CN105199134A - Polyaniline-modified graphene conductive composite film and preparation method thereof - Google Patents
Polyaniline-modified graphene conductive composite film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyaniline-modified graphene conductive composite film and a preparation method thereof, belonging to the technical field of composite materials. The preparation method comprises the following steps: adding a small amount of aniline monomer into a graphene oxide acidic dispersion solution, stirring uniformly, adding an initiator ammonium persulfate powder to initiate in-situ polymerization, and carrying out layer-by-layer self-assembly to obtain a polyaniline-modified graphene oxide film; and finally, carrying out reduction treatment on the obtained polyaniline-modified graphene oxide film, washing and drying to obtain the high-dispersity high-conductivity polyaniline-modified graphene composite conductive material. The modification of the small amount of conductive high-polymer polyaniline on the graphene can effectively improve the conductivity and dispersity of the graphene; the acidic reducer hydriodic acid can reduce the graphene oxide on the premise of not changing the doping state of the polyaniline, and has the advantages of simpler operation process, convenient technique, low cost and no toxicity as compared with common alkaline hydrazine reducers.
Description
Technical field
The invention belongs to field of compound material, graphene conductive laminated film being specifically related to a kind of Polyaniline-modified and preparation method thereof.
Background technology
Graphene, as the typical two-dimensional material of one, since Late Cambrian in 2004, has received and has paid close attention to widely and study.Because Graphene possesses many very excellent performances, such as hardness is more than 100 times of steel, high light transmittance, high thermal conductivity coefficient, high electron mobility etc.The preparation method of current Graphene mainly contains vapour deposition process, SiC thermal decomposition method, mechanically peel method and oxidation reduction process etc.Oxidation reduction process obtains a lot of concerns and research due to the advantage such as simple to operate, cost is low, raw material is wide.But the Graphene that oxidation reduction process is prepared structurally exists the defect of some unrepairables, thus its performance is caused to receive great impact.Polyaniline is as a kind of conducting polymer, the long-range conjugated structure had makes it have unique electricity and optical property, moreover, and the π system of Graphene, can also there is the noncovalent interactions such as pi-pi accumulation, hydrogen bond and electrostatic force between remaining oxygen-containing functional group in the molecular structure of its uniqueness, thus prepares a kind of matrix material with excellent photoelectric properties.
A lot of relevant graphene-polyaniline composite material and related manufacturing processes thereof is disclosed in prior art, such as, application number is the preparation method that patent discloses a kind of high concentration graphene-polyaniline nano fiber composite dispersion liquid and composite membrane of 2011110293397.4, the method is by being mixed to form composite dispersion liquid by the dispersion liquid of graphene oxide dispersion and polyaniline by ultrasonic, again by reduction, vacuum filtration prepares composite membrane, the electric conductivity of this composite conductive film is 1200S/m, but the method is simple graphene oxide and polyaniline are carried out physical mixed, substantial chemistry is not had to connect, and after reduction, acid cleaning process is loaded down with trivial details again, application number is the synthetic method that patent discloses a kind of conductive polyaniline-graphene composite of 201010287916.1, first this invention carries out the in-situ polymerization of aniline in the dispersion liquid of graphene oxide, prepare polyaniline-graphite olefinic oxide mixture, and then prepare polyaniline-graphite alkene mixture by hydrazine heat reduction, operation is simple for the method, but hydrazine is as a kind of alkaline reduction thing, the conductivity of p-poly-phenyl amine has tremendous influence, it is made to change nonconducting eigenstate into by the doping state of conducting electricity, the conductivity of the polyaniline-graphite alkene mixture thus prepared is excellent not, application number be 201210274455.3 patent discloses preparation method of a kind of Graphene and polyaniline Composite Paper and products thereof, first the mixed dispersion liquid of graphene oxide and reductive agent is coated on substrate by this invention, above again polyaniline being deposited to after oven dry, thus obtain grapheme/polyaniline composite paper, although the method is simple to operate, but rely on physical bond between graphene layer and polyaniline, can not form good conductive path therebetween, therefore conductivity is still not high, application number is the step chemical preparation process that application discloses a kind of grapheme/polyaniline composite material of 201410517425.X, first graphite oxide is dissolved in acetic acid solution, add aniline monomer again, mixed by ultrasonic disperse, then add reductive agent hydroiodic acid HI and drip ammonium persulfate oxidizing agent, magnetic agitation, the in-situ polymerization of aniline is completed while graphite oxide is reduced to Graphene, after question response is complete, filter, washing, drying can obtain grapheme/polyaniline composite material, but the in-situ polymerization of the reduction of graphene oxide and aniline carries out by this application simultaneously, hydroiodic acid HI also take part in the polymerization of aniline while serving as reductive agent as dopant acid, this preparation technology's flow process is short, but the conductivity of the grapheme/polyaniline composite material prepared is still undesirable, specific conductivity only has 0.9S/cm.
