CN107585757A - A kind of graphene, nano graphite flakes and preparation method - Google Patents
A kind of graphene, nano graphite flakes and preparation method Download PDFInfo
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- CN107585757A CN107585757A CN201710776576.0A CN201710776576A CN107585757A CN 107585757 A CN107585757 A CN 107585757A CN 201710776576 A CN201710776576 A CN 201710776576A CN 107585757 A CN107585757 A CN 107585757A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 58
- 239000010439 graphite Substances 0.000 title claims abstract description 58
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims description 3
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 229910021383 artificial graphite Inorganic materials 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 18
- 229920002678 cellulose Polymers 0.000 claims description 14
- 239000001913 cellulose Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 11
- 229910001868 water Inorganic materials 0.000 claims description 11
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 10
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 10
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 10
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000004576 sand Substances 0.000 claims description 2
- 150000004040 pyrrolidinones Chemical class 0.000 claims 1
- 239000004566 building material Substances 0.000 abstract description 3
- 239000003575 carbonaceous material Substances 0.000 abstract description 3
- 238000005034 decoration Methods 0.000 abstract description 3
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 3
- 239000011147 inorganic material Substances 0.000 abstract description 3
- 229920000620 organic polymer Polymers 0.000 abstract description 3
- 239000010410 layer Substances 0.000 description 10
- 239000000084 colloidal system Substances 0.000 description 8
- 239000003643 water by type Substances 0.000 description 8
- 239000007787 solid Substances 0.000 description 7
- 239000002002 slurry Substances 0.000 description 6
- 150000001336 alkenes Chemical class 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- -1 dimethyl methyl Chemical group 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to become more meticulous crushing and stripping is carried out to native graphite and synthetic graphite with force chemistry, obtain nano graphite flakes, even obtain few layer nano-graphene piece.The nano graphite flakes of gained and few layer nano-graphene piece are a kind of highly conductive, high heat conduction new type functional carbon materials, both can be compound with organic polymer or compound with inorganic material, have been widely used in the field such as electronics, luminous, battery, building materials, decoration, daily.
Description
Technical field
The present invention relates to become more meticulous crushing and stripping is carried out to native graphite and synthetic graphite with force chemistry, nanometer is obtained
Graphite flake, even obtain few layer nano-graphene piece.The nano graphite flakes of gained and few layer nano-graphene piece are that a kind of height is led
Electricity, the new type functional carbon material of high heat conduction, both can be compound with organic polymer or compound with inorganic material, in electronics, hair
The field such as light, battery, building materials, decoration, daily has been widely used.
Background technology
Graphene is found in two distinguished professors by Univ Manchester UK in 2004.The institute of the graphene of two-dimensional structure
So to attract attention, one is because many unrivaled advantageous properties that itself has, the second is it is thermodynamically
Uniqueness.Before this, scientists are directed to studying the graphite packing for how obtaining the fewer and fewer number of plies always, but are all
It is confined to the graphite material of three-dimensional.It is to be stabilized under limiting temperature that the crystal for thermodynamically thinking two-dimensional structure, which is,
, but seminar of University of Manchester using a kind of special mechanical stripping technology by the monolithic layer of two-dimensional structure from three-dimensional
Separated on graphite matrix out.
In carbon group material extended familys, the physicochemical properties of graphene are excellent, and are compared to the fullerene of costliness
And CNT, the raw material of graphene is easy to get, cheap, is material with broad prospects for development.So grasp prepares graphite
The method of alkene is most important.How the piece number of plies few, lamella size big and electronic structure intact graphite is prepared on a large scale
Alkene, is the premise of current graphene application, and scientists from all over the world make great efforts a direction of research.
In numerous purely mechanic stripping methods prepare the method for graphene, mechanical stripping is carried out to graphite to prepare stone in liquid phase
Black alkene is a kind of effective method.This method in the case of without using intercalator using micromechanics by being peeled off in the liquid phase
Method peeled off from graphite and obtain the graphene sheet layer of high quality.Athanasios et al. makees dispersant using PVP, go from
Graphite is peeled off to obtain a small amount of graphene using ultrasonic disperse in sub- water, concentration only has 0.1mg/ml, but these graphenes
Quality is very good, and lamellar spacing is not more than 1nm (Solid State Communications [J], 149 (2009) 2172-
2176].Olga et al. is by the use of SDBS as surfactant, and ultrasonic disperse obtains graphene sheet layer in deionized water
[J.Phys.Chem.C, 2010,114,21083-21087].Guardia et al. have studied various nonionic surface active agent
As dispersant, ultrasonic disperse obtains graphene in water, and by comparing to have obtained the relatively good non-ionic surface work of effect
Property agent is Tween 80, PVP, and PSS [CARBON, 49, (2011), 1653-1662].Chih-Jen et al. have studied it is various not
Ultrasound peels off graphite and obtains graphene in same polar solvent, and has carried out Primary Study to its mechanism.And obtain following several
The effect ranking of kind liquid：NMP ≈ DMSO ＞ DMF ＞ GBL ＞ H2O [J.AM.CHEM.SOC.2010,132,14638-
14648]。
Make the graphene quality height obtained in this way, fault of construction is few, but yield is too low, it is impossible to extensive system
It is standby, it is difficult to large-scale application.
