CN109928383A - Ionic liquid base pickering emulsion method prepares graphene/porous carbon materials preparation method - Google Patents
Ionic liquid base pickering emulsion method prepares graphene/porous carbon materials preparation method Download PDFInfo
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- CN109928383A CN109928383A CN201910331151.8A CN201910331151A CN109928383A CN 109928383 A CN109928383 A CN 109928383A CN 201910331151 A CN201910331151 A CN 201910331151A CN 109928383 A CN109928383 A CN 109928383A
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- graphene
- ionic liquid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of ionic liquid base pickering emulsion methods to prepare graphene/porous carbon materials preparation method.Method includes the following steps: being mixed with a certain amount of water and a certain amount of ionic liquid to obtain water/ion liquid microemulsion；It adds graphene oxide into and forms pickering emulsion in ion liquid microemulsion；Carbon source is added in above-mentioned pickering emulsion；Above-mentioned pickering emulsion is prepared into graphene/porous carbon materials by water-heat process.Method provided by the invention promotes the formation of pickering emulsion using the electrostatic interaction between graphene oxide and ionic liquid using graphene oxide as surfactant.After ionic liquid stablizes graphene oxide layer, carbon material polymerize in the another side of stannic oxide/graphene nano lamella.The stabilization of ionic liquid inhibits the reunion of graphene, has obtained a kind of two-dimensional nano chip architecture.The electrode that the composite material being finally prepared can be used as energy storage device uses, and shows excellent chemical property.
Description
Technical field
The present invention relates to ionic liquid base pickering emulsion methods to prepare graphene/porous carbon materials preparation method, this hair
The sulphur anode that bright composite material can be used for high-performance lithium-sulfur cell is modified.
Background technique
Graphene from 2004 by micromechanics stripping method obtained from highly oriented pyrolytic graphite since because its good conductivity,
The advantages that chemical stability height and large specific surface area, has obtained extensive concern.Nanocomposite based on graphene combines
The intrinsic good characteristic of graphene, is used to solve the fields such as energy storage, optics and electronic device and catalysis by numerous studies and deposits
Critical issue.However, existing strong Van der Waals interaction will lead to the serious group of graphene generation between graphene layer
It is poly-.In order to solve this problem, researcher is mainly compound by carrying out two-dimensional graphene and carbon material at present, and formation can be with
The structure of limitation graphene accumulation to a certain extent.However, in above-mentioned preparation process there are complex steps, time-consuming and by institute
Obtained nanocomposite is used to carry the problems such as sulphur space is extremely limited when lithium-sulfur cell sulphur anode.
The reunion for inhibiting graphene using the particular surroundings of ion liquid microemulsion is a simple effective method.From
Sub- liquid is a kind of organic salt being made of completely anions and canons, it is since its thermal stability is good, conductivity is high, vapour pressure pole
The excellent properties such as low, nonflammable, suitable polarity and wide electrochemical window, receive extensive attention, more and more grind
The person of studying carefully is used to volatile organic solvent in substituted chemistry reaction and materials synthesis using ionic liquid as " green solvent ".This
Outside, the advantages of ion liquid microemulsion formed in microemulsion has both both ionic liquid and microemulsion is added in ionic liquid:
Excellent chemical stability, thermal stability be good, wider polarity and programmable ionic liquid structure.In ion liquid microemulsion
In preparation process, surfactant can stablize the dispersion, so choosing suitable surfactant for ionic liquid
The formation of microemulsion has great importance.
The addition of graphene oxide acts not only as the surfactant of ion liquid microemulsion, improves dispersion
Stability, and new unique environments, i.e. pickering emulsion can be constructed, it is that the preparation of next graphene/porous carbon is created
Make advantage.Pickering emulsion refers to the lotion stable by solid particle, and pickering emulsion also there are conventional emulsions to have
Several types, such as oil-in-water type (O/W) lotion, water-in-oil type (W/O) lotion and the double-deck lotion.Compared with conventional emulsion, pik
Woods lotion has itself unique advantage: can form stable lotion, nothing under conditions of being not required to (or a small amount of) emulsifier
Toxicity, it is environmentally friendly, there is advantage in food, medicine and other fields, and almost because of absorption of the solids on oil-water interface
It is irreversible, therefore pickering emulsion has stronger stability.In recent years, pik woods emulsion because its low cost,
The features such as environmental-friendly and stability is high is increasingly valued by people.
