CN106146833A - A kind of flexible layer/polyaniline conductive graphene film and preparation method thereof - Google Patents
A kind of flexible layer/polyaniline conductive graphene film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of flexible layer/polyaniline conductive graphene film and preparation method thereof, first use Hummers method to prepare graphene oxide；Utilize chemical method partial reduction graphene oxide；Partial reduction graphene oxide will be obtained sulfonated, obtain sulfonated Graphene；The method using vacuum filtration, by sulfonated Graphene sucking filtration film forming, obtains flexible sulfonated graphene film；Under low temperature, in-situ preparation polyaniline on graphene film, obtain flexible polyaniline graphene film.The flexible polyaniline graphene film prepared according to flexible polyaniline graphene film preparation method of the present invention, mechanical strength is high, flexible folding, and ability of anti-deformation is strong, and prior rich in polyaniline, capacitance density is big, is especially suitable for preparing flexible capacitor.It is expected to be used as on a large scale wearable device.And above-mentioned preparation method is simple, beneficially industrialized production.
Description
Technical field
The invention belongs to the synthesis technical field of grapheme material, particularly to a kind of flexible layer/polyaniline conductive stone
Ink alkene film and preparation method thereof.
Background technology
The quick growth of the wearable device energy storage demand such as the most flexible, flexible, people be badly in need of researching and developing inexpensive, soft,
Flexible ultracapacitor, and electrode material is most important ingredient.Graphene is as a kind of novel two-dimensional nano
Material, widely studied by scientific circles in recent years.As a kind of monatomic sheet layer material, be structure zero dimension fullerene quantum dot, one
The basic structural unit of dimension CNT, due to the crystal structure of its uniqueness, Graphene has much excellent physical chemistry
Matter, such as high mechanical property, thermal conductivity, charge mobility, big specific surface area and the quantum hall effect etc. of uniqueness.So
And, owing to the Ultrahigh of material with carbon element is limited, the capacitive property of ultracapacitor based on graphene nano material does not make us
Satisfied, the most only 100～200F/g.
Polyaniline, as a kind of conducting polymer composite, has high capacitance, has a wide range of applications, the electric capacity of polyaniline
Specially good effect belongs to fake capacitance character, mainly by electrode surface or near surface, quick and reversible redox reaction occurs
Realize energy storage, but as the polyaniline of fake capacitance character, there is born stability poor.
Summary of the invention
It is an object of the invention to provide the preparation of the polyaniline graphene composite film of a kind of good mechanical property, flexible folding
Method.Polyaniline graphene film prepared by the present invention, fine and close being grown between graphene sheet layer of polyaniline, increase stone simultaneously
Ink alkene sheet interlayer spacing, contributes to realizing ion channel, accelerates electronics transfer rate between graphene sheet layer.
To achieve these goals, the present invention is by the following technical solutions: the preparation of a kind of flexible polyaniline graphene film
Method, comprises the following steps:
(1) Hummers method is used to prepare graphene oxide；
(2) chemical method partial reduction graphene oxide is utilized；
(3) partial reduction graphene oxide will be obtained sulfonated, obtain sulfonated Graphene；
(4) method using vacuum filtration, by sulfonated Graphene sucking filtration film forming, obtains flexible sulfonated graphene film；
(5) under low temperature, in-situ preparation polyaniline on graphene film, obtain flexible polyaniline graphene film.
In described step 1, preparing graphene oxide and use expansible graphite to be raw material, size is 5000～10000
Mesh.
Described step 2 prepares concretely comprising the following steps of partial reduction graphene oxide:
(1) configuration concentration is 1～2mol/mL graphene oxide dispersion, and dispersion liquid is warming up to 50～100 DEG C, stirs 10 minutes；
(2) taking 3～5g reducing agents to be slowly added in three times in graphene oxide dispersion, each time interval is 30min；
(3), after reaction 1～2h, it is centrifuged off remaining reducing agent, obtains the graphene oxide of partial reduction.
Described reducing agent is sodium borohydride, hydrazine hydrate or hydroiodic acid.
Described reaction temperature is 40～80 DEG C.
Described step 3 prepared concretely comprising the following steps of sulfonated Graphene:
(1) p-aminobenzene sulfonic acid, fluoboric acid, sodium nitrite is utilized to prepare diazol at low temperatures；
(2) being joined by diazol in partial reduction graphene oxide, stirring reaction 12～24h, reaction temperature is 40 DEG C, obtains
Sulfonated Graphene.
