CN113265090A - Preparation method for coating polyaniline-doped graphene surface - Google Patents
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Abstract
The invention belongs to the technical field of materials, and particularly relates to a preparation method of polyaniline-coated and doped graphene on the surface of graphene. Firstly, doped polyaniline existing on the surface of the coated graphene can form good compatibility with other materials; and secondly, doped polyaniline is a conductive polymer material with a conjugated structure, and can provide proper conductivity for the surface of graphene, so that the function of the graphene is fully exerted. The modified graphene can be used as a conductive filler for systems such as composite materials, coatings, printing inks, adhesives and films, and has the technical characteristics of simplicity, convenience, rapidness, environmental friendliness and the like.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of polyaniline-coated and doped graphene.
Background
Graphene (Graphene) is a new material with sp hybridized connected carbon atoms tightly packed into a single-layer two-dimensional honeycomb lattice structure. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.
Graphene is a nanoscale layered material, and is easy to agglomerate due to large specific surface area and high surface energy, so that the characteristics of the nanoscale layered material cannot be exerted. In addition, graphene is a carbon material, and the surface physicochemical characteristics and the microstructure of the graphene are greatly different from those of other materials, so that the graphene is difficult to be uniformly mixed with other materials.
Aiming at the characteristics of graphene, surface modification methods are mostly adopted at present to adjust the surface structure and state of graphene, so that the problems of poor agglomeration and dispersibility of graphene and the like are solved, and the dispersion stability of graphene is improved by the methods. But the modified graphene surface has an insulating effect, so that the graphene is forced to lose the original function.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method for coating polyaniline-doped graphene on the surface of graphene, provides polyaniline-doped graphene, has the technical characteristics of simplicity, convenience, rapidness, environmental friendliness and the like, and simultaneously provides a preparation method for polyaniline-doped graphene.
The specific technical scheme is as follows:
a preparation method for coating polyaniline-doped graphene on the surface of graphene takes graphene, aniline, ammonium persulfate, sodium dodecyl benzene sulfonate, hydrochloric acid, N-methyl pyrrolidone and deionized water as raw materials, and coats polyaniline-doped polyaniline on the surface of the modified graphene by an in-situ polymerization method to prepare the modified graphene, wherein the specific preparation method comprises the following steps:
(1) taking raw materials according to a certain mass part ratio;
(2) adding graphene and aniline into a mixed solution composed of deionized water and N-methylpyrrolidone, stirring for a period of time, carrying out ultrasonic treatment for a period of time, and standing for 24 hours at room temperature to obtain a dispersion liquid A;
(3) adding ammonium persulfate, sodium dodecyl benzene sulfonate and hydrochloric acid into deionized water, uniformly stirring to obtain a dispersion liquid B, dropwise adding the dispersion liquid B into the dispersion liquid A within a certain time, and reacting at 0 ℃ for a certain time to finish the reaction;
(4) and washing the reaction product with excessive deionized water, centrifuging the reaction product for 3 times, and drying the reaction product at 40-60 ℃ to constant weight to obtain polyaniline-coated graphene.
The raw materials in the step (1) comprise, by mass, 100 parts of graphene, 10-100 parts of aniline, 10-200 parts of ammonium persulfate, 0-50 parts of sodium dodecyl benzene sulfonate, 0-5 parts of hydrochloric acid, 30-100 parts of N-methylpyrrolidone and 1000-4000 parts of deionized water.
The graphene is one of single-layer graphene, double-layer graphene or multi-layer graphene.
The aniline, the ammonium persulfate, the sodium dodecyl benzene sulfonate, the hydrochloric acid and the N-methyl pyrrolidone are chemically pure or analytically pure.
The deionized water meets the minimum grade required by the national standard GB/T1146.1-1997.
And (4) drying in a vacuum oven.
Preferably, the raw materials in the step (1) comprise, by mass, 100 parts of graphene, 100 parts of aniline, 200 parts of ammonium persulfate, 50 parts of sodium dodecyl benzene sulfonate, 5 parts of hydrochloric acid, 100 parts of N-methylpyrrolidone and 4000 parts of deionized water.
The stirring time in the step (2) is 1-2 hours.
The ultrasonic treatment time in the step (2) is 10-30 minutes.
In the step (3), the dispersion liquid B is dripped into the dispersion liquid A for 0.5 to 2 hours; reacting for 6-12 hours at 0 ℃.
Compared with the prior art, the invention has the following beneficial technical effects:
the method is characterized in that graphene, aniline, ammonium persulfate, sodium dodecyl benzene sulfonate, hydrochloric acid, N-methyl pyrrolidone and deionized water are used as raw materials, polyaniline-doped materials are coated on the surface of the graphene through an in-situ polymerization method to prepare the modified graphene, and the polyaniline-doped materials on the surface of the modified graphene can prevent the agglomeration problem of graphene powder and endow the surface of the graphene with conductive characteristics. Firstly, doped polyaniline existing on the surface of the coated graphene can form good compatibility with other materials; and secondly, the conductivity of the doped polyaniline is higher than that of the intrinsic polyaniline, so that proper conductivity can be provided for the surface of the graphene, and the function of the graphene can be fully exerted. The modified graphene can be used as a conductive filler for systems such as composite materials, coatings, printing inks, adhesives and films, and has the technical characteristics of simplicity, convenience, rapidness, environmental friendliness and the like.