Summary of the invention
For graphene agglomeration traits existing for the nanocomposite based on graphene, the object of the present invention is to provide one
Kind can simply prepare graphene/porous carbon composite ionic liquid base pickering emulsion method.
Technical solution of the present invention:
Ionic liquid base pickering emulsion method prepares graphene/porous carbon materials preparation method, and steps are as follows:
(1) at room temperature, to be that water and ionic liquid ultrasonic mixing are prepared water/ionic liquid by 2:1~8:1 according to volume ratio micro-
Lotion；
(2) it adds graphene oxide into water/ion liquid microemulsion and is ultrasonically formed pickering emulsion, graphene oxide exists
Concentration in pickering emulsion is 2mg/mL~8mg/mL；
(3) carbon source is dispersed in pickering emulsion, the mass ratio of carbon source and graphene oxide is 4:1~10:1；
(4) under the conditions of 160 DEG C~200 DEG C of temperature, pickering emulsion hydro-thermal reaction that step (3) is obtained 12 hours~
24 hours, obtain composite material precursors；By composite material precursors successively by freeze-drying one night, high temperature cabonization, pickling and 80
Graphene/porous carbon materials are obtained after being dried overnight at DEG C.
The high temperature cabonization, in the case where environment is argon gas or helium inert atmosphere, under 800 DEG C~1000 DEG C hot conditions
Be carbonized 2h~5h.
The ionic liquid is 1- butyl -3- methylimidazole hexafluorophosphate ([BMIm] PF6), 1- hexyl -3- methyl
Limidazolium hexafluorophosphate ([HMIm] PF6), 1- octyl -3- butyl imidazole hexafluorophosphate ([OMIm] PF6), 1- butyl -3- methyl
Imidazoles iron chloride ([BMIm] [FeCl4]), double trifluoromethanesulfonimide salt ([the BMIm] [Tf of 1- butyl -3- methylimidazole2N])、
Double trifluoromethanesulfonimide salt ([the HMIm] [Tf of 1- hexyl -3- methylimidazole2N]), the double fluoroforms of 1- octyl -3- butyl imidazole
Alkane sulfimide salt ([OMIm] [Tf2N]), 1- ethyl acetate base -3- methylimidazole hexafluorophosphate ([EAMIm] PF6), 1- alkene
Propyl -3- methylimidazole hexafluorophosphate ([AMIm] PF6) one or more of mixing.
The carbon material is glucose, fructose, galactolipin, lactose, sucrose, maltose, starch, chitosan, cyclodextrin
One or more of mixing.
The graphene oxide is the suspension of 10mg/mL~20mg/mL.
The pickling is one of hydrochloric acid, nitric acid, sulfuric acid of 1mol/L.
Graphene/the porous carbon materials can be used in energy accumulating device, and wherein energy accumulating device is capacitor, surpasses
Grade capacitor or rechargeable battery.
Beneficial effects of the present invention: the present invention is using graphene oxide as surfactant, using ionic liquid Ji Pikelin
Emulsion method is prepared for graphene/porous carbon nano-composite material.Cation in surface of graphene oxide negative electrical charge and ionic liquid
Between electrostatic interaction promote the formation of pickering emulsion.After ionic liquid stablizes graphene oxide layer, the carbon materials of dissolution
Expect to polymerize in the another side of stannic oxide/graphene nano lamella.The stabilization of ionic liquid inhibits the reunion of graphene oxide,
A kind of two-dimensional nano chip architecture is obtained.The composite material being prepared is used as the electrode of energy storage device.
Detailed description of the invention
Fig. 1 is graphene/porous carbon materials scanning electron microscope (SEM) photograph in the embodiment of the present invention 1；
Fig. 2 is graphene/porous carbon materials constant current charge-discharge curve in the embodiment of the present invention 1.
Specific embodiment
The specific embodiment of preparation method of the present invention is given below.Preparation that these embodiments are only used for that the present invention will be described in detail
Method is not intended to limit the protection scope of the claim of this application.
