CN105131596B - A kind of preparation method of graphene/polyaniline compound hollow microballoon - Google Patents
A kind of preparation method of graphene/polyaniline compound hollow microballoon Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
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- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
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Abstract
The invention discloses a kind of preparation method of graphene/polyaniline compound hollow microballoon.Grapheme/polyaniline composite material is prepared first, it regard grapheme/polyaniline composite material as particle emulsifying agents (Pickering emulsifying agents), it is dispersed in water as aqueous phase, styrene and initiator are used as oil phase, emulsified, O/W type emulsions are obtained, after dispersed phase styrene polymerization, solvent dissolved polystyrene is used again, obtains graphene/polyaniline compound hollow microballoon.In the present invention graphene/polyaniline compound hollow microballoon is prepared using the method for Pickering emulsion polymerizations, the factors such as consumption, oil-water ratio, shear rate that can be by adjusting emulsifying agent, obtain various sizes of emulsion droplets, can simply and easily hollow regulating microballoon size, method is simply efficient, and obtained tiny balloon has potential application in terms of catalysis, sensor, ultracapacitor.
Description
Technical field：
The present invention relates to the preparation field of graphene composite material, more particularly to a kind of graphene/polyaniline composite hollow
The preparation method of microballoon.
Background technology：
Graphene, is the individual layer bi-dimensional cellular shape structure crystal as formed by the carbon atom of individual layer is tightly packed.Received in carbon
In rice material, graphene has big specific surface area, high conductivity, good chemical property and mechanical stability because of it, inhales
The extensive concern of researchers is drawn.These excellent performances cause graphene to have potential application in numerous areas, such as super electricity
Container, pH sensors, field-effect transistor, gas sensor, biology sensor etc..
Polyaniline is a kind of conducting polymer composite with conjugated molecule structure, with cheap, good environment
Stability, it is excellent electroactive the advantages of and unique doping/solution doping characteristic, in electricity, optics and electrochemical field
Extensive application.In past many decades, grapheme/polyaniline composite material receives the extensive concern of researchers,
Because composite has new or more excellent performance.The characteristic that two-dimensional graphene is easily reunited, makes its actual specific surface area big
Big reduction, have impact on the performance of graphene in actual applications.Therefore, researchers start to probe into three-dimensional grapheme composite wood
Material, to obtain high performance grapheme material.(the Materials Chemistry and Physics, 2012,134 such as Dong：
576-580) using nickel foam as base material, three-dimensional grapheme is obtained by chemical vapour deposition technique (CVD).Obtained three-dimensional grapheme
With continuous three-dimensional communication structure, after it is combined with polyaniline, compared to graphene-polyaniline of conventional two-dimensional structure, it is combined
The chemical property of material is effectively improved.But in article using chemical vapour deposition technique grow graphene, it is necessary to
Carried out under 1000 DEG C of high temperature, reaction can remnants H after terminating2Etc. inflammable and explosive gas, but the three-dimensional grapheme prepared has
Very big porosity (>=95%) and low bulk density, and whole building-up process is relatively complicated.
In recent years, hollow microspheres are widely paid close attention to because of its excellent characteristic, and such as specific surface area is big, density
Small, good penetrability etc..High polymer material, inorganic material, metal oxide materials etc. can be made into hollow-core construction, be released in medicine
Put, be widely used in photoelectric material, the various fields such as catalysis.Current grinding for three-dimensional grapheme/polyaniline composite material
Study carefully less, particularly the graphene composite material of three-dimensional hollow micro-sphere structure.
Preparing the method for hollow microspheres has a variety of, wherein, microemulsion polymerization method is the conventional side for preparing tiny balloon
Method.The emulsion that the emulsion droplets for being adsorbed in oil/water interface by solid particle to stablize are formed is referred to as Pickering emulsions, institute
It is referred to as particle emulsifying agents (otherwise referred to as Pickering emulsifying agents) with emulsifying agent.Pickering emulsions still have traditional table
The characteristic that activating agent stable emulsion in face has, therefore Pickering emulsifying agents can substitute surfactant, and
Pickering emulsions, which compensate for conventional emulsion, has the shortcomings that toxicity, stability is poor, emulsifying agent be difficult to separation with it is not enough.
The content of the invention：
The invention provides a kind of preparation method of graphene/polyaniline compound hollow microballoon material, this method is used
The method of Pickering emulsion polymerizations prepares graphene/polyaniline compound hollow microballoon, without additionally adding in preparation process
Surfactant, technique is simple, and reaction condition is gentleer, and raw material is easy to get, with low cost.