Drawings
Fig. 1 is a transmission electron microscope photograph of the graphene coated and doped with polyaniline of example 1.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings, but the scope of the present invention is not limited by the embodiments.
Comparative example
100 g of graphene and 100 g of aniline are added into a mixed solution consisting of 4000 g of deionized water and 100 g of N-methylpyrrolidone, stirred for 2 hours, subjected to ultrasonic treatment for 30 minutes, and then placed at room temperature for 24 hours to obtain a dispersion A. 200 g of ammonium persulfate is added into deionized water and stirred uniformly to obtain dispersion liquid B, the dispersion liquid B is dropwise added into the dispersion liquid A within 1 hour, and the reaction is finished after 6 hours of reaction at the temperature of 0 ℃. And washing the reaction product with excessive deionized water, centrifuging the reaction product for 3 times, and drying the reaction product in a vacuum oven at 40 ℃ to constant weight to obtain the polyaniline-coated modified graphene. The resistivity of the graphene is 8.2 multiplied by 10 < -2 > omega-m, the graphene is completely precipitated after being placed in xylene for 36 hours, and the surface of the graphene in the embodiment is coated with undoped eigenstate polyaniline, so that the conductivity and the compatibility of the graphene are not ideal.
Example 1
100 g of graphene and 100 g of aniline are added into a mixed solution consisting of 4000 g of deionized water and 100 g of N-methylpyrrolidone, stirred for 1 hour, subjected to ultrasonic treatment for 10 minutes, and then placed at room temperature for 24 hours to obtain a dispersion A. Adding 200 g of ammonium persulfate, 50 g of sodium dodecyl benzene sulfonate and 5 g of hydrochloric acid into deionized water, uniformly stirring to obtain a dispersion liquid B, dropwise adding the dispersion liquid B into the dispersion liquid A within 0.5 hour, and reacting for 12 hours at 0 ℃ to finish the reaction. And washing the reaction product with excessive deionized water, centrifuging the reaction product for 3 times, and drying the reaction product in a vacuum oven at 40 ℃ to constant weight to obtain polyaniline-coated graphene.
Fig. 1 is a transmission electron microscope photograph of the graphene coated with the doped polyaniline in example 1, and as shown in the figure, it is seen that cluster-like doped polyaniline exists on the surface of the graphene sheet layer. The resistivity of the graphene obtained in the embodiment is 1.8 multiplied by 10 < -4 > omega.m, and the graphene is not precipitated after being placed in xylene for 1000 hours, and the graphene surface in the embodiment is coated with doped polyaniline, so that the conductivity and the compatibility of the graphene are better than those of a comparative example.
The following examples are doped polyaniline-coated graphene, and the microstructure thereof is similar to that of example 1, and therefore similar pictures are not shown.
Example 2
100 g of graphene and 10 g of aniline are added into a mixed solution composed of 1000 g of deionized water and 90 g of N-methylpyrrolidone, stirred for 1 hour, subjected to ultrasonic treatment for 30 minutes, and then placed at room temperature for 24 hours to obtain a dispersion A. Adding 10 g of ammonium persulfate and 5 g of sodium dodecyl benzene sulfonate into deionized water, uniformly stirring to obtain a dispersion liquid B, dropwise adding the dispersion liquid B into the dispersion liquid A within 1 hour, and reacting for 11 hours at the temperature of 0 ℃ to finish the reaction. And washing the reaction product with excessive deionized water, centrifuging the reaction product for 3 times, and drying the reaction product in a vacuum oven at 60 ℃ to constant weight to obtain polyaniline-coated graphene. The resistivity of the graphene is 7.9 multiplied by 10 < -3 > omega-m, the graphene begins to precipitate after being placed in xylene for 200 hours, and the conductivity and the compatibility of the graphene are better than those of a comparative example because the surface of the graphene in the embodiment is coated with doped polyaniline.
Example 3
100 g of graphene and 40 g of aniline are added into a mixed solution composed of 1000 g of deionized water and 90 g of N-methylpyrrolidone, stirred for 1 hour, subjected to ultrasonic treatment for 30 minutes, and then placed at room temperature for 24 hours to obtain a dispersion A. 100 g of ammonium persulfate and 1 g of hydrochloric acid are added into deionized water and stirred uniformly to obtain dispersion liquid B, the dispersion liquid B is dropwise added into the dispersion liquid A within 1 hour, and the reaction is finished after the dispersion liquid B reacts for 12 hours at the temperature of 0 ℃. And washing the reaction product with excessive deionized water, centrifuging the reaction product for 3 times, and drying the reaction product in a vacuum oven at 60 ℃ to constant weight to obtain polyaniline-coated graphene. The resistivity of the graphene is 1.0 multiplied by 10 < -4 > omega.m, the graphene is completely precipitated after being placed in xylene for 120 hours, and the conductivity and the compatibility of the graphene are better than those of a comparative example because the surface of the graphene in the embodiment is coated with doped polyaniline.
