CN104495826B - 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's Nuo Woxiao love,
Successfully from graphite, isolate Graphene in experiment, and confirm that it can be with individualism, because two people are in " two-dimensional graphene material
The initiative experiment of material ", jointly obtains Nobel Prize in physics in 2010, has pulled open the prelude of Graphene preparation.Graphene is
Another important material with carbon element after fullerene and CNT.Graphene is the cellular hexagonal being formed by monolayer carbon atom arrangement
Planar crystal, carbon atom is with sp2Form hydridization.The surface area of Graphene is up to 2630m2/ g, is SWNT
Twice；Under room temperature, electron mobility is more than 200000cm2/ v s is higher than monocrystal silicon；Heat conductivity is up to 5300w/m k,
Higher than diamond；Resistivity only has 10-6ω cm, similar with silver；Single-layer graphene is almost fully transparent, and every layer only absorbs
2.3% light；Graphene is the thinnest in the world at present, and nano material the strongest, its intensity, up to 1000gpa, is steel
200 times.These excellent characteristics of Graphene make its gas sensor, opto-electronic device, chemical energy source (solaode,
Lithium ion battery), catalyst, the field such as antistatic there is huge potential application.
In actual application, graphene sheet layer is susceptible to assemble, and the performance of impact Graphene performance therefore generally will
In organic solvent or aqueous surfactant solution, solvent molecule or surfactant molecule adsorb in Graphene graphene dispersion
Surface on, rely on intermolecular force or electrostatic repulsion forces, realize the Monolayer Dispersion of Graphene.Homogeneous, stable dispersion liquid
It is the essential condition in various fields application and research for the Graphene, but the concentration of the graphene dispersing solution of current report is all relatively low,
Limit the industrialized development of Graphene.
At present, the main method of graphene dispersing solution has: directly by the mixed liquor of Graphene or Graphene and surface activity
Ultrasonic disperse under the water bath condition of ultrasound wave.For example, 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. researcher by the graphite dispersion of lamellar to solvent
In N-methyl ketopyrrolidine (nmp), using 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 long for multi-layer graphene piece, process time, seriously limits Graphene
Actual demand.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. researcher is by graphene oxide water solution a certain amount of hydrazine hydrate and ammonia
95 DEG C of reduction 1h of aqueous solution, obtaining concentration is 0.5mg ml-1Graphene dispersing solution, the graphene dispersing solution that this method obtains
Concentration is low, stability is poor it is impossible to meet the various demands of industry.On the whole, the preparation cost of existing graphene dispersing solution is relatively
Height, constrains the industrialization process of Graphene.Further, since the aggregation of graphene sheet layer, existing business-like Graphene
In dispersion liquid, graphene sheet layer is multilamellar and exists it is difficult to obtain the graphene dispersing solution of monolayer.
Cn104151582 provides a kind of preparation method of Graphene-polyimides conduction black film, first expanded graphite is entered
Row reexpansion obtains reexpansion graphite, and reexpansion graphite and the mixing of black filler dispersion liquid carry out ultrasonic stripping to it
From the dispersion liquid obtaining Graphene and black filler, this dispersion liquid can be cast on a glass in preparations such as addition diamine monomers
Material.Employ reexpansion preparing graphite alkene in the method, but, the stone being produced by the way of ultrasonic stripping
Black alkene dispersion liquid mobility is preferably it may also be said to concentration is relatively low, and cannot prove that Graphene is that monolayer exists.
Cn102942177 provides a kind of preparation method of graphene film, and expansible graphite is carried out thermal expansion and is processed into by (1)
Quasiflake graphite, then carried out ultrasonic disperse and obtained micro-nano Graphene with being placed in solvent after alkaline solution immersion, sucking filtration, washing
Piece；(2) the micro-nano graphene film preparing in step (1) is distributed in inorganic strong protonic acid and soaks, proceed to after sucking filtration
h2o2Soak in solution, then sucking filtration, washing, drying；(3) molten by transferring to through the micro-nano graphene film that step (2) was processed
Disperse in agent, constant temperature stands, then carries out reexpansion after sucking filtration or drying；(4) the micro-nano stone that will process through step (3)
Black alkene piece is transferred to and is carried out ultrasonic disperse in solvent, is transferred in the stove with reduction protection atmosphere, carries out after filtration drying
Graphene film is obtained final product after High-Temperature Deoxygenation reduction.By scanning electron microscopic picture it can be seen that the method preparation graphene dispersion relatively
Difference, produces packing phenomenon.
