CN107381559A - Two-dimensional graphene and preparation method thereof - Google Patents
Two-dimensional graphene and preparation method thereof Download PDFInfo
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- CN107381559A CN107381559A CN201710792263.4A CN201710792263A CN107381559A CN 107381559 A CN107381559 A CN 107381559A CN 201710792263 A CN201710792263 A CN 201710792263A CN 107381559 A CN107381559 A CN 107381559A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The present invention provides two-dimensional graphene and preparation method thereof, and the preparation method comprises the following steps：Step 1, it is graphite and additive is scattered in aqueous, obtain mixed liquor；Step 2, recirculation gas stripper is carried out by cutter to the mixed liquor, obtains suspension；Step 3, suspension is stood, obtains standing supernatant and staticly settle；Step 4, the standing supernatant is separated by continuous centrifugal, the suspension of isolated two-dimensional graphene and the nano graphite flakes as centrifugation.The preparation method of two-dimensional graphene according to embodiments of the present invention can obtain the two-dimensional graphene of high quality, and the preparation method is simple and easy, and size is controllable, high efficiency, low cost, green, be adapted to large-scale production.
Description
Technical field
The present invention relates to the preparation field of nano material, more particularly, to two-dimensional graphene and preparation method thereof.
Background technology
New nano material, the preparation and application research of two-dimension nano materials turn into the focus of Material Field.Two wieners
Rice material is the nano material of a kind of individual layer or few layer, shows the properties such as the mechanics, optics, magnetics of uniqueness, is had good
Application potential.Such as：Graphene is a kind of SP2The regular hexagon of hydbridized carbon atoms composition is in the two-dimensional nano of honeycomb lattice
Material.The ultra-thin two-dimensional structure of graphene makes it have some remarkable physics, chemical property, such as quantum tunneling efficiency,
Dual-polarized electricity field-effect, larger theoretical specific surface area, faster electron mobility and higher optical transmittance, excellent machine
Tool performance and thermal conductivity etc..These excellent performances make graphene have good application effect and prospect in fields such as light, electricity.
At present, although can prepare high quality two-dimension nano materials, industrialized extensive high quality of production is realized still
It is the difficult point that govern two-dimension nano materials future commercial applications, therefore solves this difficult point and pay close attention to and grind as people
The focus studied carefully.
At present, the preparation method of two-dimension nano materials has a lot, mainly has：Mechanical stripping method, chemical vapour deposition technique and
Liquid phase stripping method etc., it respectively has merits and demerits.
Mechanical stripping method be by adhesive tape in the plane of large stretch of raw material tear-off repeatedly, utilize the sticky attached of adhesive tape
Put forth effort to overcome the weak Van der Waals force of molecule interlayer, so as to reach the purpose of stripping.This method can obtain the two dimension of high quality
Nano material, but obtained lamella rate is relatively low, and there is contingency, it is difficult to large-scale production.
Reactive material is issued biochemical reaction by chemical vapour deposition technique in gaseous state first, then again in the base of heating
Deposition forms a kind of solid matter on body surface face, thus obtains a kind of technology of solid material.What the preparation method obtained
Two-dimensional nano tablet quality is high, the number of plies is controllable, and yield also improves a lot compared with mechanical stripping method, but this method is to required
Equipment requirement is higher, and because reaction generally requires high temperature, power consumption is larger, considerably increases production cost, and obtained lamella
Must shift to can just possess higher application value after corresponding substrate.
Liquid phase stripping method mainly has organic solvent stripping method, ionic liquid stripping method, surfactant auxiliary aqueous phase to peel off
Method (such as liquid phase ultrasonic method) and mixed solvent stripping method.This method is under the auxiliary of ultrasound etc., and large stretch of stratified material is entered
Row is peeled off.Although this method has the characteristics of simple to operate, convenient, cost is low, low charge stripping efficiency is its major issue.This
Outside, two-dimension nano materials are prepared using ultrasonic method stripping, to be difficult to scale amplification real due to instrument feature in itself and characteristic of experiment
Existing industrialized production.