Sulfonated Graphene is first configured to the dispersion liquid of 1～2mol/mL by described step 4, pressure be 0.7～
Vacuum filtration film forming is carried out under 1.5MPa.
Described step 5 prepares concretely comprising the following steps of flexible polyaniline graphene film:
(1) configuration concentration is 5～10mol/mL aniline monomer solution, sulfonated graphene film is immersed in aniline solution 2～5 little
Time；Be aniline monomer well into graphene sheet layer between.
(2) graphene film being full of aniline is transferred in the ammonium persulfate solution that concentration is 5～10mol/mL, in reaction
Temperature is that at 0～10 DEG C, aniline monomer is polymerized, and generation polyaniline fine and close between graphene sheet layer, due to polyaniline
Effect so that graphene film interlamellar spacing increases, and contributes to realizing ion channel, accelerates the transfer rate of electronics.Obtain high connductivity
Polyaniline graphene film；
(3) cleaning polyaniline graphene film with acetone and deionized water, 50 DEG C are dried, and obtain flexible polyaniline graphene film.
Present invention also offers a kind of flexible polyaniline graphene film using above-mentioned preparation method to prepare, polyphenyl in film
Fine and close being grown between graphene sheet layer of amine, increases graphene film interlamellar spacing simultaneously, contributes to realizing ion channel, accelerates
Electronics transfer rate between graphene sheet layer.
First redox graphene, strengthens the electric conductivity of graphene oxide, then graphene oxide is sulfonated, in oxidation
Graphene connects part sulfonic acid group, strengthens the water solublity of Graphene, it is simple to graphene uniform is dispersed in dispersion liquid；By sulfonic acid
Functionalized graphene sucking filtration film forming；Last in-situ preparation polyaniline on graphene film；Obtaining polyaniline graphene film, the present invention obtains
Polyaniline graphene film has the good mechanical property of film, flexible folding, polyaniline rich content, and is evenly distributed.It is suitable for using
In terms of the energy storage of wearable device.
The flexible polyaniline graphene film prepared according to flexible polyaniline graphene film preparation method of the present invention, polyphenyl
Fine and close being grown between graphene sheet layer of amine, increases graphene film interlamellar spacing simultaneously, contributes to realizing ion channel, accelerates
Electronics transfer rate between graphene sheet layer.Mechanical strength is high, flexible folding, and ability of anti-deformation is strong, prior rich in
Polyaniline, due to the effect of polyaniline, increases graphene film interlamellar spacing, contributes to realizing ion channel, accelerate electric transmission rate.
The capacitance density of the flexible layer/polyaniline conductive graphene film finally given, more than 800F/g, is especially suitable for preparing flexible capacitor.
It is expected to be used as on a large scale wearable device.And above-mentioned preparation method is simple, beneficially industrialized production.
Accompanying drawing explanation
Fig. 1 is the high power scanning electron microscope (SEM) photograph of the flexible polyaniline graphene membrane surface of embodiment 1.
Fig. 2 is the flexible polyaniline graphene membrane surface cross section high power scanning electron microscope (SEM) photograph of embodiment 1.
Fig. 3 is that the XRD ray of the flexible layer/polyaniline conductive graphene film of embodiment 1 characterizes structure.
Detailed description of the invention
Below mainly in combination with drawings and the specific embodiments polyaniline graphene film flexible to preparation and preparation method thereof make into
One step detailed description.
Embodiment 1
Preparing of the flexible polyaniline graphene film of the present embodiment is as follows:
Step S1: use graphite to prepare graphene oxide；Hummers method can be used to prepare.
Step S2: utilize chemical method partial reduction graphene oxide；Concrete steps,
(1) it is made into graphene oxide dispersion 1mol/mL；
(2) above-mentioned dispersion liquid is warming up to 50 DEG C, stirs 10 minutes；
(3) take 5mL hydrazine hydrate, be slowly added to successively in graphene oxide dispersion,
(4) reaction 1h, takes out above-mentioned dispersion liquid, is centrifuged off remaining hydrazine hydrate, obtains the graphene oxide of partial reduction.