Content of the invention
It is an object of the invention to provide a kind of single-layer graphene dispersion liquid and preparation method thereof, to solve single-layer graphene
It is difficult to scattered problem.
One aspect of the invention provides a kind of preparation method of single-layer graphene dispersion liquid, comprising:
Step 1, graphite is prepared into reexpansion graphite；Step 2, described reexpansion graphite, dispersant are pressed quality
It is mixed to get mixed dispersion than 5: 1～1: 5；Step 3, described mixed dispersion is carried out mechanical shearing stripping；Step
4, obtain single-layer graphene dispersion liquid.
In certain embodiments, preferably, in described step 2, described dispersant includes: dodecylbenzene sodium sulfonate, ten
Dialkyl sulfonates, Polyvinylpyrrolidone, sodium cholate, polystyrene, one or more of cetyl trimethylammonium bromide.
In certain embodiments, preferably, in described step 2, described mixed dispersion also includes: water or solvent；Institute
State solvent to include: Ketocyclopentane, Ketohexamethylene, piperidines -1- formaldehyde, vinyl pyrrolidone, 1,3- dimethyl -2- imidazoline, bromobenzene,
Benzonitrile, benzyl benzoic acid, n, n- dimethyl propylene thiazolinyl urea ketone, n- ethyl-2-pyrrolidone, n- methyl pyrrolidone, two
First and second amide, cyclohexyl pyrrolidone, benzyl oxide, isopropanol, n- octylpyrrolidone, dioxolanes, ethyl acetate, 1- quinoline,
Benzaldehyde, ethanolamine, ethyl phthalate, n- dodecyl pyrrolidone, pyridine, dimethyl phthalate, ethanol, acetone, acetic acid
Vinyl acetate, ethylene glycol, toluene, heptane, pentane, hexane, Methanamide, dimethylformamide, dimethyl sulfoxide, dichlorobenzene, chlorine
Imitative, one or more of oxolane.
In certain embodiments, preferably, in described step 3, the equipment that described mechanical shearing adopts includes: ball mill,
One or more of mulser, dispersion machine, grinder, homogenizer, fluid collider.
In certain embodiments, preferably, the speed of described mechanical shearing is 2000～15000 revs/min, and/or, institute
The time stating mechanical shearing is 1～30 hour.
In certain embodiments, preferably, in described step 1, the preparation method of described reexpansion graphite includes: step
A. described graphite is carried out oxidation processes；Graphite after the process of step a is carried out expansion process by step b.；Step c. is by step b
Graphite after process carries out oxidation processes again；Step d. by step c process after graphite carry out high temperature reduction expand obtain secondary
Expanded graphite.
In certain embodiments, preferably, in described step a, in oxidation processes, the quality of wherein graphite and oxidant
Than 25: 1～45: 1, the oxidant of employing includes: sulphuric acid, nitric acid, potassium permanganate, potassium chlorate, hydrogen peroxide, nitrous acid, hypochlorous acid
One or more of.
In certain embodiments, preferably, in described step d, the temperature that described high temperature reduction expands is 600～1800
℃.
Another aspect of the invention additionally provides a kind of single-layer graphene dispersion liquid prepared by said method, its feature
It is, comprising: the Graphene of 1～10wt%, 0.01～5wt% dispersant；The concentration of described graphene dispersing solution be 10～
60mg ml-1, a diameter of 200 nanometers～10 microns of Graphene；Described dispersant is dodecylbenzene sodium sulfonate, dodecyl
Sodium sulfonate, Polyvinylpyrrolidone, sodium cholate, polystyrene, one or more of cetyl trimethylammonium bromide.