The content of the invention
In view of this, the present invention provides a kind of two-dimensional graphene.
Present invention also offers a kind of preparation method of two-dimensional graphene.
The preparation method of the two-dimensional graphene of embodiment according to a first aspect of the present invention, comprises the following steps：
Step 1, it is graphite and additive is scattered in aqueous, obtain mixed liquor, the graphite and the additive
Weight ratio is 1：1-30：1；
Step 2, recirculation gas stripper is carried out by cutter to the mixed liquor, obtains suspension；
Step 3, suspension is stood, obtains standing supernatant and staticly settle；
Step 4, to it is described standing supernatant carry out continuous centrifugal separation, obtain two-dimensional graphene suspension and as from
The nano graphite flakes of heart precipitation.
Preferably, the graphite in the step 1 be selected from can swollen graphite, high purity graphite, native graphite, crystalline flake graphite or its
Mixture.
Preferably, the additive in the step 1 includes dispersant and polymer types of surfactants, the dispersant with
The weight ratio of the polymer types of surfactants is 1:1-10：1.
Further, the dispersant is graphite hydrophilic derivatives, and the graphite hydrophilic derivatives are selected from oxidation stone
Ink, vulcanization graphite, carboxyl graphite, graphene quantum dot and its mixture.
Further, the polymer types of surfactants is the compound of hydrophilic high mol containing phenyl ring and its derivative.
Further, the compound of hydrophilic high mol containing phenyl ring be selected from Styrene-acrylic copolymer, styrene-
Methacrylic acid copolymer, SAN, cholic acid and its derivative and its mixture.
Wherein, particularly preferred sodium taurocholate.Because its structure is close with graphene-structured, graphite raw material can be made easily to be dispersed in
In water, while the graphene obtained to stripping has good dispersion effect, it is possible to increase the solid concentration of graphene dispersing solution.With
Other additives, such as Styrene-methyl Acrylic Acid Copolymer are compared, and can increase the amount of 1 milligram of graphene in every milliliter of water.
Preferably, in the step 2, the recirculation gas stripper is carried out under the conditions of 30-90 DEG C of temperature, pH3-11.
Preferably, the precipitation in the step 3) and step 4) is used as lubriation material.
Preferably, the preparation method of two-dimensional graphene also comprises the following steps：
Step 5, the suspension of the two-dimensional graphene is dried, calcined, obtain two-dimensional graphene material after purification
Material.
Further, the drying mode can be freeze-drying or spray drying.
Further, the calcining can be vacuum calcining or be calcined under inert gas atmosphere, reducing gas atmosphere.
The two-dimensional graphene of embodiment according to a second aspect of the present invention, as the system of the two-dimensional graphene described in above-described embodiment
Preparation Method is prepared.
The above-mentioned technical proposal of the present invention has the beneficial effect that：
A kind of preparation method of two-dimensional graphene according to embodiments of the present invention, by the way that graphite is mixed with additive, and
By mixed liquor by cutter recirculation gas stripper, stand, it is that can obtain high quality that will stand supernatant and carry out continuous centrifugal separation
The suspension of two-dimentional two-dimensional graphene, this method is simple and easy, and size is controllable, high efficiency, low cost, green, is adapted to big
Large-scale production.
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method of two-dimensional graphene of the embodiment of the present invention；
Fig. 2 is the SEM figures that the embodiment of the present invention 1 peels off the two-dimensional graphene prepared；
Fig. 3 is the TEM figures that the embodiment of the present invention 1 peels off the two-dimensional graphene prepared.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
Accompanying drawing, the technical scheme of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright part of the embodiment, rather than whole embodiments.Based on described embodiments of the invention, ordinary skill
The every other embodiment that personnel are obtained, belongs to the scope of protection of the invention.
A kind of preparation method of two-dimensional graphene according to embodiments of the present invention is specifically described with reference to accompanying drawing first below.
As shown in figure 1, the preparation method of two-dimension nano materials according to embodiments of the present invention comprises the following steps：
Step 1, it is graphite and additive is scattered in aqueous, obtain mixed liquor, the graphite and the additive
Weight ratio is 1：1-30:1.