Step S3: sulfonated to the graphene oxide of partial reduction, strengthens its hydrophilic, concretely comprises the following steps:
(1) p-aminobenzene sulfonic acid, fluoboric acid, sodium nitrite is utilized to prepare diazol at low temperatures
(2) diazol is joined in step 2 gained partial reduction graphene oxide, stirring reaction 12h, reaction temperature 40 DEG C
(3) on graphene oxide, connect sulfonic acid group, obtain sulfonated graphene oxide.
Step S4: by sulfonated graphene oxide sucking filtration film forming；Obtain sulfonated graphene film, concretely comprise the following steps:
(1) sulfonated Graphene is configured to 1mol/mL dispersion liquid.
(2) method using vacuum filtration, obtains sulfonated graphene film.
Step S5: by sulfonated graphene oxide sucking filtration film forming；Obtain sulfonated graphene film, concretely comprise the following steps:
(1) configuration aniline monomer solution (5mol/mL),
(2) sulfonated graphene film is immersed in aniline solution 2 hours, between making aniline well into graphene sheet layer.
(3) again the graphene film being full of aniline is transferred to ammonium persulfate solution.The concentration of ammonium persulfate solution is 5mol/
ML, reaction temperature is 0 DEG C.
(4) under the effect of reducing agent Ammonium persulfate., aniline monomer is polymerized, and generates polyphenyl between graphene sheet layer
Amine, obtains polyaniline graphene composite material, due to the effect of polyaniline, increases graphene film interlamellar spacing, contribute to realizing from
Subchannel, accelerates electric transmission rate.
(5) clean polyaniline graphene film, removal of contamination with acetone and deionized water, obtain pure polyaniline graphene film.
(6) finally will obtain under polyaniline graphene film is at vacuum drying oven, 50 DEG C are dried, and obtain flexible polyaniline stone
Ink alkene film.
By observing the Electronic Speculum graph discovery of flexible polyaniline graphene film of example 1 preparation, cutting of the surface of film and film
Face all grown substantial amounts of polyaniline, is implicitly present in a large amount of polyaniline on explanation graphene sheet layer.Meanwhile, XRD diffraction patterns
Showing, the sheet interlayer spacing between Graphene is more than normal graphene film interlamellar spacing.
Embodiment 2
Preparing of the flexible polyaniline graphene film of the present embodiment is as follows:
Step S1: use graphite to prepare graphene oxide；Hummers method can be used to prepare.
Step S2: utilize chemical method partial reduction graphene oxide；Concrete steps,
(1) it is made into graphene oxide dispersion 1mol/mL；
(2) above-mentioned dispersion liquid is warming up to 80 DEG C, stirs 10 minutes
(3) take 5g sodium borohydride and be divided into 3 parts, be slowly added to successively in graphene oxide dispersion, between the time of every twice addition
It is divided into 30min,
(4) reaction 2h, takes out above-mentioned dispersion liquid, is centrifuged off remaining sodium borohydride, obtains the graphene oxide of partial reduction.
Step S3: sulfonated to the graphene oxide of partial reduction, strengthens its hydrophilic, concretely comprises the following steps:
(1) p-aminobenzene sulfonic acid, fluoboric acid, sodium nitrite is utilized to prepare diazol at low temperatures
(2) diazol is joined in step 2 gained partial reduction graphene oxide, stirring reaction 12h, reaction temperature 40 DEG C
(3) on graphene oxide, connect sulfonic acid group, obtain sulfonated graphene oxide.
Step S4: by sulfonated graphene oxide sucking filtration film forming；Obtain sulfonated graphene film, concretely comprise the following steps:
(1) sulfonated Graphene is configured to 2mol/mL dispersion liquid.
(2) method using vacuum filtration, obtains sulfonated graphene film.
Step S5: by sulfonated graphene oxide sucking filtration film forming；Obtain sulfonated graphene film, concretely comprise the following steps:
(1) configuration aniline monomer solution (5mol/mL),
(2) sulfonated graphene film is immersed in aniline solution 5 hours, between making aniline well into graphene sheet layer.
(3) again the graphene film being full of aniline is transferred to ammonium persulfate solution.The concentration of ammonium persulfate solution is 5mol/
ML, reaction temperature is 0 DEG C.
