CN105948026A - Method for preparing graphene through liquid phase chemical technology intercalation and graphite peeling - Google Patents
Method for preparing graphene through liquid phase chemical technology intercalation and graphite peeling Download PDFInfo
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Abstract
The invention provides a method for preparing graphene through liquid phase chemical technology intercalation and graphite peeling, and belongs to the technical field of graphene materials. The problems of complex technology, large energy consumption in the electrolysis process and high oxygen content of present graphene preparation methods are solved. The method comprises the following steps: immersing graphite in a mixed acid solution, adding an intercalator, stirring graphite, the mixed acid solution and the intercalator to obtain a mixed solution; and adding an organic reagent to the mixed solution, and reacting to obtain a water dispersion of graphene. A special reagent is used to carry out intercalation treatment, and a sharp chemical reaction is carried out to instantly gasify the reagent between graphite layers in order to peel graphite into graphene. The yield of graphene prepared through the method is extremely high, the weight of the obtained graphene is almost same to the weight of graphite, the graphene has extremely few defects, the oxygen content of the prepared graphene is 1.63% and is extremely low, and the conductivity of the graphene is high.
Description
Technical field
The invention belongs to grapheme material technical field, be specifically related to a kind of liquid chemical method intercalation and peel off graphite system
The method of standby Graphene.
Background technology
Since Graphene in 2004 comes out, the electrical properties extremely excellent due to it receives widely
Scientific attention.Such as, its carrier transport behavior is similar to the neutrino in the Theory of Relativity, considerable under room temperature
Measure quantum hall effect, the two poles of the earth field effect etc..Further, the physical and mechanical property that Graphene is unique is more
Widen the space of its application: high young's modulus, the coefficient of heat conduction is up to 5300W/mK, theoretical ratio
Surface area is up to 2630m2/ g, and energy gap is adjustable, almost all-transparent, only absorbs the light of 2.3%, and
The performance of his multiple excellence.In the near future, Graphene may be used to prepare out thinner, conduction speed
A new generation's electronic component or electron transistor faster.And due to the good light transmission of Graphene and conduction
Property, it also is adapted for for replacing ITO to manufacture transparent touch-sensitive panel, tabula rasa, even solaode.Graphene
Good mechanical performance has been applied in material contracting with heat or thin-film material improve tensile resistance.Due to
Graphene is considered as the hardest material found so far, so some researchers are being developed by stone
The flak jackets that ink alkene is made, such flak jackets is lighter and thinner, it will soldier is greatly reduced and bears a heavy burden.Stone
The ink high theoretical surface of alkene is amassed, and makes it be applied to catalytic field as the carrier material of catalyst, the most such as
This, its high electrical conductivity can promote photoelectronic transfer, improves exciton lifetime, well improves light and urges
Change efficiency, be applied to photocatalysis field.
Found that Graphene obtained Nobel Prize to the finder of Graphene in 2010 from 2004, and the most several
The increasing that Graphene research is put into by year both at home and abroad, it is anticipated that the demand of Graphene also will be along with
The extension of its application and constantly increase.Therefore one cheap and high yield prepare high-quality Graphene
Means be the most necessary.Grapheme material can be divided into powder body Graphene and thin film Graphene two class, and pin
To different applications, the fields such as wherein powder body Graphene is at the energy, anticorrosion, enhancing application is the widest
General, so the research of preparation method is the most extensive, varied: metal organic matter is catalyzed, electrochemical electrolysis
Carbon electrode method, alkali metal intercalation plavini, alkali metal reduction Ethanol Method, microwave method, oxidation-reduction method.?
In numerous methods, suffering from very important drawback, some method costs are the highest, and productivity is the lowest, has
Method productivity high but the quality of Graphene is the poorest, defect is many, and the bad control of stability tested, and
And most method can consume the highest.
As a example by the graphite preparation method as raw material: electrochemistry auxiliary intercalation is dialled from method (application number
CN201510811360.4) complex process, electrode process energy consumption is relatively big, and time-consumingly；Oxidation-reduction method, band
Carrying out heavy metal pollution, and the quality of graphene generated is the highest, oxygen content and defect are high.
Summary of the invention
The invention aims to solve existing graphene preparation method complex process, electrode process energy consumption
Greatly, and hyperoxic problem, and provide a kind of liquid chemical method intercalation to peel off the side of preparing graphite alkene
Method.
The present invention provides a kind of method that liquid chemical method intercalation peels off preparing graphite alkene, and the method includes:
Step one: be immersed in mixed acid solution by graphite, is subsequently adding intercalator stirring, obtains mixed solution；
Step 2: organic reagent is joined in the mixed solution that step one obtains and react, obtain Graphene
Aqueous dispersions.