Wherein, may be selected from can swollen graphite, high purity graphite, native graphite, crystalline flake graphite etc. or its mixture for graphite.
Additive can be dispersant and polymer types of surfactants, and the dispersant is lived with the species surface that polymerize
Property agent weight ratio be 1：1-10:1.
Preferably, dispersant can be graphite hydrophilic derivatives, and the graphite hydrophilic derivatives can include oxidation
Graphite, vulcanization graphite, carboxyl graphite, graphene quantum dot etc. and its mixture.
Polymer types of surfactants is the compound of hydrophilic high mol containing phenyl ring and its derivative, it is preferable that containing phenyl ring parent
Water high-molecular compound can be selected from Styrene-acrylic copolymer, Styrene-methyl Acrylic Acid Copolymer, styrene-propene
Lonitrile copolymer etc. and its mixture.
Step 2, recirculation gas stripper is carried out by cutter to the mixed liquor, obtains suspension.
Further, the condition of recirculation gas stripper can be 30-90 DEG C in temperature, before pH 3-11, preferably temperature are 60 DEG C
Afterwards, pH=9) under conditions of carry out.
Step 3, suspension is stood, obtains standing supernatant and staticly settle.
Wherein, the nano graphite flakes containing additive, graphene and low layer number in supernatant are stood, traveling one is entered to it
Step processing (referring to following step 4) can obtain graphene.
Step 4, the supernatant is separated by continuous centrifugal, isolated centrifuged supernatant and as centrifugation
Graphene nanometer sheet.
That is, pass through the two-dimensional graphene isolated to the standing further continuous centrifugal of supernatant after standing
Suspension, as two-dimensional graphene, two-dimensional graphene purity height has better performance, and this method is simple and easy, size
Controllable, efficiency high, cost is low, green suitable large-scale production.Step 5, the suspension of the two-dimensional graphene is carried out
Dry, calcining, you can obtain two-dimensional graphene material after purification.
Preferably, the drying mode can be freeze-drying or spray drying.The calcining can be vacuum calcining or
Calcined under inert gas atmosphere, reducing gas atmosphere.Two-dimensional graphene after purification is obtained, advantageously in preservation and fortune
It is defeated.
In addition, the precipitation in above-mentioned steps 3 and 4 can use as high performance lubriation material, to improve the profit of material
With rate, environmental protection and energy saving.
Below, the preparation method of the two-dimensional graphene according to the present invention is further illustrated in conjunction with specific embodiments.
Embodiment 1：
Two-dimensional graphene material is prepared, using DE-200 type high-speed shearing machines, is comprised the following steps：
1) weigh 5g can swollen graphite, using improved Hummers methods, graphite is aoxidized, through persalt and deionization
After the washing of water, freeze-drying, complete oxidation graphite (GO) is prepared, using graphite oxide as additive, weighs oxidation stone
Black 0.2g mixes with 150mL deionized waters, and magneton stirring 30min, obtains dispersion liquid a of the graphite oxide in water.
2) weigh 0.6g can the mixing of swollen graphite and 3g sodium chloride, and grind 20min, form the well mixed grey mixture of colours
Thing, sodium chloride crystal is then cleaned into removal with deionized water, after being handled can swollen graphite, weigh processing after can swollen stone
Black 0.6g and deionized water 300mL is mixed to get dispersion liquid b, and the Sewage treatment of cleaning utilizes.
3) dispersion liquid a and dispersion liquid b are mixed into mixed liquor, and poured into by charging aperture in cutter, in temperature 60 C, pH
It is worth to carry out recirculation gas stripper under conditions of 7, obtains suspension.
4) suspension for obtaining step 3) stands 24h, takes and stands supernatant in the case where rotating speed is 4000rpm, centrifuges 1h, from
The centrifuged supernatant that gains in depth of comprehension arrive is the suspension of two-dimensional graphene, and centrifugation is nano graphite flakes.
