CN104495826A - Single-layer graphene dispersion liquid and preparation method thereof - Google Patents
Single-layer graphene dispersion liquid and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of nanomaterial processing, and particularly relates to a single-layer graphene dispersion liquid and a preparation method thereof. The dispersion liquid comprises the following raw materials in percentage by weight: 1wt%-10wt% of graphene and 0.01wt%-5wt% of a dispersing agent, wherein the concentration of the graphene dispersion liquid is 10-60mg mL<-1>; the diameter of graphene is 200nm-10mn; and the preparation method comprises the following steps: preparing secondary expansion graphite from graphite; mixing secondary expansion graphite with the dispersing agent to obtain a mixed dispersing system; and carrying out mechanical shearing and peeling on the mixed dispersing system, so as to obtain the single-layer graphene dispersion liquid. According to the single-layer graphene dispersion liquid, flakes of secondary expansion graphite can be subjected to mechanical separating, so as to obtain single-layer graphene; and by virtue of the dispersion action of the dispersing agent, the obtained graphene dispersion liquid is relatively good in dispersity, and exists in a single layer.
Description
Technical field
The present invention relates to nano material manufacture field, in particular to single-layer graphene dispersion liquid and preparation method thereof.
Background technology
2004, Univ Manchester UK physicist An Deliehaimu and Constantine Nuo Woxiaoluofu, successfully from graphite, isolate Graphene in an experiment, and confirm that it can Individual existence, because two people are in " the initiative experiment of two-dimensional graphene material ", common acquisition Nobel Prize in physics in 2010, has pulled open prelude prepared by Graphene.Graphene is another important carbon material after soccerballene and carbon nanotube.Graphene is the cellular hexaplanar two dimensional crystal formed by monolayer carbon atomic arrangement, and carbon atom is with sp
2form hydridization.The surface-area of Graphene is up to 2630m
2/ g is the twice of Single Walled Carbon Nanotube; Under normal temperature, electronic mobility is more than 200000cm
2/ Vs is higher than silicon single crystal; Thermal conductivity up to 5300W/mK, higher than diamond; Resistivity only has 10
-6Ω cm, similar with silver; Single-layer graphene is almost completely transparent, the light of every layer absorption 2.3%; Graphene is the thinnest in the world at present, and the strongest nano material, and its intensity can reach 1000GPa, is 200 times of steel.The characteristic of these excellences of Graphene makes it have huge potential application in gas sensor, opto-electronic device, chemical energy source (solar cell, lithium ion battery), catalyzer, the field such as antistatic.
In the application of reality, graphene sheet layer is easily assembled, affect the performance of Graphene performance, therefore usual by graphene dispersion in organic solvent or water phase surfactant mixture, solvent molecule or surfactant molecule are adsorbed on the surface of Graphene, rely on Intermolecular Forces or electrostatic repulsion forces, realize the Monolayer Dispersion of Graphene.Homogeneous, stable dispersion liquid is the essential condition of Graphene at various fields application and research, but the concentration of the graphene dispersing solution of report is all lower at present, limits the industrialized development of Graphene.
At present, the main method of graphene dispersing solution has: directly by Graphene or Graphene and surface-active mixed solution ultrasonic disperse under hyperacoustic water bath condition.Such as, Jonathan N.Coleman (Umar Khan, Arlene O ' Neill, Mustafa Lotya, Sukanta De, Jonathan N.Coleman.High-Concentration Solvent Exfoliation of Graphene, Small, 2010,6,864-871.) etc. investigator by the graphite dispersion of sheet in solvent nitrogen methyl-2-pyrrolidone (NMP), utilize ultrasonic echography 460h, obtain graphene dispersing solution, its concentration is 3.3mg mL
-1.The graphene dispersing solution concentration that this method obtains is low, and is that multi-layer graphene sheet, treatment time are long, seriously limits the actual demand of Graphene.Dan Li (Dan Li, Marc B.M ü ller, Scott Gilje, Richard B.Kaner, Gordon G.Wallace.Processable Aqueous Dispersions of Graphene Nanosheets, Nature Nanotechnology, 2008,3,101-105.) etc. investigator by graphene oxide water solution with a certain amount of hydrazine hydrate and ammonia soln 95 DEG C reduction 1h, obtaining concentration is 0.5mg mL
-1graphene dispersing solution, the graphene dispersing solution concentration that this method obtains is low, poor stability, can not meet industry various demands.On the whole, the preparation cost of existing graphene dispersing solution is higher, constrains the industrialization process of Graphene.In addition, due to the congregation of graphene sheet layer, in existing business-like graphene dispersing solution, graphene sheet layer is multilayer existence, is difficult to the graphene dispersing solution obtaining individual layer.