Preferably, described graphite is expanded graphite or crystalline flake graphite.
Preferably, described mixed acid solution is made up of strong absorptive concentrated acid and oxidisability concentrated acid.
Preferably, described strong absorptive concentrated acid includes concentrated sulphuric acid, strong phosphoric acid or pyrosulfuric acid.
Preferably, described oxidisability concentrated acid preferably include concentrated nitric acid, pyrosulfuric acid, iodic acid, periodic acid,
Perchloric acid or bromic acid.
Preferably, described strong absorptive concentrated acid and the volume ratio of oxidisability concentrated acid are (0.5-8): (1-2).
Preferably, described intercalator is preferably selected from iodic acid, periodic acid, perchloric acid, bromic acid or chlorosulfonic acid
In one or more.
Preferably, the mixing time of described step one is 6-24 hour.
Preferably, described organic reagent includes hydrazine hydrate, organic amine, the saturated aqueous solution of reproducibility salt
Or the CS of S2Saturated solution.
Preferably, the response time of described step 2 is 2-10min.
Beneficial effects of the present invention
The present invention provides a kind of method that liquid chemical method intercalation peels off preparing graphite alkene, and the method first will
Graphite is immersed in mixed acid solution, is subsequently adding intercalator stirring, obtains mixed solution；Then by organic examination
Agent joins in mixed solution reacts, and obtains the aqueous dispersions of Graphene.Compare with prior art, this
Bright utilize special reagent to carry out intercalation processing after, then by violent chemical reaction by the reagent of graphite layers
Transient evaporation, peels off into Graphene by graphite.Graphene productivity prepared by this method is high, almost has many
Few gram graphite just can separate how many grams of Graphenes, and the Graphene defect obtained is few, the stone prepared
Ink alkene oxygen content only has 1.63%, and oxygen content is extremely low, and electrical conductivity is higher.Utilize various sizes of graphite raw material,
50 microns of-600 microns of arbitrary sizes, especially big size graphenes can be obtained.The graphene film ratio obtained
Surface area is at 200 800m2Between/g, thickness distribution concentrates on 3-8 layer.And stone prepared by the method
Ink alkene, relative to the graphite before peeling off, does not carries out any destruction to the lamella of graphite, maintains graphite former
Some electrical properties.The preparation method of the present invention is simple, convenient production, and energy consumption is low, low for equipment requirements,
It is more suitable for commercial production, processes easily, the shortest.
Accompanying drawing explanation
Fig. 1 is electron scanning micrograph and the transmission electricity of the Graphene that the embodiment of the present invention 1 prepares
Sub-microphotograph；
Fig. 2 is the x-ray photoelectron energy spectrogram of the Graphene that the embodiment of the present invention 1 prepares；
Fig. 3 is the Raman figure of the Graphene that the embodiment of the present invention 1 prepares.
Detailed description of the invention
The present invention provides a kind of method that liquid chemical method intercalation peels off preparing graphite alkene, and the method includes:
Step one: be immersed in mixed acid solution by graphite, is subsequently adding intercalator stirring, obtains mixed solution；
Step 2: organic reagent is joined in the mixed solution that step one obtains and react, obtain Graphene
Aqueous dispersions.
According to the present invention, first graphite is immersed in mixed acid solution, is subsequently adding intercalator stirring, is mixed
Close solution；Described mixing time is preferably 6-24 hour, the most before stirring, is first carried out by mixture
Having children outside the state plan, the described excusing from death time is preferably 30min；The quality (g) of described graphite: the body of mixed acid solution
Long-pending (ml) is preferably 10:(200-1000).In order to increase severe degree and the discharge quantity of reaction, preferably exist
Adding inorganic salt during immersion, make peeling effect more preferable, the addition of described inorganic salt is preferably graphite quality
10-50%, described inorganic salt preferably includes ammonium nitrate, potassium chlorate, potassium hyperchlorate, lithium chlorate, high chlorine
Acid lithium, phosphorus pentoxide or Ammonium persulfate..