(4) under the effect of reducing agent Ammonium persulfate., aniline monomer is polymerized, and generates polyphenyl in the graphene sheet layer time
Amine, obtains polyaniline graphene composite material, due to the effect of polyaniline, increases graphene film interlamellar spacing, contribute to realizing from
Subchannel, accelerates electric transmission rate.
(5) clean polyaniline graphene film, removal of contamination with acetone and deionized water, obtain pure polyaniline graphene film.
(6) finally will obtain under polyaniline graphene film is at vacuum drying oven, 50 DEG C are dried, and obtain flexible polyaniline stone
Ink alkene film.
Embodiment 3
Preparing of the flexible polyaniline graphene film of the present embodiment is as follows:
Step S1: use graphite to prepare graphene oxide；Hummers method can be used to prepare.
Step S2: utilize chemical method partial reduction graphene oxide；Concrete steps,
(1) it is made into graphene oxide dispersion 1mol/mL；
(2) above-mentioned dispersion liquid is warming up to 50 DEG C, stirs 10 minutes
(3) take 5mL hydroiodic acid, be slowly added in graphene oxide dispersion,
(4) reaction 2h, takes out above-mentioned dispersion liquid, is centrifuged off remaining sodium borohydride, obtains the graphene oxide of partial reduction.
Step S3: sulfonated to the graphene oxide of partial reduction, strengthens its hydrophilic, concretely comprises the following steps:
(1) p-aminobenzene sulfonic acid, fluoboric acid, sodium nitrite is utilized to prepare diazol at low temperatures
(2) diazol is joined in step 2 gained partial reduction graphene oxide, stirring reaction 12h, reaction temperature 40 DEG C
(3) on graphene oxide, connect sulfonic acid group, obtain sulfonated graphene oxide.
Step S4: by sulfonated graphene oxide sucking filtration film forming；Obtain sulfonated graphene film, concretely comprise the following steps:
(1) sulfonated Graphene is configured to 1mol/mL dispersion liquid.
(2) method using vacuum filtration, obtains sulfonated graphene film.
Step S5: by sulfonated graphene oxide sucking filtration film forming；Obtain sulfonated graphene film, concretely comprise the following steps:
(1) configuration aniline monomer solution (5mol/mL),
(2) sulfonated graphene film is immersed in aniline solution 2～5 hours, between making aniline well into graphene sheet layer.
(3) again the graphene film being full of aniline is transferred to ammonium persulfate solution.The concentration of ammonium persulfate solution is 5mol/
ML, reaction temperature is 0 DEG C.
(4) under the effect of reducing agent Ammonium persulfate., aniline monomer is polymerized, and generates polyphenyl in the graphene sheet layer time
Amine, obtains polyaniline graphene composite material, due to the effect of polyaniline, increases graphene film interlamellar spacing, contribute to realizing from
Subchannel, accelerates electric transmission rate.
(5) clean polyaniline graphene film, removal of contamination with acetone and deionized water, obtain pure polyaniline graphene film.
(6) finally will obtain under polyaniline graphene film is at vacuum drying oven, 50 DEG C are dried, and obtain flexible polyaniline stone
Ink alkene film.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Therefore the restriction to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that, for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. the preparation method of a flexible layer/polyaniline conductive graphene film, it is characterised in that comprise the following steps:
(1) Hummers method is used to prepare graphene oxide；
(2) chemical method partial reduction graphene oxide is utilized；
(3) partial reduction graphene oxide will be obtained sulfonated, obtain sulfonated Graphene；
(4) method using vacuum filtration, by sulfonated Graphene sucking filtration film forming, obtains flexible sulfonated graphene film；
(5) under low temperature, in-situ preparation polyaniline on graphene film, obtain flexible polyaniline graphene film.
Flexible polyaniline graphene film preparation method the most according to claim 1, it is characterised in that: in described step 1, system
Standby graphene oxide uses expansible graphite to be raw material, and size is 5000～10000 mesh.
Flexible polyaniline graphene film preparation method the most according to claim 1, it is characterised in that: prepared by described step 2
Concretely comprising the following steps of partial reduction graphene oxide:
(1) configuration concentration is 1～2mol/mL graphene oxide dispersion, and dispersion liquid is warming up to 50～100 DEG C, stirs 10 minutes；
(2) taking 3～5g reducing agents to be slowly added in three times in graphene oxide dispersion, each time interval is 30min；
(3), after reaction 1～2h, it is centrifuged off remaining reducing agent, obtains the graphene oxide of partial reduction.
