-07 | 深圳市佩成科技有限责任公司 | Preparation method for pani/mwcnts composite material |
| CN108530620A (en) * | 2018-03-19 | 2018-09-14 | 厦门理工学院 | The preparation method of the compound and the compound of Polyaniline and its derivative and carbon nanotube |
| CN109135279A (en) * | 2018-07-11 | 2019-01-04 | 常州大学 | A kind of preparation method based on polyamidoimide high-strength high-conductivity film |
| CN109251337A (en) * | 2018-09-26 | 2019-01-22 | 北京化工大学 | A kind of preparation method of polyaniline carbon pipe flexible compound thermoelectric film material |
| CN109267199A (en) * | 2018-08-16 | 2019-01-25 | 吉祥三宝高科纺织有限公司 | A kind of electrically conductive polyaniline/carbon nano-tube fibre composite material and preparation method and purposes |
| CN110550705A (en) * | 2019-07-02 | 2019-12-10 | 陕西科技大学 | preparation method of membrane electrode for electrolyzing dye wastewater containing heavy metals |
| CN111472165A (en) * | 2020-04-24 | 2020-07-31 | 安徽工程大学 | Polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric and preparation method thereof |
| CN112430352A (en) * | 2020-12-01 | 2021-03-02 | 福州大学 | Double-network cross-linked and coated polyaniline/multi-walled carbon nanotube composite conductive filler and preparation method thereof |
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| CN105200848A (en) * | 2015-08-09 | 2015-12-30 | 浙江理工大学 | Nanometer composite conductive paint and preparation method thereof |
| CN105801850A (en) * | 2016-03-30 | 2016-07-27 | 重庆金固特新材料科技有限公司 | Synthesis method of conductive polyaniline and carbon nanotube compound |
| WO2018157401A1 (en) * | 2017-03-03 | 2018-09-07 | 深圳市佩成科技有限责任公司 | Preparation method for pani/mwcnts composite material |
| CN107344996A (en) * | 2017-07-05 | 2017-11-14 | 安徽中威光电材料有限公司 | A kind of compound-type conducting heat conduction particle of polyaniline packaged silicon carbide multi-walled carbon nanotube and preparation method thereof |
| CN107337926A (en) * | 2017-07-17 | 2017-11-10 | 徐州乐泰机电科技有限公司 | A kind of preparation method of butadiene Polymerization of Polyaniline/carbon Nanotube anti-static material |
| CN108410084A (en) * | 2018-02-12 | 2018-08-17 | 北京理工大学珠海学院 | A kind of preparation method of multi-walled carbon nanotube/polyvinylidene fluoride composite material |
| CN108530620B (en) * | 2018-03-19 | 2021-03-12 | 厦门理工学院 | Polyaniline and its derivative and carbon nanotube compound and preparation method thereof |
| CN108530620A (en) * | 2018-03-19 | 2018-09-14 | 厦门理工学院 | The preparation method of the compound and the compound of Polyaniline and its derivative and carbon nanotube |
| CN108490051A (en) * | 2018-05-21 | 2018-09-04 | 吉林大学 | A kind of flexible miniature is from driving gas at normal temperature sensor and preparation method thereof |
| CN109135279A (en) * | 2018-07-11 | 2019-01-04 | 常州大学 | A kind of preparation method based on polyamidoimide high-strength high-conductivity film |
| CN109267199A (en) * | 2018-08-16 | 2019-01-25 | 吉祥三宝高科纺织有限公司 | A kind of electrically conductive polyaniline/carbon nano-tube fibre composite material and preparation method and purposes |
| CN109251337A (en) * | 2018-09-26 | 2019-01-22 | 北京化工大学 | A kind of preparation method of polyaniline carbon pipe flexible compound thermoelectric film material |
| CN110550705A (en) * | 2019-07-02 | 2019-12-10 | 陕西科技大学 | preparation method of membrane electrode for electrolyzing dye wastewater containing heavy metals |
| CN111472165A (en) * | 2020-04-24 | 2020-07-31 | 安徽工程大学 | Polyaniline-coated carbon nanotube coating flexible electromagnetic shielding fabric and preparation method thereof |
| CN112430352A (en) * | 2020-12-01 | 2021-03-02 | 福州大学 | Double-network cross-linked and coated polyaniline/multi-walled carbon nanotube composite conductive filler and preparation method thereof |
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Application publication date: 20150603 |