In certain embodiments, preferably, single-layer graphene dispersion liquid also includes: water or solvent, and described solvent includes: ring
Pentanone, Ketohexamethylene, piperidines -1- formaldehyde, vinyl pyrrolidone, 1,3- dimethyl -2- imidazoline, bromobenzene, benzonitrile, benzyl peace
The fragrant acid of breath, n, n- dimethyl propylene thiazolinyl urea ketone, n- ethyl-2-pyrrolidone, n- methyl pyrrolidone, acetic acid dimethylamide, hexamethylene
Base ketopyrrolidine, benzyl oxide, isopropanol, n- octylpyrrolidone, dioxolanes, ethyl acetate, 1- quinoline, benzaldehyde, ethanol
Amine, ethyl phthalate, n- dodecyl pyrrolidone, pyridine, dimethyl phthalate, ethanol, acetone, vinyl acetate, ethylene glycol,
Toluene, heptane, pentane, hexane, Methanamide, dimethylformamide, dimethyl sulfoxide, dichlorobenzene, chloroform, the one of oxolane
Plant or multiple.
Single-layer graphene dispersion liquid provided in an embodiment of the present invention and preparation method thereof, compared with prior art, first will
Graphite is prepared into reexpansion graphite, destroys the Van der Waals force between graphitic molecules, and reexpansion graphite assumes lamella isolating construction；
Dispersant agent is added to increase dispersibility on this basis；Machinery is carried out to the mixed dispersion of reexpansion graphite and dispersant
Shearing is peeled off, and the lamella of reexpansion graphite is separated and can get single-layer graphene, by the peptizaiton of dispersant, obtain
Dispersibility is preferable, the graphene dispersing solution being existed with monolayer.
Brief description
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 dispersion.
Specific embodiment
Combine accompanying drawing below by specific embodiment the present invention is described in further detail.
Consider that single-layer graphene makes difficulty up till now, and the problem of easily gathering, the invention provides a kind of monolayer stone
Black alkene dispersion liquid and preparation method thereof.
A kind of this preparation method of single-layer graphene dispersion liquid, comprising:
Step 1, graphite is prepared into reexpansion graphite；
Step 2, reexpansion graphite, dispersant in mass ratio 5: 1～1: 5 is mixed to get mixed dispersion；
Step 3, mixed dispersion is carried out mechanical shearing stripping；
Step 4, obtains single-layer graphene dispersion liquid.
Single-layer graphene dispersion liquid by the preparation method preparation of above-mentioned single-layer graphene dispersion liquid, comprising: 1～
The Graphene of 10wt%, 0.01～5wt% dispersant；The concentration of graphene dispersing solution is 10～60mg ml-1；Graphene straight
Footpath is 200 nanometers～10 microns；Dispersant is dodecylbenzene sodium sulfonate, dodecyl sodium sulfate, Polyvinylpyrrolidone, gallbladder
Sour sodium, polystyrene, one or more of cetyl trimethylammonium bromide.
In the present embodiment, first graphite is prepared into reexpansion graphite, destroys the Van der Waals force between graphitic molecules, two
Secondary expanded graphite assumes lamella isolating construction；Dispersant is added to increase dispersibility on this basis；To reexpansion graphite and point
The mixed dispersion of powder carries out mechanical shearing, the lamella of reexpansion graphite is separated and can get single-layer graphene, borrow
The peptizaiton of dispersion aids, obtains dispersibility preferably, the graphene dispersing solution being existed with monolayer.
The standby layer graphite of reexpansion graphite is separated by mechanical shearing, studies through inventor and finds, using plant equipment such as
Ball mill, mulser, dispersion machine, grinder, homogenizer, fluid collider carry out peeling off the Graphene that can obtain few layer,
Increase spherical, bar-shaped abrasive media in these plant equipment, it is possible to increase the section of shear, improve peeling effect further, can get
Single-layer graphene.And the use of abrasive media is dispersed beneficial to dispersion liquid, improve the dispersion effect of dispersion liquid.