CN104151582 provides the preparation method of a kind of Graphene-polyimide conduction black film, first reexpansion is carried out to expanded graphite and obtain reexpansion graphite, by reexpansion graphite and the mixing of black fillers dispersed liquid, the dispersion liquid that ultrasonic stripping obtains Graphene and black filler is carried out to it, this dispersion liquid add the preparation such as diamine monomer can curtain coating material on a glass.Have employed reexpansion preparing graphite alkene in the method, but the graphene dispersing solution mobility adopting the mode of ultrasonic stripping to produce is better, and alternatively concentration is lower, and cannot proves that Graphene is that individual layer exists.
CN102942177 provides a kind of preparation method of graphene film, and expansible black lead is carried out thermal expansion and is processed into quasiflake graphite by (1), then is placed in solvent with basic solution immersion, suction filtration, washing and carries out ultrasonic disperse and obtain micro-nano graphene film; (2) the micro-nano graphene film prepared in step (1) is distributed in inorganic strong protonic acid soaks, after suction filtration, proceed to H
2o
2soak in solution, then suction filtration, washing, drying; (3) transferred in solvent by the micro-nano graphene film processed through step (2) and disperse, constant temperature leaves standstill, then carries out reexpansion after suction filtration or drying; (4) the micro-nano graphene film processed through step (3) is transferred in solvent carry out ultrasonic disperse, be transferred in the stove with reduction protection atmosphere after filtration drying, after carrying out High-Temperature Deoxygenation reduction, namely obtain graphene film.Can find out that graphene dispersion prepared by the method is poor by scanning electron microscopic picture, produce packing phenomenon.
Summary of the invention
The object of the present invention is to provide a kind of single-layer graphene dispersion liquid and preparation method thereof, to solve the problem that single-layer graphene is difficult to disperse.
One aspect of the invention provides a kind of preparation method of single-layer graphene dispersion liquid, comprising:
Step 1, is prepared into reexpansion graphite by graphite; Step 2, is mixed to get mixed dispersion in mass ratio by described reexpansion graphite, dispersion agent at 5: 1 ~ 1: 5; Step 3, carries out mechanical shearing stripping by described mixed dispersion; Step 4, obtains single-layer graphene dispersion liquid.
In certain embodiments, be preferably, in described step 2, described dispersion agent comprises: Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, polyvinylpyrrolidone, Sodium cholic acid, polystyrene, cetyl trimethylammonium bromide one or more.
In certain embodiments, be preferably, in described step 2, described mixed dispersion also comprises: water or solvent, described solvent comprises: cyclopentanone, pimelinketone, piperidines-1-formaldehyde, vinyl pyrrolidone, 1, 3-dimethyl-2-tetrahydroglyoxaline, bromobenzene, benzonitrile, phenmethyl M-nitro benzoic acid, N, N-dimethyl propylene thiazolinyl urea ketone, N-ethyl-2-pyrrolidone, N-Methyl pyrrolidone, acetic acid dimethylamide, cyclohexyl pyrrolidone, benzyl oxide, Virahol, NOP, dioxolane, ethyl acetate, 1-quinoline, benzaldehyde, thanomin, Unimoll DA, N-dodecylpyrrolidone, pyridine, dimethyl phthalate, ethanol, acetone, vinyl-acetic ester, ethylene glycol, toluene, heptane, pentane, hexane, methane amide, dimethyl formamide, dimethyl sulfoxide (DMSO), dichlorobenzene, chloroform, one or more of tetrahydrofuran (THF).
In certain embodiments, be preferably, in described step 3, the equipment that described mechanical shearing adopts comprises: one or more in ball mill, mulser, dispersion machine, shredder, homogenizer, fluid collider.