According to the present invention, described graphite is preferably expanded graphite or the crystalline flake graphite of commercialization, described stone
The carbon content of ink is preferably more than 98%；Described mixed acid solution is preferably dense by strong absorptive concentrated acid and oxidisability
Acid composition, strong absorptive concentrated acid preferably includes concentrated sulphuric acid, strong phosphoric acid or pyrosulfuric acid, and oxidisability concentrated acid preferably wraps
Include concentrated nitric acid, pyrosulfuric acid, iodic acid, periodic acid, perchloric acid or bromic acid；Described intercalator is preferably selected from iodine
One or more in acid, periodic acid, perchloric acid, bromic acid or chlorosulfonic acid；Described strong absorptive concentrated acid,
The volume ratio of oxidisability concentrated acid and intercalator is preferably (0.5-8): (1-3): 1；
According to the present invention, organic reagent joining stirring reaction in above-mentioned mixed solution, abnormal reaction is violent,
During until flowable mixed liquor becomes the gel close to solid phase, reaction terminates, and is washed by above-mentioned gel,
Gained gel is cleaned to neutral, by supersound process, the graphene dispersing solution of gained is preferably disperseed, this
The Graphene lumpd in cleaning process can be separated by sample, becomes fluffy cotton-shaped, described sonication treatment time
It is preferably 30 minutes, i.e. can get the aqueous dispersions of Graphene.
Preferably, described organic reagent is preferably the organic reagent containing reducing agent, more preferably includes water
Close hydrazine, organic amine, the saturated aqueous solution of reproducibility salt or the CS of S2Saturated solution；Described organic amine is excellent
Choosing includes ethylenediamine or the third three；The saturated aqueous solution of reproducibility salt preferably includes NaS2、Na2S2O3Or
Na2S2O4；Described nitration mixture and the volume ratio of organic reagent are preferably (2-10): (1-5)；Described stirring
Response time is 2-10min.
According to the present invention, the Graphene in order to make reaction finally give disperses more preferably in water, preferably can be
Mixed acid solution adds organic surface active agent, it is possible to after the completion of reaction, gel is dissolved in polarity organic molten
In agent, the most ultrasonic washing adjusts pH value, and the graphene dispersion so obtained is more preferable, and monolayer is more
Many, it is to avoid certain Second Aggregation.The addition of described organic surface active agent is preferably graphite quality
5-25%, preferably include PVP, PVA, PSS, dodecyl sodium sulfate, cetyl benzenesulfonic acid sodium,
Triton X-100, P123, P127 or CMC；Described polar organic solvent is preferably methylformamide
(DMF), N methyl pyrrolidone (NMP) or dimethyl sulfoxide (DMSO)；Described nitration mixture and pole
The volume ratio of property organic reagent is (2-10): (5-10)
The present invention a kind of liquid chemical method intercalation peels off the method for preparing graphite alkene, is by graphite
Learning intercalation, then in solid phase or liquid phase, intercalation compound in graphite enters with other reagent added
The violent chemical reaction of row, discharges gas and is strutted by graphite and peel off into Graphene.The graphite that the method obtains
Alkene is not through redox process, and defect is less, and electrical conductivity is higher, close to ideal state.
Being further elaborated the present invention below in conjunction with embodiment, the raw material related in embodiment is business
Available from.
Embodiment 1
10g expanded graphite (25 mesh) is joined in 200mL nitration mixture (concentrated sulphuric acid and concentrated nitric acid), so
Rear addition perchloric acid, the denseest H2SO4/HClO4/ dense HNO3=0.5/1/1, stir and close,
After supersound process 30 minutes, magnetic agitation 6 hours, then it is slowly added dropwise in mixed liquor while stirring
100mL hydrazine hydrate solution, stirs 2min, and said mixture can drastically expand by volume, becomes dark thick glue
Body, cleans gained gel to neutral with deionized water, and excusing from death processes 30min, obtains the moisture of Graphene
Dissipate liquid.
Fig. 1 is that the electron scanning micrograph (a) of the Graphene that the embodiment of the present invention 1 prepares is with saturating
Penetrate electron micrograph (b)；It can be seen that graphite is by nitration mixture intercalation the play with reducing agent from Fig. 1 a
Strong reaction has been lifted off of, and owing to there is a lot of folds in reaction very acutely graphene layer, defines
The flower-like structure of porous.From transmission electron microscope figure it will be seen that as shown in Figure 1 b, this Graphene is
There is the transparent membrane of micron-scale.
Fig. 2 is the x-ray photoelectron power spectrum that liquid phase directly peels off the Graphene obtained；Figure it is seen that
The oxygen content of the Graphene of the present invention is extremely low, and only 1.63%.
Fig. 3 is the Raman figure of the Graphene that the embodiment of the present invention 1 prepares, Fig. 3 it can be seen that this
Graphene defect content prepared by bright method is extremely low, and it can be seen that graphited 2D peak structure, this explanation
Prepared quality of graphene is high, close to the Graphene of perfect condition.