In sum, need badly develop that a kind of specific conductivity is high, good dispersity, simple to operate, with low cost, feasibility is high, the graphene conductive composite material of the Polyaniline-modified of environmental protection and preparation method thereof.
Summary of the invention
The present invention is directed to the deficiency of problem pointed in background technology and prior art existence, graphene conductive laminated film that the object of the present invention is to provide a kind of Polyaniline-modified and preparation method thereof, obtained conductive composite film electric conductivity is high.
In order to realize above-mentioned purpose of the present invention, contriver, through a large amount of experimental studies, have developed a kind of graphene conductive laminated film of Polyaniline-modified, and described conductive composite film is prepared from by each raw material of following weight part:
The graphene oxide film of Polyaniline-modified 1 part
Hydroiodic acid HI 5 ~ 30 parts, wherein, the graphene oxide film of described Polyaniline-modified is adopted and is prepared from the following method:
(1) in-situ polymerization prepares the graphene oxide of Polyaniline-modified
First take that graphene oxide is ultrasonic to be dispersed in dilute hydrochloric acid solution, then aniline monomer is added, it is ultrasonic agitation 1 ~ 5 hour under the condition of 10 ~ 30 DEG C in temperature, obtain finely dispersed mixed system, subsequently to adding ammonium persulphate powder initiation in-situ polymerization in described mixed system, temperature of reaction is kept to be 10 ~ 30 DEG C, continue to react 3 ~ 10 hours under ultrasonic agitation condition, after reaction terminates, reaction product is centrifugal, take off layer throw out ultrasonic disperse in dilute hydrochloric acid, recentrifuge takes off layer throw out ultrasonic disperse in dilute hydrochloric acid, after repeating twice by throw out ultrasonic disperse in deionized water, obtain the graphene oxide dispersion of Polyaniline-modified,
(2) by the graphene oxide film of LBL self-assembly legal system for Polyaniline-modified
The graphene oxide dispersion of described for step (1) obtained Polyaniline-modified is incubated 10 ~ 60 minutes under the temperature condition of 80 ~ 100 DEG C, film can be formed on the surface of dispersion liquid, then by described film drying, the graphene oxide film of described Polyaniline-modified is obtained.
Further, in technique scheme, the mass ratio of step (1) described graphene oxide and aniline monomer, ammonium persulphate powder is 1:0.1 ~ 10:0.1 ~ 10.
Further, in technique scheme, the mass concentration of step (1) described dilute hydrochloric acid is 1 ~ 10%.
Further, the mass concentration of hydroiodic acid HI described in technique scheme is preferably 47%.
Further, the described concrete drying conditions of technique scheme step (2) is under the temperature condition of 60 ~ 80 DEG C dry 6 ~ 12 hours.