The present invention relates to become more meticulous crushing and stripping is carried out to native graphite and synthetic graphite with force chemistry, nanometer is obtained
Graphite flake, even obtain few layer nano-graphene piece.This method is applied to prepare with scale nano graphite flakes and few layer nanometer stone
Not only quality is high for black alkene piece, resulting graphene and nano graphite flakes, and fault of construction is few.
The content of the invention
The present invention relates to become more meticulous crushing and stripping is carried out to native graphite and synthetic graphite with force chemistry, nanometer is obtained
Graphite flake, even obtain few layer nano-graphene piece.The nano graphite flakes of gained and few layer nano-graphene piece are that a kind of height is led
Electricity, the new type functional carbon material of high heat conduction, both can be compound with organic polymer or compound with inorganic material, in electronics, hair
The field such as light, battery, building materials, decoration, daily has been widely used.
The object of the present invention is achieved like this：
Native graphite or synthetic graphite are the graphite raw materials for preparing graphene and nano graphite flakes, and these graphite are former
Material be scattered in liquid medium, described liquid medium be water, isopropanol, dimethylformamide, 1-METHYLPYRROLIDONE, γ-
Hydroxybutyric acid lactone, vinyl pyrrolidone, dimethyl sulfoxide (DMSO) and their compound.Added in above-mentioned graphite dispersing solution anti-
Heavy agent is disperseed, with good mobility.Described anti-settling agent be carboxymethyl cellulose, nano-cellulose, carbon black,
CNT, polyvinyl alcohol and their compound.
Above-mentioned graphite dispersing solution is successively carried out by sand mill, homogenizer, large power supersonic dispersion machine and ball mill
Gradually grinding distribution, the mixed dispersion liquid of graphene and nano graphite flakes can be obtained.
Embodiment
Embodiment 1
100 grams of the commercially available native graphite of 1000 purposes, it is scattered in 1000 grams of deionized waters, adds carboxymethyl cellulose 2
Gram, under slow stirring, carboxymethyl cellulose is dissolved completely in graphite dispersing solution, circulated and disperseed two times with colloid mill, and
With ball mill ball milling 8 hours, the mixed dispersion liquid of graphene and nano graphite flakes is obtained.
The mixed dispersion liquid is separated in centrifuge, the separation factor of centrifuge takes upper strata clear up to more than 10,000
Liquid, dispersion of the single-layer graphene in dimethylformamide can be obtained；Remaining dispersion liquid, it is the dimethyl methyl of form the few-layer graphene alkene
Acid amides dispersion liquid.
Embodiment 2
100 grams of the commercially available native graphite of 1000 purposes, it is scattered in 1000 grams of deionized waters, adds the nanometer of low-crystallinity
100 grams of the water-based slurry of cellulose, the wherein solid content of cellulose are 5%, are circulated and disperseed two times with colloid mill, and use ball mill
Ball milling 8 hours, obtain the mixed dispersion liquid of the good graphene of dispersed and anti-settling property and nano graphite flakes.
Embodiment 3
100 grams of the commercially available native graphite of 400 purposes, it is scattered in 1000 grams of deionized waters, adds the nanometer of low-crystallinity
100 grams of the water-based slurry of cellulose, the wherein solid content of cellulose are 5%.1 gram of carboxymethyl cellulose is added, is slowly being stirred
Mix down, be completely dissolved carboxymethyl cellulose, circulated scattered two times with colloid mill, and with ball mill ball milling 8 hours, obtain dispersed
The mixed dispersion liquid of good graphene and nano graphite flakes with anti-settling property.
Embodiment 4
100 grams of the commercially available synthetic graphite of 400 purposes, it is scattered in 1000 grams of deionized waters, adds the nanometer of low-crystallinity
100 grams of the water-based slurry of cellulose, the wherein solid content of cellulose are 5%.10 grams of carbon black is added, is circulated with colloid mill scattered
, it can finally be obtained dispersed and anti-with large power supersonic dispersion machine ultrasonic disperse 4 hours again two time, and with ball mill ball milling 8 hours
The mixed dispersion liquid of the good graphene of heavy property and nano graphite flakes.
Embodiment 5
100 grams of the commercially available native graphite of 1000 purposes, it is scattered in 1000 grams of deionized waters, adds carboxymethyl cellulose 2
Gram, under slow stirring, carboxymethyl cellulose is dissolved completely in graphite dispersing solution, circulated and disperseed two times with colloid mill,
Handled 1 hour with homogenizer under circulation pattern, obtain the mixed dispersion liquid of graphene and nano graphite flakes.