Flexible polyaniline graphene film preparation method the most according to claim 3, it is characterised in that: described reducing agent is boron
Sodium hydride, hydrazine hydrate or hydroiodic acid.
Flexible polyaniline graphene film preparation method the most according to claim 3, it is characterised in that: described reaction temperature is
40～80 DEG C.
Flexible polyaniline graphene film preparation method the most according to claim 1, it is characterised in that: described step 3 is made
Concretely comprising the following steps of standby sulfonated Graphene:
(1) p-aminobenzene sulfonic acid, fluoboric acid, sodium nitrite is utilized to prepare diazol at low temperatures；
(2) being joined by diazol in partial reduction graphene oxide, stirring reaction 12～24h, reaction temperature is 40 DEG C, obtains
Sulfonated Graphene.
Flexible polyaniline graphene film preparation method the most according to claim 1, it is characterised in that: in described step 4 first
Sulfonated Graphene is configured to the dispersion liquid of 1～2mol/mL, under pressure is 0.7～1.5MPa, carries out vacuum filtration one-tenth
Film.
Flexible polyaniline graphene film preparation method the most according to claim 1, it is characterised in that: prepared by described step 5
Concretely comprising the following steps of flexible polyaniline graphene film:
(1) configuration concentration is 5～10mol/mL aniline monomer solution, sulfonated graphene film is immersed in aniline solution 2～5 little
Time；
(2) graphene film being full of aniline is transferred in the ammonium persulfate solution that concentration is 5～10mol/mL, in reaction temperature
It is that at 0～10 DEG C, aniline monomer is polymerized, generates polyaniline in the graphene sheet layer time, obtain polyaniline graphene film；
(3) cleaning polyaniline graphene film with acetone and deionized water, 50 DEG C are dried, and obtain flexible polyaniline graphene film.
9. a flexible layer/polyaniline conductive graphene film, it is characterised in that: in described layer/polyaniline conductive graphene film, polyaniline causes
Close is grown between graphene sheet layer, increases graphene film interlamellar spacing simultaneously, and described layer/polyaniline conductive graphene film uses
The arbitrary described preparation method of the claims 1 to 8 is prepared from.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108593167A (en) * | 2018-03-20 | 2018-09-28 | 武汉铂纳智感科技有限公司 | A kind of flexible electronic skin and preparation method thereof of while sensed pressure and air-sensitive |
| CN109517382A (en) * | 2018-10-19 | 2019-03-26 | 孙薇薇 | A kind of polyaniline graphene conductive film used for solar batteries and preparation method thereof |
| CN110339733A (en) * | 2019-06-21 | 2019-10-18 | 广东工业大学 | A kind of graphene oxide/polyaniline composite film and its application |
| CN111554521A (en) * | 2020-05-11 | 2020-08-18 | 中国海洋大学 | Preparation method of graphene/polyaniline flexible thin film electrode material |
| CN113659284A (en) * | 2021-08-05 | 2021-11-16 | 合肥国轩高科动力能源有限公司 | Diaphragm for lithium-sulfur battery and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108593167A (en) * | 2018-03-20 | 2018-09-28 | 武汉铂纳智感科技有限公司 | A kind of flexible electronic skin and preparation method thereof of while sensed pressure and air-sensitive |
| CN109517382A (en) * | 2018-10-19 | 2019-03-26 | 孙薇薇 | A kind of polyaniline graphene conductive film used for solar batteries and preparation method thereof |
| CN110339733A (en) * | 2019-06-21 | 2019-10-18 | 广东工业大学 | A kind of graphene oxide/polyaniline composite film and its application |
| CN110339733B (en) * | 2019-06-21 | 2022-01-28 | 广东工业大学 | Graphene oxide/polyaniline composite membrane and application thereof |
| CN111554521A (en) * | 2020-05-11 | 2020-08-18 | 中国海洋大学 | Preparation method of graphene/polyaniline flexible thin film electrode material |
| CN111554521B (en) * | 2020-05-11 | 2021-07-30 | 中国海洋大学 | Preparation method of graphene/polyaniline flexible thin film electrode material |
| CN113659284A (en) * | 2021-08-05 | 2021-11-16 | 合肥国轩高科动力能源有限公司 | Diaphragm for lithium-sulfur battery and preparation method thereof |
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