Embodiment 1
(1) graphene oxide is prepared using improved Hummers method.
(2) 1.0mL ionic liquid [BMIm] [FeCl is added into 2.5mL deionized water4], be ultrasonically treated 2h, formed from
Sub- liquid microemulsion.
(3) 35mg graphene oxide is dissolved in 2.5mL deionized water, is dispersed into 14.0mg/mL graphene oxide suspension.
(4) 2.5mL graphene oxide suspension is added in Xiang Shangshu ion liquid microemulsion, is ultrasonically treated 3h, forms skin
Crin lotion.
(5) 1.0g sucrose is dispersed in above-mentioned pickering emulsion, at room temperature, is ultrasonically treated 1h.
(6) it fills this blend into 25mLPTFE liner autoclave, is reacted 20 hours at 180 DEG C.
(7) composite material precursors cleaned after hydro-thermal reaction with ethyl alcohol and deionized water and one night of freeze-drying.
(8) gained powder is mixed with solid KOH according to 3:1 mass ratio, then in 800 DEG C, the tube furnace of Ar gas
4h is managed, heating rate is 5 DEG C/min.
(9) by the composite material of synthesis and 1M HCL aqueous solution ultrasonic mixing 1h, next by black powder suspension mistake
Filter until solution ph reaches 7, is finally dried overnight with ultrapure water at 80 DEG C.
Embodiment 2
(1) graphene oxide is prepared using improved Hummers method.
(2) 1.5mL ionic liquid [BMIm] PF is added into 4mL deionized water6, it is ultrasonically treated 2h, forms ionic liquid
Microemulsion.
(3) 70mg graphene oxide is dissolved in 4mL deionized water, is dispersed into 17.5mg/mL graphene oxide suspension.
(4) 2.5mL graphene oxide suspension is added in Xiang Shangshu ion liquid microemulsion, is ultrasonically treated 3h, forms skin
Crin lotion.
(5) 1.5g glucose is dispersed in above-mentioned pickering emulsion, at room temperature, is ultrasonically treated 1h.
(6) it fills this blend into 25mLPTFE liner autoclave, is reacted 16 hours at 160 DEG C.
(7) composite material precursors cleaned after hydro-thermal reaction with ethyl alcohol and deionized water and one night of freeze-drying.
(8) gained powder is mixed with solid KOH according to 3:1 mass ratio, then in 850 DEG C, the tube furnace of Ar gas
3h is managed, heating rate is 5 DEG C/min.
(9) by the composite material of synthesis and 1M HCL aqueous solution ultrasonic mixing 1h, next by black powder suspension mistake
Filter until solution ph reaches 7, is finally dried overnight with ultrapure water at 80 DEG C.
Embodiment 3
(1) graphene oxide is prepared using improved Hummers method.
(2) 2.0mL ionic liquid [HMIm] [Tf is added into 6mL deionized water2N], it is ultrasonically treated 2h, forms ionic liquid
Body microemulsion.
(3) 70mg graphene oxide is dissolved in 7mL deionized water, is dispersed into 10mg/mL graphene oxide suspension.
(4) 2.5mL graphene oxide suspension is added in Xiang Shangshu ion liquid microemulsion, is ultrasonically treated 3h, forms skin
Crin lotion.
(5) 1.0g galactolipin is dispersed in above-mentioned pickering emulsion, at room temperature, is ultrasonically treated 1h.
(6) it fills this blend into 25mLPTFE liner autoclave, is reacted 22 hours at 190 DEG C.
(7) composite material precursors cleaned after hydro-thermal reaction with ethyl alcohol and deionized water and one night of freeze-drying.
(8) gained powder is mixed with solid KOH according to 3:1 mass ratio, then in 900 DEG C, the tube furnace of Ar gas
2h is managed, heating rate is 5 DEG C/min.
(9) by the composite material of synthesis and 1M HCL aqueous solution ultrasonic mixing 1h, next by black powder suspension mistake
Filter until solution ph reaches 7, is finally dried overnight with ultrapure water at 80 DEG C.