Embodiment 6
100 grams of the commercially available native graphite of 1000 purposes, it is scattered in 1000 grams of deionized waters, adds the nanometer of low-crystallinity
100 grams of the water-based slurry of cellulose, the wherein solid content of cellulose are 5%, are circulated and disperseed two times with colloid mill, in circulation pattern
It is lower to be handled 1 hour with homogenizer, obtain the mixed dispersion liquid of the good graphene of dispersed and anti-settling property and nano graphite flakes.
Embodiment 7
100 grams of the commercially available native graphite of 400 purposes, it is scattered in 1000 grams of deionized waters, adds the nanometer of low-crystallinity
100 grams of the water-based slurry of cellulose, the wherein solid content of cellulose are 5%.1 gram of carboxymethyl cellulose is added, is slowly being stirred
Mix down, be completely dissolved carboxymethyl cellulose, circulated and disperseed two times with colloid mill, it is small with homogenizer processing 2 under circulation pattern
When, obtain the mixed dispersion liquids of the good graphene of dispersed and anti-settling property and nano graphite flakes.
Embodiment 8
100 grams of the commercially available synthetic graphite of 400 purposes, it is scattered in 1000 grams of deionized waters, adds the nanometer of low-crystallinity
100 grams of the water-based slurry of cellulose, the wherein solid content of cellulose are 5%.10 grams of carbon black is added, is circulated with colloid mill scattered
Two times, handled 2 hours with homogenizer under circulation pattern, obtain the good graphene of dispersed and anti-settling property and nano graphite flakes
Mixed dispersion liquid.
Embodiment 9
The mixed dispersion liquid for obtaining the good graphene of dispersed and anti-settling property and nano graphite flakes of the gained of embodiment 2
100 grams, it is placed in convection oven and drying 2 hours is carried out at 400 DEG C, obtains the mixed powder of graphene and nano graphite flakes, the powder
With good dispersiveness.
Embodiment 10
The mixed dispersion liquid for obtaining the good graphene of dispersed and anti-settling property and nano graphite flakes of the gained of embodiment 8
100 grams, it is placed in convection oven and drying 2 hours is carried out at 360 DEG C, obtains the mixed powder of graphene and nano graphite flakes, the powder
With good dispersiveness.
Claims (7)
1. a kind of graphene, nano graphite flakes and preparation method.
It is 2. as claimed in claim 1, it is characterised in that：It is described be used to prepare graphene and the graphite raw material of nano graphite flakes be
Native graphite or synthetic graphite.
It is 3. as claimed in claim 1, it is characterised in that：Described prepare graphene and the method for nano graphite flakes is a kind of power
Method.
It is 4. as claimed in claim 3, it is characterised in that：Described graphite raw material is first carried out with specific liquid medium and anti-settling agent
It is scattered, with good mobility.
It is 5. as claimed in claim 3, it is characterised in that：Described liquid medium is water, isopropanol, dimethylformamide, N- first
Base pyrrolidones, gamma-hydroxybutyric acid lactone, vinyl pyrrolidone, dimethyl sulfoxide (DMSO) and their compound.
It is 6. as claimed in claim 3, it is characterised in that：Described anti-settling agent be carboxymethyl cellulose, nano-cellulose, carbon black,
CNT, polyvinyl alcohol and their compound.
It is 7. as claimed in claim 1, it is characterised in that：Described graphite dispersing solution is successively by sand mill, homogenizer, high-power
Ultrasonic disperse machine and ball mill are ground scattered, can obtain the mixed dispersion liquid of graphene and nano graphite flakes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108622888A (en) * | 2018-03-08 | 2018-10-09 | 北京地泽科技有限公司 | A kind of method, apparatus of high-volume scale continuous production graphene and graphene prepared therefrom |
| CN110616470A (en) * | 2019-10-11 | 2019-12-27 | 上海烯望材料科技有限公司 | Method for modifying cellulose fiber by using few-layer two-dimensional material |
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| CN104966837A (en) * | 2015-04-24 | 2015-10-07 | 深圳市德方纳米科技股份有限公司 | Graphene conductive liquid as well as preparation method and application thereof |
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| CN106629580A (en) * | 2016-11-08 | 2017-05-10 | 华南理工大学 | Preparation method of graphite oxide/silicon dioxide/carbon nanotube multi-dimension composite nanomaterial |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103733271A (en) * | 2011-08-22 | 2014-04-16 | 拜耳知识产权有限责任公司 | Dispersion comprising carbon nanotubes and graphene platelets |
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| CN108622888A (en) * | 2018-03-08 | 2018-10-09 | 北京地泽科技有限公司 | A kind of method, apparatus of high-volume scale continuous production graphene and graphene prepared therefrom |
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