Embodiment 2
10g crystalline flake graphite (200 mesh) is joined in 1L nitration mixture (concentrated sulphuric acid and concentrated nitric acid), then
Add bromic acid, the denseest H2SO4/HBrO3/ dense HNO3=8/1/3, stir and close, ultrasonic place
After managing 30 minutes, magnetic agitation 24 hours, then while stirring, in mixed liquor, it is slowly added dropwise 500mL
Hydrazine hydrate solution, stirs 10min, and said mixture can drastically expand by volume, becomes dark thick colloid, uses
Gained gel is cleaned to neutral by deionized water, and excusing from death processes 30min, obtains the aqueous dispersions of Graphene.
Test result indicate that: the oxygen content of the Graphene that embodiment 2 prepares is 1.98%.
Embodiment 3
10g crystalline flake graphite (100 mesh) is joined in 500mL nitration mixture (concentrated sulphuric acid and concentrated nitric acid),
It is subsequently adding periodic acid, the denseest H2SO4/HIO4/ dense HNO3=3/1/2, stir and close, super
After sonication 30 minutes, magnetic agitation 12 hours, then it is slowly added dropwise in mixed liquor while stirring
300mL hydrazine hydrate solution, stirs 5min, and said mixture can drastically expand by volume, becomes dark thick glue
Body, cleans gained gel to neutral with deionized water, and excusing from death processes 30min, obtains the moisture of Graphene
Dissipate liquid.
Test result indicate that: the oxygen content of the Graphene that embodiment 3 prepares is 1.71%.
Embodiment 4
10g expanded graphite (25 mesh) is joined in 200mL nitration mixture (concentrated sulphuric acid and concentrated nitric acid), so
Rear addition perchloric acid, the denseest H2SO4/HClO4/ dense HNO3=0.5/1/1, stir and close,
After supersound process 30 minutes, magnetic agitation 6 hours, then it is slowly added dropwise in mixed liquor while stirring
100mL hydrazine hydrate solution, stirs 2min, and said mixture can drastically expand by volume, becomes dark thick glue
Body, joins in 500ml methylformamide (DMF), with deionized water by gained by dark thick colloid
Gel cleans to neutral, and excusing from death processes 30min, obtains the aqueous dispersions of Graphene.
Embodiment 5
10g expanded graphite (25 mesh) and 0.5g dodecyl sodium sulfate are joined 200mL nitration mixture (dense
Sulphuric acid and concentrated nitric acid) in, it is subsequently adding perchloric acid, the denseest H2SO4/HClO4/ dense HNO3=0.5/1/
1, stir and close, supersound process is after 30 minutes, magnetic agitation 6 hours, then same in stirring
Time in mixed liquor, be slowly added dropwise 100mL hydrazine hydrate solution, stir 2min, said mixture can volume anxious
Acute expansion, becomes dark thick colloid, dark thick colloid joins 500ml methylformamide (DMF)
In, with deionized water, gained gel to be cleaned to neutral, excusing from death processes 30min, obtains the moisture of Graphene
Dissipate liquid.
Embodiment 6
10g expanded graphite (25 mesh) and 2.5g ammonium nitrate are joined 200mL nitration mixture (concentrated sulphuric acid and dense
Nitric acid) in, it is subsequently adding perchloric acid, the denseest H2SO4/HClO4/ dense HNO3=0.5/1/1, stirring
Uniformly closing, supersound process is after 30 minutes, and magnetic agitation 6 hours, then to mixing while stirring
Being slowly added dropwise 100mL hydrazine hydrate solution in liquid, stir 2min, said mixture can drastically expand by volume,
Become dark thick colloid, dark thick colloid is joined in 500ml methylformamide (DMF), use
Gained gel is cleaned to neutral by deionized water, and excusing from death processes 30min, obtains the aqueous dispersions of Graphene.
Embodiment 7
10g expanded graphite (25 mesh) is joined in 200mL nitration mixture (concentrated sulphuric acid and concentrated nitric acid), so
Rear addition perchloric acid, the denseest H2SO4/HClO4/ dense HNO3=0.5/1/1, stir and close,
After supersound process 30 minutes, magnetic agitation 6 hours, then it is slowly added dropwise in mixed liquor while stirring
100mL Na2S2O4Saturated aqueous solution, stir 2min, said mixture can volume drastically expand, become
Dark thick colloid, joins dark thick colloid in 500ml methylformamide (DMF), spend from
Gained gel is cleaned to neutral by sub-water, and excusing from death processes 30min, obtains the aqueous dispersions of Graphene.
Claims (10)
1. the method that a liquid chemical method intercalation peels off preparing graphite alkene, it is characterised in that the method
Including:
Step one: be immersed in mixed acid solution by graphite, is subsequently adding intercalator stirring, obtains mixed solution；
Step 2: organic reagent is joined in the mixed solution that step one obtains and react, obtain Graphene
Aqueous dispersions.