Claims (9)
1. a kind of ionic liquid base pickering emulsion method prepares graphene/porous carbon materials preparation method, which is characterized in that step
It is rapid as follows:
(1) at room temperature, water and ionic liquid ultrasonic mixing are prepared into water/ionic liquid micro emulsion for 2:1~8:1 according to volume ratio
Liquid；
(2) it adds graphene oxide into water/ion liquid microemulsion and is ultrasonically formed pickering emulsion, graphene oxide is in pik
Concentration in woods lotion is 2mg/mL~8mg/mL；
(3) carbon source is dispersed in pickering emulsion, the mass ratio of carbon source and graphene oxide is 4:1~10:1；
(4) under the conditions of 160 DEG C~200 DEG C of temperature, the pickering emulsion hydro-thermal reaction 12 hours~24 that step (3) is obtained is small
When, obtain composite material precursors；By composite material precursors successively by one night of freeze-drying, high temperature cabonization, pickling and 80 DEG C
Graphene/porous carbon materials are obtained after being dried overnight.
2. preparation method according to claim 1, which is characterized in that high temperature cabonization described in step (4) is in environment
Under argon gas or helium inert atmosphere, be carbonized 2h~5h under 800 DEG C~1000 DEG C hot conditions；The pickling is 1mol/L's
Hydrochloric acid, nitric acid or sulfuric acid.
3. preparation method according to claim 1 or 2, which is characterized in that the ionic liquid is 1- butyl -3- methyl
Limidazolium hexafluorophosphate, 1- hexyl -3- methylimidazole hexafluorophosphate, 1- octyl -3- butyl imidazole hexafluorophosphate, 1- fourth
The double trifluoromethanesulfonimide salt of base -3- methylimidazole iron chloride, 1- butyl -3- methylimidazole, 1- hexyl -3- methylimidazole are double
The double trifluoromethanesulfonimide salt of trifluoromethanesulfonimide salt, 1- octyl -3- butyl imidazole, 1- ethyl acetate base -3- methyl
The mixing of one or more of limidazolium hexafluorophosphate, 1- allyl -3- methylimidazole hexafluorophosphate.
4. preparation method according to claim 1 or 2, which is characterized in that the carbon source is glucose, fructose, gala
The mixing of one or more of sugar, lactose, sucrose, maltose, starch, chitosan, cyclodextrin.
5. preparation method according to claim 3, which is characterized in that the carbon source be glucose, fructose, galactolipin,
The mixing of one or more of lactose, sucrose, maltose, starch, chitosan, cyclodextrin.
6. according to claim 1, preparation method described in 2 or 5, which is characterized in that the graphene oxide of addition is in step (2)
The suspension of 10mg/mL~20mg/mL.
7. preparation method according to claim 3, which is characterized in that the graphene oxide added in step (2) is 10mg/
The suspension of mL~20mg/mL.
8. the preparation method according to claim 4, which is characterized in that the graphene oxide added in step (2) is 10mg/
The suspension of mL~20mg/mL.
9. the above-mentioned graphene/porous carbon materials being prepared are used in energy accumulating device, wherein energy accumulating device is electricity
Container, supercapacitor or rechargeable battery.
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| CN110828838A (en) * | 2019-11-22 | 2020-02-21 | 河北师范大学 | Preparation method of palladium-based catalyst with particle size larger than 10 microns and snowflake ball morphology |
| CN112794303A (en) * | 2019-11-14 | 2021-05-14 | 中国科学院化学研究所 | Super-amphiphilic carbon and preparation method and application thereof |
| CN113012945A (en) * | 2021-02-25 | 2021-06-22 | 山东大学 | Modified Ppy-MXene composite material and preparation method and application thereof |
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| CN110408074B (en) * | 2019-08-16 | 2022-05-20 | 哈尔滨工业大学 | Preparation method of alkylation modified graphene oxide-based super-hydrophobic material |
| CN112794303A (en) * | 2019-11-14 | 2021-05-14 | 中国科学院化学研究所 | Super-amphiphilic carbon and preparation method and application thereof |
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| CN110828838A (en) * | 2019-11-22 | 2020-02-21 | 河北师范大学 | Preparation method of palladium-based catalyst with particle size larger than 10 microns and snowflake ball morphology |
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