In certain embodiments, be preferably, the speed of described mechanical shearing is 2000 ~ 15000 revs/min, and/or the time of described mechanical shearing is 1 ~ 30 hour.
In certain embodiments, be preferably, in described step 1, the preparation method of described reexpansion graphite comprises: described graphite is carried out oxide treatment by step a.; Graphite after step a process is carried out expansion process by step b.; Graphite after step b process is carried out oxide treatment by step c again; Steps d. the graphite after step c process is carried out high temperature reduction expansion and obtain reexpansion graphite.
In certain embodiments, be preferably, in described step a, in oxide treatment, the wherein mass ratio 25: 1 ~ 45: 1 of graphite and oxygenant, the oxygenant of employing comprises: one or more in sulfuric acid, nitric acid, potassium permanganate, Potcrate, hydrogen peroxide, nitrous acid, hypochlorous acid.
In certain embodiments, be preferably, in described steps d, the temperature that described high temperature reduction expands is 600 ~ 1800 DEG C.
Another aspect of the present invention additionally provides a kind of single-layer graphene dispersion liquid prepared by aforesaid method, it is characterized in that, comprising: the Graphene of 1 ~ 10wt%, 0.01 ~ 5wt% dispersion agent; The concentration of described graphene dispersing solution is 10 ~ 60mg mL
-1, Graphene diameter be 200 nanometer ~ 10 micron; Described dispersion agent be Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, polyvinylpyrrolidone, Sodium cholic acid, polystyrene, cetyl trimethylammonium bromide one or more.
In certain embodiments, be preferably, single-layer graphene dispersion liquid also comprises: water or solvent, described solvent comprises: cyclopentanone, pimelinketone, piperidines-1-formaldehyde, vinyl pyrrolidone, 1, 3-dimethyl-2-tetrahydroglyoxaline, bromobenzene, benzonitrile, phenmethyl M-nitro benzoic acid, N, N-dimethyl propylene thiazolinyl urea ketone, N-ethyl-2-pyrrolidone, N-Methyl pyrrolidone, acetic acid dimethylamide, cyclohexyl pyrrolidone, benzyl oxide, Virahol, NOP, dioxolane, ethyl acetate, 1-quinoline, benzaldehyde, thanomin, Unimoll DA, N-dodecylpyrrolidone, pyridine, dimethyl phthalate, ethanol, acetone, vinyl-acetic ester, ethylene glycol, toluene, heptane, pentane, hexane, methane amide, dimethyl formamide, dimethyl sulfoxide (DMSO), dichlorobenzene, chloroform, one or more of tetrahydrofuran (THF).
Single-layer graphene dispersion liquid that the embodiment of the present invention provides and preparation method thereof, compared with prior art, is first prepared into reexpansion graphite by graphite, and destroy the Van der Waals force between graphitic molecules, reexpansion graphite presents lamella isolating construction; Adding dispersion agent agent on this basis increases dispersed; Mechanical shearing stripping is carried out to the mixed dispersion of reexpansion graphite and dispersion agent, the lamella of reexpansion graphite is separated and can obtains single-layer graphene, by the dissemination of dispersion agent, obtain better dispersed, the graphene dispersing solution existed with individual layer.
Accompanying drawing explanation
Fig. 1 is graphene dispersing solution optical photograph in the embodiment of the present invention 1;
Fig. 2 is graphene dispersing solution transmission electron microscope photo in the embodiment of the present invention 1;
Fig. 3 is Graphene Raman spectrum in the embodiment of the present invention 1;
Fig. 4 is that in the embodiment of the present invention 1, graphene dispersion uv-vis spectra proves good dispersity.
Embodiment
By reference to the accompanying drawings the present invention is described in further detail below by specific embodiment.
Consider that current single-layer graphene makes difficulty, and the problem of very easily assembling, the invention provides a kind of single-layer graphene dispersion liquid and preparation method thereof.
The preparation method of this kind of single-layer graphene dispersion liquid, comprising:
Step 1, is prepared into reexpansion graphite by graphite;
Step 2, is mixed to get mixed dispersion in mass ratio by reexpansion graphite, dispersion agent at 5: 1 ~ 1: 5;
Step 3, carries out mechanical shearing stripping by mixed dispersion;
Step 4, obtains single-layer graphene dispersion liquid.