Another object of the present invention is to the preparation method of the graphene conductive laminated film providing a kind of Polyaniline-modified described above, described method comprises the steps:
(1) in-situ polymerization prepares the graphene oxide of Polyaniline-modified
First take that graphene oxide is ultrasonic to be dispersed in dilute hydrochloric acid solution, then aniline monomer is added, it is ultrasonic agitation 1 ~ 5 hour under the condition of 10 ~ 30 DEG C in temperature, obtain finely dispersed mixed system, subsequently to adding ammonium persulphate powder initiation in-situ polymerization in described mixed system, temperature of reaction is kept to be 10 ~ 30 DEG C, continue to react 3 ~ 10 hours under ultrasonic agitation condition, after reaction terminates, reaction product is centrifugal, take off layer throw out ultrasonic disperse in dilute hydrochloric acid, recentrifuge takes off layer throw out ultrasonic disperse in dilute hydrochloric acid, after repeating twice by throw out ultrasonic disperse in deionized water, obtain the graphene oxide dispersion of Polyaniline-modified,
(2) by the graphene oxide film of LBL self-assembly legal system for Polyaniline-modified
The graphene oxide dispersion of described for above-mentioned steps (1) obtained Polyaniline-modified is incubated 10 ~ 60 minutes under the temperature condition of 80 ~ 100 DEG C, film can be formed on the surface of dispersion liquid, then by described film drying, the graphene oxide film of described Polyaniline-modified is obtained;
(3) Graphene of Polyaniline-modified is prepared by hydroiodic acid HI reduction
The graphene oxide film taking the described obtained Polyaniline-modified of above-mentioned steps (2) joins in 5 ~ 30 parts of hydroiodic acid HIs, under dark conditions and temperature of reaction be carry out reduction reaction under the condition of 10 ~ 30 DEG C, reaction times is 12 ~ 24 hours, after reaction terminates, repeatedly with a large amount of deionized water rinsing film until pH value is in neutral, then vacuum-drying, obtains the graphene conductive laminated film of Polyaniline-modified.
Further, in technique scheme, the mass ratio of step (1) described graphene oxide and aniline monomer, ammonium persulphate powder is 1:0.1 ~ 10:0.1 ~ 10.
Further, in technique scheme, the mass ratio of step (1) described graphene oxide and dilute hydrochloric acid is 1:40 ~ 50.
Further, in technique scheme, the described hydroiodic acid HI mass concentration of step (3) is preferably 47%.
Further, the described concrete drying conditions of technique scheme step (2) is under the temperature condition of 60 ~ 80 DEG C dry 6 ~ 12 hours.
Further, the described vacuum-drying condition of technique scheme step (3) is under the temperature condition of 60 ~ 80 DEG C dry 6 ~ 12 hours.
Compared with prior art, the present invention has following beneficial effect:
(1) first the present invention adopts in-situ polymerization to prepare Polyaniline-modified graphene oxide dispersion, again by LBL self-assembly legal system standby go out ultra-thin Polyaniline-modified graphene oxide film, finally utilize hydroiodic acid HI redox graphene, improve the reducing degree of graphene oxide, the Polyaniline-modified graphene composite film obtained has higher conductivity, square resistance is minimum is about 156 Ω/, and be converted into specific conductivity and be about 1000S/cm, electric conductivity is high;
(2) good dispersity of polyaniline in Graphene in the laminated film that obtains of the present invention;
(3) the present invention is polymerized by the acid dispersion situ of aniline monomer at graphene oxide, conductive polymer polyanilinc can be combined by chemical interactions with graphene oxide, in the process of reduction, adopt acidic reduction agent hydroiodic acid HI not only can ensure the abundant reduction to graphene oxide, but also Polyaniline Doped state can not be changed, ensure that polyaniline conductivity is not damaged, do not change polyaniline structure, thus ensure that the Graphene of Polyaniline-modified has good electric property, more general alkaline hydrazine class reductive agent, simple to operate, technique is convenient, cost is low and nontoxic.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the graphene conductive laminated film of the Polyaniline-modified that the embodiment of the present invention 1 obtains.
Embodiment
Form is described in further detail foregoing of the present invention again by the following examples, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to following embodiment, all technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
The graphene conductive laminated film of a kind of Polyaniline-modified of the present embodiment, described laminated film is prepared from by each raw material of following weight part:
The graphene oxide film of Polyaniline-modified 1 part
Mass concentration is the hydroiodic acid HI 8 parts of 47%.