A kind of preparation method of graphene/polyaniline compound hollow microballoon material, comprises the following steps：
(1) preparation of grapheme/polyaniline composite material：Graphene oxide is dispersed in water, hydrazine hydrate is added, 80
Reaction obtains graphene in 6~12 hours at~100 DEG C.Above-mentioned graphene dispersing solution is mixed super with a certain amount of polystyrolsulfon acid
Sonication 12~24 hours, the black dispersion liquid stablized；A certain amount of aniline monomer is added in above-mentioned graphene dispersing solution,
Oxidant ammonium persulfate is added under stirring state and triggers aniline polymerization, the reaction time is 5~10 hours, it is mixed by what is obtained after reaction
Liquid suction filtration, deionized water washing are closed, grapheme/polyaniline composite material is obtained；
(2) graphene/polyaniline/polystyrene is combined the preparation of solid microsphere：By graphene/polyaniline obtained above
Composite, by ultrasonic disperse in certain volume water；It will be added in the dispersion liquid of above-mentioned grapheme/polyaniline composite material
The oil phase styrene (initiator that mass fraction is 0.6~2% is included in oil phase) of certain volume, 1~5 is emulsified using homogenizer
Minute, obtain O/W type emulsions；Emulsion obtained above is placed in 50~60 DEG C of water-baths, reaction 15~24 hours are stood；Will be anti-
Should after product centrifuged, washed 3~5 times with deionized water, 30~40 DEG C of dryings 6~10 hours, obtain stone in vacuum drying oven
Black alkene/polyaniline/polystyrene is combined solid microsphere；
(3) preparation of graphene/polyaniline compound hollow microballoon：Take graphene/polyaniline/polystyrene obtained above
1~3g of compound solid microsphere, adds 20~60mL tetrahydrofurans, stirs 2~4 hours, is completely dissolved to polystyrene, by solution
Centrifugation, is repeatedly washed using tetrahydrofuran, until washing away polystyrene completely；Obtained solid is placed in vacuum drying chamber,
30~40 DEG C of dryings 1~2 hour, obtain graphene/polyaniline compound hollow microballoon.
In step (1), the mass ratio of polystyrolsulfon acid and graphene is 50: 1~200: 1, and sonication treatment time is 15
~24 hours；The mass ratio of aniline monomer and graphene is 0.5: 1~10: 1, and the mass ratio of aniline monomer and ammonium persulfate is 1:
1~4: 1；Ultrasonic power is 200~400W.
In step (2), ultrasonic power is 200~400W, and ultrasonic time is 10~30 minutes；The rotating speed of homogenizer is 8000
~30000rpm；The concentration of composite dispersion liquid is 1~10mg/mL；The volume ratio of oil phase and aqueous phase is 1.5: 1~1: 3；Draw
Hair agent is the oil-soluble initiators of the initiation temperature at 40~65 DEG C such as ABVN, azodiisobutyronitrile.
In step (3), centrifugal speed is 4000~8000rpm, and the time is 2~5 minutes；Take centrifugation after supernatant liquor with etc.
Volume absolute ethyl alcohol is mixed, and no precipitation then proves the complete washes clean of polystyrene.
Compared with prior art, the invention has the advantages that：
(1) can be by adjusting the consumption of emulsifying agent, oil-water ratio, the factor such as shear rate obtains various sizes of emulsion
Drop, can simply and easily hollow regulating microballoon size.
(2) three-dimensional hollow micro-sphere structure, is effectively improved the specific surface area of grapheme/polyaniline composite material, fully
Utilize the advantage of the big specific surface area of graphene.
(3) three-dimensional grapheme/polyaniline hollow-core construction provides highly conductive network for electric transmission, compared to conventional two-dimensional knot
Graphene-polyaniline of structure, the chemical property of composite can be effectively improved, in the side such as sensor, ultracapacitor
Face has potential application.
(4) graphene/polyaniline compound hollow microballoon, method are prepared using the method for Pickering emulsions in the present invention
Simply, efficiently, reaction condition is gentleer, and raw material is easy to get, with low cost.
Embodiment：
Below by embodiment, the present invention is further detailed.
Embodiment 1：
(1) preparation of grapheme/polyaniline composite material：Take 30mg graphene oxides, ultrasonic disperse in 15mL water, to
The DMF (DMF) that 100mL is added in the suspension of the brown obtains uniform graphene oxide dispersion.To
Add at 30 μ L 80 DEG C of hydrazine hydrate and react 10 hours in the dispersion liquid, obtain the graphene dispersing solution of black, then with 2g polyphenyl
The black dispersion liquid that vinyl sulfonic acid mixing ultrasonication is stablized for 12 hours.Then to the graphite that polystyrolsulfon acid is stable
15mg aniline monomer is added in alkene aqueous dispersions, lower addition 15mg ammonium persulfates is stirred vigorously and triggers aniline polymerization, at 0 DEG C
Reaction 12 hours.The composite of graphene/polyaniline is obtained by suction filtration and deionized water washing.