Example 4
100 g of graphene and 50 g of aniline are added into a mixed solution consisting of 2600 g of deionized water and 30 g of N-methylpyrrolidone, stirred for 1.5 hours, subjected to ultrasonic treatment for 20 minutes, and then placed at room temperature for 24 hours to obtain a dispersion A. Adding 110 g of ammonium persulfate, 15 g of sodium dodecyl benzene sulfonate and 3 g of hydrochloric acid into deionized water, uniformly stirring to obtain a dispersion liquid B, dropwise adding the dispersion liquid B into the dispersion liquid A within 2 hours, and reacting for 8 hours at 0 ℃ to finish the reaction. And washing the reaction product with excessive deionized water, centrifuging the reaction product for 3 times, and drying the reaction product in a vacuum oven at 40 ℃ to constant weight to obtain polyaniline-coated graphene. The resistivity of the graphene is 7.5 multiplied by 10 < -4 > omega-m, the graphene begins to precipitate after being placed in xylene for 600 hours, and the conductivity and the compatibility of the graphene are better than those of a comparative example because the surface of the graphene in the embodiment is coated with doped polyaniline.
Claims (10)
1. A preparation method of coating polyaniline-doped graphene surface is characterized by comprising the following steps: the preparation method comprises the following steps of taking graphene, aniline, ammonium persulfate, sodium dodecyl benzene sulfonate, hydrochloric acid, N-methyl pyrrolidone and deionized water as raw materials, coating polyaniline-doped substances on the surface of the graphene by an in-situ polymerization method to prepare modified graphene, wherein the polyaniline-doped substances on the surface of the modified graphene are specifically prepared by the following steps:
(1) taking raw materials according to a certain mass part ratio;
(2) adding graphene and aniline into a mixed solution composed of deionized water and N-methylpyrrolidone, stirring for a period of time, carrying out ultrasonic treatment for a period of time, and standing for 24 hours at room temperature to obtain a dispersion liquid A;
(3) adding ammonium persulfate, sodium dodecyl benzene sulfonate and hydrochloric acid into deionized water, uniformly stirring to obtain a dispersion liquid B, dropwise adding the dispersion liquid B into the dispersion liquid A within a certain time, and reacting at 0 ℃ for a certain time to finish the reaction;
(4) and washing the reaction product with excessive deionized water, centrifuging the reaction product for 3 times, and drying the reaction product at 40-60 ℃ to constant weight to obtain polyaniline-coated graphene.
2. The method for preparing the graphene surface coated and doped polyaniline according to claim 1, which is characterized in that: the raw materials in the step (1) comprise, by mass, 100 parts of graphene, 10-100 parts of aniline, 10-200 parts of ammonium persulfate, 0-50 parts of sodium dodecyl benzene sulfonate, 0-5 parts of hydrochloric acid, 30-100 parts of N-methylpyrrolidone and 1000-4000 parts of deionized water.
3. The method for preparing the graphene surface coated and doped polyaniline according to claim 2, which is characterized in that: the graphene is one of single-layer graphene, double-layer graphene or multi-layer graphene.
4. The method for preparing the graphene surface coated and doped polyaniline according to claim 2, which is characterized in that: the aniline, the ammonium persulfate, the sodium dodecyl benzene sulfonate, the hydrochloric acid and the N-methyl pyrrolidone are chemically pure or analytically pure.
5. The method for preparing the graphene surface coated and doped polyaniline according to claim 2, which is characterized in that: the deionized water meets the minimum grade required by the national standard GB/T1146.1-1997.
6. The method for preparing the graphene surface coated and doped polyaniline according to claim 1, which is characterized in that: and (4) drying in a vacuum oven.
7. The method for preparing the graphene surface coated and doped polyaniline according to claim 2, which is characterized in that: preferably, the raw materials in the step (1) comprise, by mass, 100 parts of graphene, 100 parts of aniline, 200 parts of ammonium persulfate, 50 parts of sodium dodecyl benzene sulfonate, 5 parts of hydrochloric acid, 100 parts of N-methylpyrrolidone and 4000 parts of deionized water.
8. The method for preparing the graphene surface coated and doped polyaniline according to claim 1, which is characterized in that: the stirring time in the step (2) is 1-2 hours.
9. The method for preparing the graphene surface coated and doped polyaniline according to claim 1, which is characterized in that: the ultrasonic treatment time in the step (2) is 10-30 minutes.
10. The method for preparing the graphene surface coated and doped polyaniline according to claim 1, which is characterized in that: in the step (3), the dispersion liquid B is dripped into the dispersion liquid A for 0.5 to 2 hours; reacting for 6-12 hours at 0 ℃.
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