The graphene conductive laminated film of Polyaniline-modified described above is adopted and is prepared from the following method, comprises the steps:
(1) in-situ polymerization prepares the graphene oxide of Polyaniline-modified
Take 1 part of graphene oxide, ultrasonic disperse is in the dilute hydrochloric acid of 2% in 50ml mass concentration, add 0.1 part of aniline monomer subsequently, be stir 1 hour under the condition of 10 DEG C in temperature, add 0.1 part of ammonium persulphate powder initiation in-situ polymerization subsequently, react 5 hours under the temperature condition of 10 DEG C, after reaction terminates, reaction product is centrifugal, taking off layer throw out ultrasonic disperse is in the dilute hydrochloric acid of 2% in mass concentration, it is in the dilute hydrochloric acid of 2% in mass concentration that recentrifuge takes off layer throw out ultrasonic disperse, after repeating twice by throw out ultrasonic disperse in deionized water, obtain the graphene oxide dispersion of Polyaniline-modified,
(2) by the graphene oxide film of LBL self-assembly legal system for Polyaniline-modified
The graphene oxide dispersion of described for step (1) obtained Polyaniline-modified is heated to 80 DEG C, then under the temperature condition of 80 DEG C, 30 minutes are incubated, film can be formed on the surface of described dispersion liquid, then by described film under the temperature condition of 60 DEG C dry 12 hours, the graphene oxide film of described Polyaniline-modified is obtained;
(3) Graphene of Polyaniline-modified is prepared by hydroiodic acid HI reduction
It is in the hydroiodic acid HI of 47% that the graphene oxide film taking 1 part of described obtained Polyaniline-modified of step (2) joins 8 parts of mass concentrations, under dark conditions and temperature of reaction be carry out reduction reaction under the condition of 10 DEG C, reaction times is 12 hours, after reaction terminates, repeatedly with a large amount of deionized water rinsing film until pH value is in neutral, then vacuum-drying 12 hours under 60 DEG C of temperature condition, obtains the graphene conductive laminated film of Polyaniline-modified.
The graphene conductive laminated film of the above-mentioned obtained Polyaniline-modified of the present embodiment, recording square resistance through square resistance instrument is 156 Ω/.
Fig. 1 is the transmission electron microscope picture of the graphene conductive laminated film of the Polyaniline-modified that the present embodiment obtains.As can be seen from this figure, Graphene presents complete sheet, light transmission is fine, sheet interlayer has partial folds, graphene sheet layer adhering to black particle is polyaniline, polyaniline is deposited on graphene sheet layer with chemistry, physical action, and polyaniline is evenly distributed at graphene film, has good dispersiveness.
Embodiment 2
The graphene conductive laminated film of a kind of Polyaniline-modified of the present embodiment, described laminated film is prepared from by each raw material of following weight part:
The graphene oxide film of Polyaniline-modified 1 part
Mass concentration is the hydroiodic acid HI 15 parts of 47%.
The graphene conductive laminated film of Polyaniline-modified described above is adopted and is prepared from the following method, comprises the steps:
(1) in-situ polymerization prepares the graphene oxide of Polyaniline-modified
Take 1 part of graphene oxide, ultrasonic disperse is in the dilute hydrochloric acid of 5% in 50ml mass concentration, add 0.3 part of aniline monomer subsequently, be stir 2 hours under the condition of 20 DEG C in temperature, add 0.3 part of ammonium persulphate powder initiation in-situ polymerization subsequently, react 8 hours under the temperature condition of 20 DEG C, after reaction terminates, reaction product is centrifugal, taking off layer throw out ultrasonic disperse is in the dilute hydrochloric acid of 5% in mass concentration, it is in the dilute hydrochloric acid of 5% in mass concentration that recentrifuge takes off layer throw out ultrasonic disperse, after repeating twice by throw out ultrasonic disperse in deionized water, obtain the graphene oxide dispersion of Polyaniline-modified,
(2) by the graphene oxide film of LBL self-assembly legal system for Polyaniline-modified
The graphene oxide dispersion of described for step (1) obtained Polyaniline-modified is heated to 90 DEG C, 20 minutes are incubated under the temperature condition of 90 DEG C, film can be formed on the surface of described dispersion liquid, then by described film under the temperature condition of 70 DEG C dry 10 hours, the graphene oxide film of described Polyaniline-modified is obtained;
(3) Graphene of Polyaniline-modified is prepared by hydroiodic acid HI reduction
It is reduction treatment in the hydroiodic acid HI of 47% that the graphene oxide film taking the described obtained Polyaniline-modified of step (2) joins 15 parts of mass concentrations, under dark conditions and temperature of reaction be carry out reduction reaction under the condition of 20 DEG C, reaction times is 15 hours, after reaction terminates, repeatedly with a large amount of deionized water rinsing film until pH value is in neutral, then dry vacuum-drying in 10 hours under the temperature condition of 70 DEG C, obtains the graphene conductive laminated film of Polyaniline-modified.