By single-layer graphene dispersion liquid prepared by the preparation method of above-mentioned single-layer graphene dispersion liquid, comprising: the Graphene of 1 ~ 10wt%, 0.01 ~ 5wt% dispersion agent; The concentration of graphene dispersing solution is 10 ~ 60mg mL
-1; The diameter of Graphene is 200 nanometer ~ 10 micron; Dispersion agent be Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, polyvinylpyrrolidone, Sodium cholic acid, polystyrene, cetyl trimethylammonium bromide one or more.
In the present embodiment, first graphite is prepared into reexpansion graphite, destroy the Van der Waals force between graphitic molecules, reexpansion graphite presents lamella isolating construction; Adding dispersion agent on this basis increases dispersed; Mechanical shearing is carried out to the mixed dispersion of reexpansion graphite and dispersion agent, the lamella of reexpansion graphite is separated and can obtains single-layer graphene, by the dissemination of dispersion agent, obtain better dispersed, the graphene dispersing solution existed with individual layer.
The standby layer graphite of reexpansion graphite is separated by mechanical shearing, discovery is studied through contriver, mechanical means such as ball mill, mulser, dispersion machine, shredder, homogenizer, fluid collider is adopted to carry out peeling off the Graphene that can obtain few layer, spherical, bar-shaped grinding medium is increased in these mechanical means, shear area can be increased, improve peeling effect further, can single-layer graphene be obtained.And the use of grinding medium is beneficial to the dispersed of dispersion liquid, improve the dispersion effect of dispersion liquid.
Next, explanation is specifically done to the preparation of this single-layer graphene dispersion liquid:
Embodiment 1
Preparation reexpansion graphite: 5g graphite is put in the there-necked flask of 500mL, there-necked flask is dipped in mixture of ice and water, then add the concentrated nitric acid of 45mL and the vitriol oil of 87.5mL, the Potcrate of 55g is added in there-necked flask slowly and (at least adds more than 15 minutes.Attention: can produce dioxide peroxide when adding Potcrate, can produce blast during concentration height), this process stir process 72 hours, washes into neutrality with a large amount of water by the graphite of process, obtains powder after drying; Then to oxidation after graphite in tube furnace, Bulking Time 30 seconds-5 minutes temperature are carried out high temperature reduction and are obtained an expanded graphite in 1000-1300 DEG C of situation, and expanding at 600-1500 DEG C of high temperature reduction after adopting above-mentioned same method process expanded graphite obtains reexpansion graphite.
Prepare single-layer graphene dispersion liquid: reexpansion graphite, polyvinylpyrrolidone are mixed to get mixed dispersion in mass ratio 3: 2; Carry out mechanical shearing by ball mill to mixed dispersion, velocity of shear is 2000 revs/min, and the time of described mechanical shearing is 20 hours, obtains single-layer graphene dispersion liquid, wherein contains: the Graphene of 6wt%, 4wt% dispersion agent; The diameter of described Graphene is 200 nanometer ~ 8 micron;
It should be noted that, in the present embodiment, oxygenant can also replace with in potassium permanganate, hydrogen peroxide, hypochlorous acid, nitrous acid one or more.
Dispersion agent can also be selected from: Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, Sodium cholic acid, polystyrene, cetyl trimethylammonium bromide one or more.
The graphene dispersing solution this embodiment obtained carries out optical imagery, and as shown in Figure 1, this single-layer graphene dispersion liquid is the slurry of dark thick, is inverted by dispersion liquid, flows hardly, have good good dispersity, the feature of stability, high concentration.Take pictures under transmission electron microscope, as shown in Figure 2, dispersion liquid is all almost single-layer graphene film.The powder preparing dispersion liquid is carried out Raman sign, and by the shape at 2D peak, we judge to obtain single-layer graphene, as shown in Figure 3.After the graphene dispersing solution dilution this embodiment obtained, measure the absorption spectrum of the ultraviolet-visible of dilution different concns dispersion liquid, the linear good dispersity showing graphene dispersing solution of maximum absorption peak, as shown in Figure 4.Can see from these four figure, it relates to the high-content of graphene dispersing solution, good dispersiveness and individual layer characteristic.This graphene dispersing solution solves Graphene bad dispersibility, problem such as stability is low, concentration is lower in water and various organic solvent thereof.