Next, the preparation of this single-layer graphene dispersion liquid is done with more detailed description:
Embodiment 1
Preparation reexpansion graphite: 5g graphite is put in the there-necked flask of 500ml, there-necked flask is dipped into mixture of ice and water
In, it is subsequently adding the concentrated nitric acid of 45ml and the concentrated sulphuric acid of 87.5ml, the potassium chlorate of 55g is slowly added in there-necked flask (extremely
Less plus more than 15 minutes.Note: chlorine dioxide can be produced when adding potassium chlorate, blast when concentration is high, can be produced), this process is stirred
Mix process 72 hours, with substantial amounts of water, the graphite of process is washed into neutrality, after being dried, obtain powder；Then to the graphite after oxidation
In tube furnace, 30 seconds -5 minutes temperature of Bulking Time carry out high temperature reduction in the case of 1000-1300 DEG C and are once expanded
Graphite, is processed using above-mentioned same method and obtains reexpansion in 600-1500 DEG C of high temperature reduction expansion after an expanded graphite
Graphite.
Prepare single-layer graphene dispersion liquid: reexpansion graphite, Polyvinylpyrrolidone are mixed to get hybrid dispersions
System in mass ratio 3: 2；Mechanical shearing is carried out to mixed dispersion by ball mill, shear rate is 2000 revs/min, described
The time of mechanical shearing is 20 hours, obtains single-layer graphene dispersion liquid, wherein contains: the Graphene of 6wt%, 4wt% dispersion
Agent；A diameter of 200 nanometers～8 microns of described Graphene；
It should be noted that in the present embodiment, oxidant may be replaced by potassium permanganate, hydrogen peroxide, hypochlorous acid, Asia
One or more of nitric acid.
Dispersant is also selected from: dodecylbenzene sodium sulfonate, dodecyl sodium sulfate, sodium cholate, polystyrene, 16
One or more of alkyl trimethyl ammonium bromide.
The graphene dispersing solution that this embodiment is obtained carries out optical imagery, as shown in figure 1, this single-layer graphene dispersion liquid
For the slurry of dark thick, dispersion liquid is inverted, hardly flows, there is good good dispersion, stability, high dense
The feature of degree.Take pictures under transmission electron microscope, as shown in Fig. 2 dispersion liquid almost all is single-layer graphene film.Dispersion liquid will be prepared
Powder carry out Raman sign, by the shape at 2d peak, we judge obtained single-layer graphene, as shown in Figure 3.This is implemented
After the graphene dispersing solution dilution that example obtains, the absorption spectrum of the ultraviolet-visible of measurement dilution variable concentrations dispersion liquid, maximum
The linear good dispersion showing graphene dispersing solution of absworption peak, as shown in Figure 4.Can see from this four figures, it
It is related to high-load, good dispersibility and the monolayer characteristic of graphene dispersing solution.This graphene dispersing solution solves Graphene and exists
Bad dispersibility in water and its various organic solvent, the problems such as stability is low, concentration is relatively low.
Embodiment 2
Preparation reexpansion graphite: 5g graphite is put in the there-necked flask of 500ml, there-necked flask is dipped into mixture of ice and water
In, it is subsequently adding the concentrated nitric acid of 50ml and the hydrogen peroxide of 98ml, the potassium chlorate of 45g is slowly added in there-necked flask (at least
Plus more than 15min.Note: chlorine dioxide can be produced when adding potassium chlorate, blast when concentration is high, can be produced), this process stirs
Process 72h, with substantial amounts of water, the graphite of process is washed into neutrality, after being dried, obtain powder；Then to the graphite after oxidation in pipe
In formula stove, Bulking Time 30s～5min, temperature carries out high temperature reduction in the case of 1300～1500 DEG C and is once expanded stone
Ink, is processed using above-mentioned same method and obtains reexpansion in 800～1800 DEG C of high temperature reductions expansions after an expanded graphite
Graphite.
Prepare single-layer graphene dispersion liquid: reexpansion graphite, Polyvinylpyrrolidone mass ratio 1: 1 are mixed to get
Mixed dispersion；Mechanical shearing is carried out to mixed dispersion by fluid collider, shear rate is 10500 revs/min,
The time of described mechanical shearing is 5 hours, obtains single-layer graphene dispersion liquid, its, the Graphene of 7wt%, 7wt% dispersant；
A diameter of 500 nanometers～10 microns of described Graphene；
It should be noted that in the present embodiment, oxidant can also be in the present embodiment, and oxidant can also be replaced
For one or more of potassium permanganate, sulphuric acid, hypochlorous acid, nitrous acid.