(2) graphene/polyaniline/polystyrene is combined the preparation of solid microsphere：0.0273g is added in 3mL styrene
ABVN as oil phase, take graphene/polyaniline aqueous dispersions and styrene that 3mL mass concentrations are 10mg/mL
In sample bottle, homogeneous 2min prepares Pickering emulsions under 20500rpm rotating speeds on high speed dispersor.Sample bottle is placed in
In 50 DEG C of water-baths, reaction 15 hours are stood.Product after polymerization is washed with deionized, centrifuged, 30 DEG C in vacuum drying oven
Dry 8 hours, obtain graphene/polyaniline/polystyrene and be combined solid microsphere.
(3) preparation of graphene/polyaniline/polystyrene compound hollow microballoon：1g solid microspheres are taken, 20mL tetra- is dissolved in
In hydrogen furans, stir 4 hours, by solution centrifugal, speed is 4000rpm, and the time is 3 minutes, is repeated several times, and is taken upper after centrifugation
Layer clear liquid, mix with isometric ethanol, until without precipitation after mixing, by obtained sample be placed in vacuum drying chamber 30 DEG C it is dry
Dry 1 hour, that is, obtain graphene/polyaniline compound hollow microballoon.
Embodiment 2：
(1) preparation of grapheme/polyaniline composite material：Take 15mg graphene oxides, ultrasonic disperse in 5mL water, to
The DMF (DMF) that 45mL is added in the dispersion liquid of the brown obtains uniform graphene oxide dispersion.To
Add at 50 μ L 90 DEG C of hydrazine hydrate and react 10 hours in the dispersion liquid, obtain the graphene dispersing solution of black.With 2g polyphenyl second
The black dispersion liquid that alkene sulfonic acid mixing ultrasonication is stablized for 15 hours.Then to the graphene that polystyrolsulfon acid is stable
45mg aniline monomer is added in aqueous dispersions, lower addition 25mg ammonium persulfates is stirred vigorously and triggers aniline polymerization, it is anti-at 0 DEG C
Answer 18 hours.The composite of graphene/polyaniline is obtained by suction filtration and deionized water washing.
(2) graphene/polyaniline/polystyrene is combined the preparation of solid microsphere：0.0546g is added in 4mL styrene
ABVN as oil phase, take graphene/polyaniline aqueous dispersions that 6mL mass concentrations are 5mg/mL and styrene in
In sample bottle, homogeneous 5min prepares Pickering emulsions under 8000rpm rotating speeds on high speed dispersor.Sample bottle is placed in 55
In DEG C water-bath, reaction 24 hours are stood.Product after polymerization is washed with deionized, centrifuged, is done for 35 DEG C in vacuum drying oven
Dry 6 hours, obtain graphene/polyaniline/polystyrene and be combined solid microsphere.
(3) preparation of graphene/polyaniline/polystyrene compound hollow microballoon：2g solid microspheres are taken, 40mL tetra- is dissolved in
In hydrogen furans, stir 4 hours, by solution centrifugal, speed is 8000rpm, and the time is 2 minutes, is repeated several times, and is taken upper after centrifugation
Layer clear liquid, mix with isometric ethanol, until without precipitation after mixing, by obtained sample be placed in vacuum drying chamber 35 DEG C it is dry
Dry 1 hour, that is, obtain graphene/polyaniline compound hollow microballoon.
Embodiment 3：
(1) preparation of grapheme/polyaniline composite material：Take 15mg graphene oxides, ultrasonic disperse in 5mL water, to
The DMF (DMF) that 45mL is added in the dispersion liquid of the brown obtains uniform graphene oxide dispersion.To
Add at 50 μ L 100 DEG C of hydrazine hydrate and react 6 hours in the dispersion liquid, obtain the graphene dispersing solution of black.With 3g polyphenyl second
The black dispersion liquid that alkene sulfonic acid mixing ultrasonication is stablized for 15 hours.Then to the graphene that polystyrolsulfon acid is stable
150mg aniline monomer is added in aqueous dispersions, lower addition 40mg ammonium persulfates is stirred vigorously and triggers aniline polymerization, at 0 DEG C
Reaction 18 hours.The composite of graphene/polyaniline is obtained by suction filtration and deionized water washing.
(2) graphene/polyaniline/polystyrene is combined the preparation of solid microsphere：0.0546g is added in 4mL styrene
Azodiisobutyronitrile as oil phase, take graphene/polyaniline aqueous dispersions that 6mL mass concentrations are 5mg/mL and styrene in
In sample bottle, homogeneous 5min prepares Pickering emulsions under 8000rpm rotating speeds on high speed dispersor.Sample bottle is placed in 55
In DEG C water-bath, reaction 24 hours are stood.Product after polymerization is washed with deionized, centrifuged, is done for 30 DEG C in vacuum drying oven
Dry 8 hours, obtain graphene/polyaniline/polystyrene and be combined solid microsphere.