Embodiment 2
Preparation reexpansion graphite: 5g graphite is put in the there-necked flask of 500mL, there-necked flask is dipped in mixture of ice and water, then add the concentrated nitric acid of 50mL and the hydrogen peroxide of 98mL, the Potcrate of 45g is added in there-necked flask slowly and (at least adds more than 15min.Attention: can produce dioxide peroxide when adding Potcrate, can produce blast during concentration height), this process stir process 72h, washes into neutrality with a large amount of water by the graphite of process, obtains powder after drying; Then to oxidation after graphite in tube furnace, Bulking Time 30S ~ 5min, temperature is carried out high temperature reduction and is obtained an expanded graphite in 1300 ~ 1500 DEG C of situations, and expanding at 800 ~ 1800 DEG C of high temperature reductions after adopting above-mentioned same method process expanded graphite obtains reexpansion graphite.
Prepare single-layer graphene dispersion liquid: by reexpansion graphite, polyvinylpyrrolidone mass ratio 1: 1, be mixed to get mixed dispersion; Carry out mechanical shearing by fluid collider to mixed dispersion, velocity of shear is 10500 revs/min, and the time of described mechanical shearing is 5 hours, obtains single-layer graphene dispersion liquid, its, the Graphene of 7wt%, 7wt% dispersion agent; The diameter of described Graphene is 500 nanometer ~ 10 micron;
It should be noted that, in the present embodiment, oxygenant can also in the present embodiment, oxygenant can also replace with in potassium permanganate, sulfuric acid, hypochlorous acid, nitrous acid one or more.
Dispersion agent can also be selected from: Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, Sodium cholic acid, polystyrene, cetyl trimethylammonium bromide ammonium one or more.
Embodiment 3
Preparation reexpansion graphite: 5g graphite is put in the there-necked flask of 500mL, there-necked flask is dipped in mixture of ice and water, then add the nitrous acid of 45mL and the hydrogen peroxide of 87.5mL, the hypochlorous acid of 55g is added in there-necked flask slowly and (at least adds more than 15min.), this process stir process 72h, washes into neutrality with a large amount of water by the graphite of process, obtains powder after drying; Then to oxidation after graphite in tube furnace, Bulking Time 30S ~ 5min, temperature is carried out high temperature reduction and is obtained an expanded graphite in 1300 ~ 1500 DEG C of situations, and expanding at 1300 ~ 1500 DEG C of high temperature reductions after adopting above-mentioned same method process expanded graphite obtains reexpansion graphite.
Prepare single-layer graphene dispersion liquid: be 3: 1 in mass ratio by reexpansion graphite, Sodium cholic acid, be mixed to get mixed dispersion; Solvent NOP is added in mixed dispersion, in clarifixator (the spherical grinding medium of interior loading), mechanical shearing is carried out to mixing the solution finally obtained by fluid mulser, velocity of shear is 8000 revs/min, the time of mechanical shearing is 30 hours, obtain single-layer graphene dispersion liquid, wherein, Graphene, the 1.7wt% dispersion agent of 5wt%; The diameter of described Graphene is 200 nanometer ~ 8 micron;
It should be noted that, in the present embodiment, oxygenant can also one or more in the vitriol oil, concentrated nitric acid, potassium permanganate, Potcrate.
Dispersion agent can also be selected from: Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, polyvinylpyrrolidone, polystyrene, cetyl trimethylammonium bromide one or more, or Sodium cholic acid and other alternative dispersion agents share.
Solvent can also be substituted by following material: cyclopentanone, pimelinketone, piperidines-1-formaldehyde, vinyl pyrrolidone, 1, 3-dimethyl-2-tetrahydroglyoxaline, bromobenzene, benzonitrile, phenmethyl M-nitro benzoic acid, N, N-dimethyl propylene thiazolinyl urea ketone, N-ethyl-2-pyrrolidone, N-Methyl pyrrolidone, acetic acid dimethylamide, cyclohexyl pyrrolidone, benzyl oxide, Virahol, dioxolane, ethyl acetate, 1-quinoline, benzaldehyde, thanomin, Unimoll DA, N-dodecylpyrrolidone, pyridine, dimethyl phthalate, ethanol, acetone, vinyl-acetic ester, ethylene glycol, toluene, heptane, pentane, hexane, methane amide, dimethyl formamide, dimethyl sulfoxide (DMSO), dichlorobenzene, chloroform, one or more of tetrahydrofuran (THF).