The graphene conductive laminated film of the above-mentioned obtained Polyaniline-modified of the present embodiment, recording square resistance through square resistance instrument is 189 Ω/.
Embodiment 3
The graphene conductive laminated film of a kind of Polyaniline-modified of the present embodiment, described laminated film is prepared from by each raw material of following weight part:
The graphene oxide film of Polyaniline-modified 1 part
Mass concentration is the hydroiodic acid HI 23 parts of 47%.
The graphene conductive laminated film of Polyaniline-modified described above is adopted and is prepared from the following method, comprises the steps:
(1) in-situ polymerization prepares the graphene oxide of Polyaniline-modified
Take 1 part of graphene oxide, ultrasonic disperse is in the dilute hydrochloric acid of 8% in 50ml mass concentration, add 0.5 part of aniline monomer subsequently, be stir 5 hours under the condition of 30 DEG C in temperature, add 0.5 part of ammonium persulphate powder initiation in-situ polymerization subsequently, react 10 hours under the temperature condition of 30 DEG C, after reaction terminates, reaction product is centrifugal, taking off layer throw out ultrasonic disperse is in the dilute hydrochloric acid of 8% in mass concentration, it is in the dilute hydrochloric acid of 8% in mass concentration that recentrifuge takes off layer throw out ultrasonic disperse, after repeating twice by throw out ultrasonic disperse in deionized water, obtain the graphene oxide dispersion of Polyaniline-modified,
(2) by the graphene oxide film of LBL self-assembly legal system for Polyaniline-modified
The graphene oxide dispersion of described for step (1) obtained Polyaniline-modified is heated to 100 DEG C, 10 minutes are incubated under the temperature condition of 90 DEG C, film can be formed on the surface of described dispersion liquid, then by described film under the temperature condition of 80 DEG C dry 6 hours, the graphene oxide film of described Polyaniline-modified is obtained;
(3) Graphene of Polyaniline-modified is prepared by hydroiodic acid HI reduction
It is reduction treatment in the hydroiodic acid HI of 47% that the graphene oxide film taking 1 part of described obtained Polyaniline-modified of step (2) joins 23 parts of mass concentrations, under dark conditions and temperature of reaction be carry out reduction reaction under the condition of 30 DEG C, reaction times is 12 hours, after reaction terminates, repeatedly with a large amount of deionized water rinsing film until pH value is in neutral, then vacuum-drying 6 hours under the temperature condition of 80 DEG C, obtains the graphene conductive laminated film of Polyaniline-modified.
The graphene conductive laminated film of the above-mentioned obtained Polyaniline-modified of the present embodiment, recording square resistance through square resistance instrument is 213 Ω/.
Claims (10)
1. a graphene conductive laminated film for Polyaniline-modified, is characterized in that: described conductive composite film is prepared from by each raw material of following weight part:
The graphene oxide film of Polyaniline-modified 1 part
Hydroiodic acid HI 5 ~ 30 parts, wherein, the graphene oxide film of described Polyaniline-modified is adopted and is prepared from the following method:
(1) in-situ polymerization prepares the graphene oxide of Polyaniline-modified
First take that graphene oxide is ultrasonic to be dispersed in dilute hydrochloric acid solution, then aniline monomer is added, it is ultrasonic agitation 1 ~ 5 hour under the condition of 10 ~ 30 DEG C in temperature, obtain finely dispersed mixed system, subsequently to adding ammonium persulphate powder initiation in-situ polymerization in described mixed system, temperature of reaction is kept to be 10 ~ 30 DEG C, continue to react 3 ~ 10 hours under ultrasonic agitation condition, after reaction terminates, reaction product is centrifugal, take off layer throw out ultrasonic disperse in dilute hydrochloric acid, recentrifuge takes off layer throw out ultrasonic disperse in dilute hydrochloric acid, after repeating twice by throw out ultrasonic disperse in deionized water, obtain the graphene oxide dispersion of Polyaniline-modified,
(2) by the graphene oxide film of LBL self-assembly legal system for Polyaniline-modified
The graphene oxide dispersion of described for step (1) obtained Polyaniline-modified is incubated 10 ~ 60 minutes under the temperature condition of 80 ~ 100 DEG C, film can be formed on the surface of dispersion liquid, then by described film drying, the graphene oxide film of described Polyaniline-modified is obtained.