In addition, above-mentioned steps 3) and 4) in staticly settle and centrifugation (containing unstripped graphene and oxidation stone
Black alkene) lubriation material can be directly used as.
5) suspension of the isolated two-dimensional graphene of continuous centrifugal in step 4) is freeze-dried, vacuum again
Calcining, the two-dimensional nano-graphene 0.19g purified.
Its SEM photograph and TEM photos are shown in Fig. 2 and Fig. 3.From Fig. 2 and Fig. 3, obtained two-dimensional nano graphite
8.6 μm of the length scale average out to of alkene matter, the number of plies are 3-7 layers.By calculating, it is 31.7% that it, which peels off yield,.Embodiment
2：
Become outside the pale of civilization except following, remaining process is with embodiment 1, i.e.,：Graphite uses native graphite.
Obtained graphene quality is 0.18g, and 8.2 μm of length scale average out to, the number of plies is 5-8 layers, peels off yield and is
30%.
Embodiment 3：
Become outside the pale of civilization except following, remaining process is with embodiment 1, i.e.,：Graphite uses crystalline flake graphite.
Obtained graphene quality is 0.17g, and 9.1 μm of length scale average out to, the number of plies is 3-7 layers, peels off yield and is
28%.
Embodiment 4：
Become outside the pale of civilization except following, remaining process is with embodiment 1, i.e.,：In addition to graphite oxide, styrene-propene also added
Acid copolymer 0.2g is as polymeric surfactant.
Obtained graphene quality is 0.17g, and 8.7 μm of length scale average out to, the number of plies is 5-8 layers, peels off yield and is
29%.
Embodiment 5：
Become outside the pale of civilization except following, remaining process is with embodiment 1, i.e.,：In addition to graphite oxide, sodium taurocholate 0.3g works are also added
For polymeric surfactant, obtained graphene quality is 0.16g, and 8.6 μm of length scale average out to, the number of plies is 3-7 layers, stripping
It is 28% from yield.
Embodiment 6：
Become outside the pale of civilization except following, remaining process is with embodiment 1, i.e.,：For the exfoliation temperature of cutter at 30 DEG C, pH value is 3 bar
Carried out under part.
Obtained graphene quality is 0.18g, and 8.6 μm of length scale average out to, the number of plies is 3-8 layers, peels off yield and is
30%.
Embodiment 7：
Become outside the pale of civilization except following, remaining process is with embodiment 1, i.e.,：For the exfoliation temperature of cutter at 90 DEG C, pH value is 11 bar
Carried out under part.
Obtained graphene quality is 0.16g, and 8.6 μm of length scale average out to, the number of plies is 3-7 layers, peels off yield and is
30%.
Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, on the premise of principle of the present invention is not departed from, some improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (13)
1. a kind of preparation method of two-dimensional graphene, it is characterised in that comprise the following steps：
Step 1, it is graphite and additive is scattered in aqueous, obtain mixed liquor, the weight of the graphite and the additive
Than for 1：1-30：Between 1；
Step 2, recirculation gas stripper is carried out by cutter to the mixed liquor, obtains suspension；
Step 3, the suspension is stood, obtains standing supernatant and staticly settle；
Step 4, continuous centrifugal separation is carried out to the standing supernatant, obtains the suspension of two-dimensional graphene and sunk as centrifugation
The nano graphite flakes in shallow lake.
2. the preparation method of two-dimensional graphene according to claim 1, it is characterised in that the graphite choosing in the step 1
From can swollen graphite, high purity graphite, native graphite, crystalline flake graphite or its mixture.
3. the preparation method of two-dimensional graphene according to claim 1, it is characterised in that the additive in the step 1
Including dispersant and polymer types of surfactants, the weight ratio of the dispersant and the polymer types of surfactants is 1:
1-10：1.
4. the preparation method of two-dimensional graphene according to claim 3, it is characterised in that the dispersant is that graphite is hydrophilic
Property derivative, the graphite hydrophilic derivatives be selected from graphite oxide, vulcanization graphite, carboxyl graphite, graphene quantum dot and
Its mixture.