Embodiment 4:
Preparation reexpansion graphite: 5g graphite is put in the there-necked flask of 500mL, there-necked flask is dipped in mixture of ice and water, then add the potassium permanganate of 45mL and the nitrous acid of 87.5mL, the Potcrate of 55g is added in there-necked flask slowly and (at least adds more than 15min.Attention: can produce dioxide peroxide when adding Potcrate, can produce blast during concentration height), this process stir process 72h, washes into neutrality with a large amount of water by the graphite of process, obtains powder after drying; Then to oxidation after graphite in tube furnace, Bulking Time 30S ~ 5min, temperature is carried out high temperature reduction and is obtained an expanded graphite in 1300 ~ 1500 DEG C of situations, and after adopting above-mentioned same method process expanded graphite, high temperature reduction expands and obtains reexpansion graphite.
Prepare single-layer graphene dispersion liquid: reexpansion graphite, cetyl trimethylammonium bromide are mixed to get mixed dispersion in mass ratio at 5: 1; Add again solvent Unimoll DA; By dispersion machine (including bar-shaped grinding medium), mechanical shearing is carried out to mixed dispersion, velocity of shear is 13500 revs/min, and the time of described mechanical shearing is 4 hours, obtains single-layer graphene dispersion liquid, wherein, Graphene, the 0.2wt% dispersion agent of 1wt%; The diameter of described Graphene is 800 nanometer ~ 5 micron;
It should be noted that, in the present embodiment, oxygenant can also one or more in concentrated nitric acid, the vitriol oil, hypochlorous acid, hydrogen peroxide.
Dispersion agent can also be selected from: Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, polyvinylpyrrolidone, Sodium cholic acid, polystyrene one or more, or cetyl trimethylammonium bromide and other alternative dispersion agents share.
Solvent can also be substituted by following material: cyclopentanone, pimelinketone, piperidines-1-formaldehyde, vinyl pyrrolidone, 1, 3-dimethyl-2-tetrahydroglyoxaline, bromobenzene, benzonitrile, phenmethyl M-nitro benzoic acid, N, N-dimethyl propylene thiazolinyl urea ketone, N-ethyl-2-pyrrolidone, N-Methyl pyrrolidone, acetic acid dimethylamide, cyclohexyl pyrrolidone, benzyl oxide, Virahol, NOP, dioxolane, ethyl acetate, 1-quinoline, benzaldehyde, thanomin, N-dodecylpyrrolidone, pyridine, dimethyl phthalate, ethanol, acetone, vinyl-acetic ester, ethylene glycol, toluene, heptane, pentane, hexane, methane amide, dimethyl formamide, dimethyl sulfoxide (DMSO), dichlorobenzene, chloroform, one or more of tetrahydrofuran (THF), or Unimoll DA shares with other alternative solvents.
The graphene dispersing solution concentration that the method obtains is high, stability is strong and be single-layer graphene film.In addition, preparation technology is simple, cost is low, and is conducive to the advantages such as industrialization production.The graphene dispersing solution of this acquisition has potential actual application value in fields such as optical, electrical materials.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a preparation method for single-layer graphene dispersion liquid, is characterized in that, comprising:
Step 1, is prepared into reexpansion graphite by graphite;
Step 2, is mixed to get mixed dispersion in mass ratio by described reexpansion graphite, dispersion agent at 5: 1 ~ 1: 5;
Step 3, carries out mechanical shearing stripping by described mixed dispersion;
Step 4, obtains single-layer graphene dispersion liquid.
2. the preparation method of single-layer graphene dispersion liquid as claimed in claim 1, it is characterized in that, in described step 2, described dispersion agent comprises: Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, polyvinylpyrrolidone, Sodium cholic acid, polystyrene, cetyl trimethylammonium bromide one or more.