2. the graphene conductive laminated film of a kind of Polyaniline-modified according to claim 1, is characterized in that: the mass ratio of step (1) described graphene oxide and aniline monomer, ammonium persulphate powder is 1:0.1 ~ 10:0.1 ~ 10.
3. the graphene conductive laminated film of a kind of Polyaniline-modified according to claim 1, is characterized in that: the mass concentration of step (1) described dilute hydrochloric acid is 1 ~ 10%.
4. the graphene conductive laminated film of a kind of Polyaniline-modified according to claim 1, is characterized in that: the mass concentration of described hydroiodic acid HI is 47%.
5. the graphene conductive laminated film of a kind of Polyaniline-modified according to claim 1, is characterized in that: the described concrete drying conditions of step (2) is under the temperature condition of 60 ~ 80 DEG C dry 6 ~ 12 hours.
6. a preparation method for the graphene conductive laminated film of the Polyaniline-modified according to any one of Claims 1 to 5, described method comprises the steps:
(1) in-situ polymerization prepares the graphene oxide of Polyaniline-modified
First take that graphene oxide is ultrasonic to be dispersed in dilute hydrochloric acid solution, then aniline monomer is added, it is ultrasonic agitation 1 ~ 5 hour under the condition of 10 ~ 30 DEG C in temperature, obtain finely dispersed mixed system, subsequently to adding ammonium persulphate powder initiation in-situ polymerization in described mixed system, temperature of reaction is kept to be 10 ~ 30 DEG C, continue to react 3 ~ 10 hours under ultrasonic agitation condition, after reaction terminates, reaction product is centrifugal, take off layer throw out ultrasonic disperse in dilute hydrochloric acid, recentrifuge takes off layer throw out ultrasonic disperse in dilute hydrochloric acid, after repeating twice by throw out ultrasonic disperse in deionized water, obtain the graphene oxide dispersion of Polyaniline-modified,
(2) by the graphene oxide film of LBL self-assembly legal system for Polyaniline-modified
The graphene oxide dispersion of described for above-mentioned steps (1) obtained Polyaniline-modified is incubated 10 ~ 60 minutes under the temperature condition of 80 ~ 100 DEG C, film can be formed on the surface of dispersion liquid, then by described film drying, the graphene oxide film of described Polyaniline-modified is obtained;
(3) Graphene of Polyaniline-modified is prepared by hydroiodic acid HI reduction
The graphene oxide film taking the described obtained Polyaniline-modified of above-mentioned steps (2) joins in 5 ~ 30 parts of hydroiodic acid HIs, under dark conditions and temperature of reaction be carry out reduction reaction under the condition of 10 ~ 30 DEG C, reaction times is 12 ~ 24 hours, after reaction terminates, repeatedly with a large amount of deionized water rinsing film until pH value is in neutral, then vacuum-drying, obtains the graphene conductive laminated film of Polyaniline-modified.
7. the preparation method of the graphene conductive laminated film of Polyaniline-modified according to claim 6, is characterized in that: the mass ratio of step (1) described graphene oxide and aniline monomer, ammonium persulphate powder is 1:0.1 ~ 10:0.1 ~ 10.
8. the preparation method of the graphene conductive laminated film of Polyaniline-modified according to claim 6, is characterized in that: the mass concentration of step (1) described dilute hydrochloric acid is 1 ~ 10%.
9. the preparation method of the graphene conductive laminated film of Polyaniline-modified according to claim 6, is characterized in that: the described hydroiodic acid HI mass concentration of step (3) is 47%.
10. the preparation method of the graphene conductive laminated film of Polyaniline-modified according to claim 6, is characterized in that: the described concrete drying conditions of step (2) is under the temperature condition of 60 ~ 80 DEG C dry 6 ~ 12 hours.
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