5. the preparation method of two-dimensional graphene according to claim 3, it is characterised in that the polymerization species surface-active
Agent is the compound of hydrophilic high mol containing phenyl ring and its derivative.
6. the preparation method of two-dimensional graphene according to claim 5, it is characterised in that the hydrophilic high mol containing phenyl ring
Compound is selected from Styrene-acrylic copolymer, Styrene-methyl Acrylic Acid Copolymer, SAN, courage
Acid and its derivative and its mixture.
7. the preparation method of two-dimensional graphene according to claim 6, it is characterised in that the hydrophilic high mol containing phenyl ring
Compound is sodium taurocholate.
8. the preparation method of two-dimensional graphene according to claim 1, it is characterised in that in the step 2, the circulation
Stripping is carried out under the conditions of 30-90 DEG C of temperature, pH3-11.
9. the preparation method of two-dimensional graphene according to claim 1, it is characterised in that will be heavy in the step 3 and 4
Shallow lake is used as lubriation material.
10. the preparation method of two-dimensional graphene according to claim 1, it is characterised in that also comprise the following steps：
Step 5, the suspension of the two-dimensional graphene is dried, calcined, obtain two-dimensional graphene material after purification.
11. the preparation method of two-dimensional graphene according to claim 10, it is characterised in that the drying mode is freezing
Dry or be spray-dried.
12. the preparation method of two-dimensional graphene according to claim 10, it is characterised in that the calcining is vacuum calcining
Or calcined under inert gas atmosphere, reducing gas atmosphere.
13. a kind of two-dimensional graphene, it is characterised in that as the preparation of the two-dimensional graphene described in any one of claim 1 to 12
Method is prepared.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108545734A (en) * | 2018-06-01 | 2018-09-18 | 东莞市鸿亿导热材料有限公司 | A method of preparing ultra-thin two-dimension graphite sheet |
| WO2019184289A1 (en) * | 2018-03-29 | 2019-10-03 | 山东欧铂新材料有限公司 | Method for preparing high-fluidity graphene conductive paste |
| CN114835110A (en) * | 2022-06-08 | 2022-08-02 | 安徽大学 | Application of star-shaped block polymer as dispersing agent in preparation of graphene dispersion liquid |
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| CN105330791A (en) * | 2015-10-28 | 2016-02-17 | 武汉理工大学 | Preparing method of surfactant for stripping compatibility-controllable oxidized graphene |
| CN106566303A (en) * | 2016-10-21 | 2017-04-19 | 成都新柯力化工科技有限公司 | Graphene micro-sheet used for waterborne anticorrosive coating and preparation method thereof |
| CN106672951A (en) * | 2016-12-14 | 2017-05-17 | 北京化工大学 | Environment-friendly, high-efficiency and large-scale graphene preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105217612A (en) * | 2015-09-29 | 2016-01-06 | 北京航空航天大学 | A kind of ultrasonic assistant sand mill peels off the method preparing Graphene and the device peeling off Graphene processed |
| CN105330791A (en) * | 2015-10-28 | 2016-02-17 | 武汉理工大学 | Preparing method of surfactant for stripping compatibility-controllable oxidized graphene |
| CN106566303A (en) * | 2016-10-21 | 2017-04-19 | 成都新柯力化工科技有限公司 | Graphene micro-sheet used for waterborne anticorrosive coating and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019184289A1 (en) * | 2018-03-29 | 2019-10-03 | 山东欧铂新材料有限公司 | Method for preparing high-fluidity graphene conductive paste |
| CN108545734A (en) * | 2018-06-01 | 2018-09-18 | 东莞市鸿亿导热材料有限公司 | A method of preparing ultra-thin two-dimension graphite sheet |
| CN114835110A (en) * | 2022-06-08 | 2022-08-02 | 安徽大学 | Application of star-shaped block polymer as dispersing agent in preparation of graphene dispersion liquid |
| CN114835110B (en) * | 2022-06-08 | 2024-01-05 | 合肥艾克思维新材料科技有限公司 | Application of star-shaped block polymer as dispersing agent in preparation of graphene dispersion liquid |
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