Dispersant is also selected from: dodecylbenzene sodium sulfonate, dodecyl sodium sulfate, sodium cholate, polystyrene, 16
One or more of alkyl trimethyl ammonium bromide ammonium.
Embodiment 3
Preparation reexpansion graphite: 5g graphite is put in the there-necked flask of 500ml, there-necked flask is dipped into mixture of ice and water
In, it is subsequently adding the nitrous acid of 45ml and the hydrogen peroxide of 87.5ml, the hypochlorous acid of 55g is slowly added in there-necked flask (extremely
Less plus more than 15min.), this process stir process 72h, with substantial amounts of water, the graphite of process is washed into neutrality, obtain after being dried
Powder；Then to the graphite after oxidation in tube furnace, Bulking Time 30s～5min, temperature is in the case of 1300～1500 DEG C
Carry out high temperature reduction and obtain an expanded graphite, processed after an expanded graphite 1300～1500 using above-mentioned same method
DEG C high temperature reduction expands and obtains reexpansion graphite.
Prepare single-layer graphene dispersion liquid: reexpansion graphite, sodium cholate be 3: 1 in mass ratio, be mixed to get mixing
Dispersion；Add solvent n- octylpyrrolidone in mixed dispersion, by fluid mulser, mixing is finally obtained
Solution carry out mechanical shearing in homogenizer (interior loading spherical abrasive media), shear rate is 8000 revs/min, mechanical shear
The time cut is 30 hours, obtains single-layer graphene dispersion liquid, wherein, the Graphene of 5wt%, 1.7wt% dispersant；Described stone
A diameter of 200 nanometers～8 microns of black alkene；
It should be noted that in the present embodiment, oxidant can also be in concentrated sulphuric acid, concentrated nitric acid, potassium permanganate, potassium chlorate
One or more of.
Dispersant is also selected from: dodecylbenzene sodium sulfonate, dodecyl sodium sulfate, Polyvinylpyrrolidone, polyphenyl
One or more of ethylene, cetyl trimethylammonium bromide, or sodium cholate is shared with other dispersants alternative.
Solvent can also be substituted by following material: Ketocyclopentane, Ketohexamethylene, piperidines -1- formaldehyde, vinyl pyrrolidone, 1,
3- dimethyl -2- imidazoline, bromobenzene, benzonitrile, benzyl benzoic acid, n, n- dimethyl propylene thiazolinyl urea ketone, n- ethyl -2- pyrroles
Alkanone, n- methyl pyrrolidone, acetic acid dimethylamide, cyclohexyl pyrrolidone, benzyl oxide, isopropanol, dioxolanes, ethyl acetate,
1- quinoline, benzaldehyde, ethanolamine, ethyl phthalate, n- dodecyl pyrrolidone, pyridine, dimethyl phthalate, ethanol, third
Ketone, vinyl acetate, ethylene glycol, toluene, heptane, pentane, hexane, Methanamide, dimethylformamide, dimethyl sulfoxide, dichloro
For benzene, chloroform, one or more of oxolane.
Embodiment 4:
Preparation reexpansion graphite: 5g graphite is put in the there-necked flask of 500ml, there-necked flask is dipped into mixture of ice and water
In, it is subsequently adding the potassium permanganate of 45ml and the nitrous acid of 87.5ml, the potassium chlorate of 55g is slowly added in there-necked flask
(at least plus more than 15min.Note: chlorine dioxide can be produced when adding potassium chlorate, blast when concentration is high, can be produced), this process
The graphite of process is washed into neutrality with substantial amounts of water by stir process 72h, obtains powder after being dried；Then to the graphite after oxidation
In tube furnace, Bulking Time 30s～5min, temperature carries out high temperature reduction in the case of 1300～1500 DEG C and is once expanded
Graphite, processes high temperature reduction expansion after an expanded graphite using above-mentioned same method and obtains reexpansion graphite.
Prepare single-layer graphene dispersion liquid: reexpansion graphite, cetyl trimethylammonium bromide in mass ratio 5: 1 are mixed
Conjunction obtains mixed dispersion；Add solvent ethyl phthalate again；By dispersion machine (including bar-shaped abrasive media) to mixing point
Prose style free from parallelism system carries out mechanical shearing, and shear rate is 13500 revs/min, and the time of described mechanical shearing is 4 hours, obtains monolayer
Graphene dispersing solution, wherein, the Graphene of 1wt%, 0.2wt% dispersant；A diameter of 800 nanometers～the 5 of described Graphene are micro-
Rice；
It should be noted that in the present embodiment, oxidant can also be in concentrated nitric acid, concentrated sulphuric acid, hypochlorous acid, hydrogen peroxide
One or more.