(3) preparation of graphene/polyaniline compound hollow microballoon：2g solid microspheres are taken, are dissolved in 40mL tetrahydrofurans,
Stirring 4 hours, by solution centrifugal, speed is 8000rpm, and the time is 2 minutes, is repeated several times, and takes the supernatant liquor after centrifugation, with
Isometric ethanol mixing, until without precipitation after mixing, 30 DEG C of dryings 1 hour are placed in vacuum drying chamber by obtained sample,
Obtain graphene/polyaniline compound hollow microballoon.
Claims (4)
1. a kind of preparation method of graphene/polyaniline compound hollow microballoon, comprises the following steps：
(1) preparation of grapheme/polyaniline composite material：Graphene oxide is dispersed in water, hydrazine hydrate is added, 80~
Reaction obtains graphene in 6~12 hours at 100 DEG C；Above-mentioned graphene dispersing solution is mixed into ultrasound with a certain amount of polystyrolsulfon acid
Processing 12~24 hours, the black dispersion liquid stablized；A certain amount of aniline monomer is added in above-mentioned graphene dispersing solution, is stirred
Oxidant ammonium persulfate is added in the case of mixing and triggers aniline polymerization, the reaction time is 5~10 hours, the mixing that will be obtained after reaction
Liquid suction filtration, deionized water washing, obtain grapheme/polyaniline composite material；
(2) graphene/polyaniline/polystyrene is combined the preparation of solid microsphere：Graphene/polyaniline obtained above is combined
Material, by ultrasonic disperse in certain volume water；It is certain by being added in the dispersion liquid of above-mentioned grapheme/polyaniline composite material
Comprising the initiator that mass fraction is 0.6~2% in the oil phase styrene of volume, oil phase, emulsified 1~5 minute using homogenizer,
Obtain O/W type emulsions；Emulsion obtained above is placed in 50~60 DEG C of water-baths, reaction 15~24 hours are stood；After reacting
Product centrifuged, washed 3~5 times with deionized water, 30~40 DEG C of dryings 6~10 hours in vacuum drying oven, obtain graphene/
Polyaniline/polystyrene is combined solid microsphere；
(3) preparation of graphene/polyaniline compound hollow microballoon：Graphene/polyaniline/polystyrene obtained above is taken to be combined
1~3g of solid microsphere, add 20~60mL tetrahydrofurans, stir 2~4 hours, be completely dissolved to polystyrene, by solution from
The heart, is repeatedly washed using tetrahydrofuran, until washing away polystyrene completely；Obtained solid is placed in vacuum drying chamber, 30
~40 DEG C of dryings 1~2 hour, obtain graphene/polyaniline compound hollow microballoon.
2. a kind of preparation method of graphene/polyaniline compound hollow microballoon according to claim 1, it is characterised in that：
In step (1), the mass ratio of polystyrolsulfon acid and graphene is 50: 1~200: 1, and sonication treatment time is 15~24 hours；
The mass ratio of aniline monomer and graphene is 0.5: 1~10: 1, and the mass ratio of aniline monomer and ammonium persulfate is 1: 1~4: 1；It is super
Acoustical power is 200~400W.
3. a kind of preparation method of graphene/polyaniline compound hollow microballoon according to claim 1, it is characterised in that：
In step (2), ultrasonic power is 200~400W, and ultrasonic time is 10~30 minutes；The rotating speed of homogenizer be 8000~
30000rpm；The concentration of composite dispersion liquid is 1~10mg/mL；The volume ratio of oil phase and aqueous phase is 1.5: 1~1: 3；Trigger
Agent is ABVN, azodiisobutyronitrile.
4. a kind of preparation method of graphene/polyaniline compound hollow microballoon according to claim 1, it is characterised in that：
Centrifugal speed is 4000~8000rpm in step (3), and the time is 2~5 minutes；Take centrifugation after supernatant liquor with equal volume it is anhydrous
Ethanol is mixed, and no precipitation then proves the complete washes clean of polystyrene.
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| CN106084775B (en) * | 2016-06-14 | 2017-11-28 | 齐鲁工业大学 | Three layers of vesica shape polyaniline/graphene composite material and preparation method thereof |
| CN106433121B (en) * | 2016-09-09 | 2018-10-30 | 江南大学 | A kind of preparation method of polyaniline-graphite alkene tiny balloon |
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| CN112980184B (en) * | 2021-02-26 | 2022-02-01 | 江南大学 | Preparation method of ionic liquid modified graphene composite polyaniline hollow microspheres |
| CN114558471B (en) * | 2021-12-25 | 2023-05-09 | 福建师范大学 | Application of terpineol modified graphene oxide nanoparticles in pickering emulsion |
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