A kind of liquid chemical method intercalation the most according to claim 1 peels off the method for preparing graphite alkene,
It is characterized in that, described graphite is expanded graphite or crystalline flake graphite.
A kind of liquid chemical method intercalation the most according to claim 1 peels off the method for preparing graphite alkene,
It is characterized in that, described mixed acid solution is made up of strong absorptive concentrated acid and oxidisability concentrated acid.
A kind of liquid chemical method intercalation the most according to claim 3 peels off the method for preparing graphite alkene,
It is characterized in that, described strong absorptive concentrated acid includes concentrated sulphuric acid, strong phosphoric acid or pyrosulfuric acid.
A kind of liquid chemical method intercalation the most according to claim 3 peels off the method for preparing graphite alkene,
It is characterized in that, described oxidisability concentrated acid preferably includes concentrated nitric acid, pyrosulfuric acid, iodic acid, periodic acid, height
Chloric acid or bromic acid.
A kind of liquid chemical method intercalation the most according to claim 3 peels off the method for preparing graphite alkene,
It is characterized in that, described strong absorptive concentrated acid and the volume ratio of oxidisability concentrated acid are (0.5-8): (1-2).
A kind of liquid chemical method intercalation the most according to claim 1 peels off the method for preparing graphite alkene,
It is characterized in that, described intercalator is preferably selected from iodic acid, periodic acid, perchloric acid, bromic acid or chlorosulfonic acid
One or more.
A kind of liquid chemical method intercalation the most according to claim 1 peels off the method for preparing graphite alkene,
It is characterized in that, the mixing time of described step one is 6-24 hour.
A kind of liquid chemical method intercalation the most according to claim 1 peels off the method for preparing graphite alkene,
It is characterized in that, described organic reagent includes hydrazine hydrate, organic amine, the saturated aqueous solution of reproducibility salt or S
CS2Saturated solution.
A kind of liquid chemical method intercalation the most according to claim 1 peels off the side of preparing graphite alkene
Method, it is characterised in that the response time of described step 2 is 2-10min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107285302A (en) * | 2017-08-17 | 2017-10-24 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of graphene |
| CN107416813A (en) * | 2017-10-03 | 2017-12-01 | 王干 | A kind of simple and easy method for preparing high-quality graphene |
| CN108428883A (en) * | 2018-04-24 | 2018-08-21 | 盐城师范学院 | A kind of small size edge is grapheme modified with silicon combination electrode material preparation method |
| CN112973640A (en) * | 2021-03-24 | 2021-06-18 | 兰州大学 | Preparation method of 3D printing reduced graphene oxide filter element for treating uranium-containing wastewater |
| WO2021217898A1 (en) * | 2020-04-30 | 2021-11-04 | 北京超思电子技术有限责任公司 | Mixed inorganic acid solvent-based graphene preparation method |
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| CN104556018A (en) * | 2015-01-23 | 2015-04-29 | 青岛科技大学 | Preparation method of high quality graphene conductive film |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107285302A (en) * | 2017-08-17 | 2017-10-24 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of graphene |
| CN107285302B (en) * | 2017-08-17 | 2020-05-26 | 中国科学院宁波材料技术与工程研究所 | Preparation method of graphene |
| CN107416813A (en) * | 2017-10-03 | 2017-12-01 | 王干 | A kind of simple and easy method for preparing high-quality graphene |
| CN108428883A (en) * | 2018-04-24 | 2018-08-21 | 盐城师范学院 | A kind of small size edge is grapheme modified with silicon combination electrode material preparation method |
| WO2021217898A1 (en) * | 2020-04-30 | 2021-11-04 | 北京超思电子技术有限责任公司 | Mixed inorganic acid solvent-based graphene preparation method |
| JP2022544446A (en) * | 2020-04-30 | 2022-10-19 | 北京超思電子技術有限責任公司 | Preparation of graphene based on mixed inorganic acid solvents |
| JP7374235B2 (en) | 2020-04-30 | 2023-11-06 | 北京超思電子技術有限責任公司 | Preparation method of graphene based on mixed inorganic acid solvent |
| CN112973640A (en) * | 2021-03-24 | 2021-06-18 | 兰州大学 | Preparation method of 3D printing reduced graphene oxide filter element for treating uranium-containing wastewater |
| CN112973640B (en) * | 2021-03-24 | 2022-04-15 | 兰州大学 | Preparation method of 3D printing reduced graphene oxide filter element for treating uranium-containing wastewater |
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