3. the preparation method of single-layer graphene dispersion liquid as claimed in claim 1, it is characterized in that, in described step 2, described mixed dispersion also comprises: water or solvent;
Described solvent comprises: cyclopentanone, pimelinketone, piperidines-1-formaldehyde, vinyl pyrrolidone, 1, 3-dimethyl-2-tetrahydroglyoxaline, bromobenzene, benzonitrile, phenmethyl M-nitro benzoic acid, N, N-dimethyl propylene thiazolinyl urea ketone, N-ethyl-2-pyrrolidone, N-Methyl pyrrolidone, acetic acid dimethylamide, cyclohexyl pyrrolidone, benzyl oxide, Virahol, NOP, dioxolane, ethyl acetate, 1-quinoline, benzaldehyde, thanomin, Unimoll DA, N-dodecylpyrrolidone, pyridine, dimethyl phthalate, ethanol, acetone, vinyl-acetic ester, ethylene glycol, toluene, heptane, pentane, hexane, methane amide, dimethyl formamide, dimethyl sulfoxide (DMSO), dichlorobenzene, chloroform, one or more of tetrahydrofuran (THF).
4. the preparation method of single-layer graphene dispersion liquid as claimed in claim 1, it is characterized in that, in described step 3, the equipment that described mechanical shearing adopts comprises: one or more in ball mill, mulser, dispersion machine, shredder, homogenizer, fluid collider.
5. the preparation method of single-layer graphene dispersion liquid as claimed in claim 4, it is characterized in that, the speed of described mechanical shearing is 2000 ~ 15000 revs/min, and/or the time of described mechanical shearing is 1 ~ 30 hour.
6. the preparation method of the single-layer graphene dispersion liquid as described in any one of claim 1-5, is characterized in that, in described step 1, the preparation method of described reexpansion graphite comprises:
Described graphite is carried out oxide treatment by step a.;
Graphite after step a process is carried out expansion process by step b.;
Graphite after step b process is carried out oxide treatment by step c again;
Steps d. the graphite after step c process is carried out high temperature reduction expansion and obtain reexpansion graphite.
7. the preparation method of single-layer graphene dispersion liquid as claimed in claim 6, it is characterized in that, in described step a, in oxide treatment, the wherein mass ratio 25: 1 ~ 45: 1 of graphite and oxygenant, the oxygenant of employing comprises: one or more in sulfuric acid, nitric acid, potassium permanganate, Potcrate, hydrogen peroxide, hypochlorous acid, nitrous acid.
8. the preparation method of single-layer graphene dispersion liquid as claimed in claim 6, is characterized in that, in described steps d, the temperature that described high temperature reduction expands is 600 ~ 1800 DEG C.
9. by a single-layer graphene dispersion liquid prepared by the preparation method of single-layer graphene dispersion liquid described in any one of claim 1-8, it is characterized in that, comprising: the Graphene of 1 ~ 10wt%, 0.01 ~ 5wt% dispersion agent; The concentration of described graphene dispersing solution is 10 ~ 60mg mL
-1, Graphene diameter be 200 nanometer ~ 10 micron; Described dispersion agent be Sodium dodecylbenzene sulfonate, sodium laurylsulfonate, polyvinylpyrrolidone, Sodium cholic acid, polystyrene, cetyl trimethylammonium bromide one or more.
10. single-layer graphene dispersion liquid as claimed in claim 9, it is characterized in that, also comprise: water or solvent, described solvent comprises: cyclopentanone, pimelinketone, piperidines-1-formaldehyde, vinyl pyrrolidone, 1, 3-dimethyl-2-tetrahydroglyoxaline, bromobenzene, benzonitrile, phenmethyl M-nitro benzoic acid, N, N-dimethyl propylene thiazolinyl urea ketone, N-ethyl-2-pyrrolidone, N-Methyl pyrrolidone, acetic acid dimethylamide, cyclohexyl pyrrolidone, benzyl oxide, Virahol, NOP, dioxolane, ethyl acetate, 1-quinoline, benzaldehyde, thanomin, Unimoll DA, N-dodecylpyrrolidone, pyridine, dimethyl phthalate, ethanol, acetone, vinyl-acetic ester, ethylene glycol, toluene, heptane, pentane, hexane, methane amide, dimethyl formamide, dimethyl sulfoxide (DMSO), dichlorobenzene, chloroform, one or more of tetrahydrofuran (THF).
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