Dispersant is also selected from: dodecylbenzene sodium sulfonate, dodecyl sodium sulfate, Polyvinylpyrrolidone, cholic acid
One or more of sodium, polystyrene, or cetyl trimethylammonium bromide is shared with other dispersants alternative.
Solvent can also be substituted by following material: Ketocyclopentane, Ketohexamethylene, piperidines -1- formaldehyde, vinyl pyrrolidone, 1,
3- dimethyl -2- imidazoline, bromobenzene, benzonitrile, benzyl benzoic acid, n, n- dimethyl propylene thiazolinyl urea ketone, n- ethyl -2- pyrroles
Alkanone, n- methyl pyrrolidone, acetic acid dimethylamide, cyclohexyl pyrrolidone, benzyl oxide, isopropanol, n- octylpyrrolidone, dioxy
Penta ring, ethyl acetate, 1- quinoline, benzaldehyde, ethanolamine, n- dodecyl pyrrolidone, pyridine, dimethyl phthalate, ethanol,
Acetone, vinyl acetate, ethylene glycol, toluene, heptane, pentane, hexane, Methanamide, dimethylformamide, dimethyl sulfoxide, two
Chlorobenzene, chloroform, one or more of oxolane；Or ethyl phthalate and other alternative solvents share.
The graphene dispersing solution concentration that the method obtains is high, stability by force and is single-layer graphene film.Additionally, preparation work
Skill is simple, low cost, and the advantages of be conducive to industrialization production.The graphene dispersing solution of this acquisition is led in light, electric material etc.
Domain has potential actual application value.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, made any repair
Change, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of preparation method of single-layer graphene dispersion liquid is it is characterised in that include:
Step 1, graphite is prepared into reexpansion graphite；
Step 2, described reexpansion graphite, dispersant 5:1～1:5 in mass ratio are mixed to get mixed dispersion；
Step 3, described mixed dispersion is carried out mechanical shearing stripping；
Step 4, obtains single-layer graphene dispersion liquid；
Described dispersant includes: dodecylbenzene sodium sulfonate, Polyvinylpyrrolidone, sodium cholate, polystyrene, cetyl three
One or more of methyl bromide ammonium；
In described step 2, described mixed dispersion also includes: water or solvent；
Described solvent includes: Ketocyclopentane, Ketohexamethylene, piperidines -1- formaldehyde, vinyl pyrrolidone, 1,3- dimethyl -2- imidazoles
Quinoline, bromobenzene, benzonitrile, benzyl benzoic acid, n, n- dimethyl propylene thiazolinyl urea ketone, n- ethyl-2-pyrrolidone, n- methylpyrrole
Alkanone, acetic acid dimethylamide, cyclohexyl pyrrolidone, benzyl oxide, isopropanol, n- octylpyrrolidone, dioxolanes, ethyl acetate,
1- quinoline, benzaldehyde, ethanolamine, ethyl phthalate, n- dodecyl pyrrolidone, pyridine, dimethyl phthalate, ethanol, third
Ketone, vinyl acetate, ethylene glycol, toluene, heptane, pentane, hexane, Methanamide, dimethylformamide, dimethyl sulfoxide, dichloro
For benzene, chloroform, one or more of oxolane.
In described step 3, the equipment that described mechanical shearing adopts includes: ball mill, mulser, dispersion machine, grinder, homogeneous
One or more of machine, fluid collider.
2. the preparation method of single-layer graphene dispersion liquid as claimed in claim 1 is it is characterised in that the speed of described mechanical shearing
Spend for 2000～15000 revs/min, and/or, the time of described mechanical shearing is 1～30 hour.
3. the preparation method of the single-layer graphene dispersion liquid as described in any one of claim 1-2 is it is characterised in that described step
In 1, the preparation method of described reexpansion graphite includes:
Described graphite is carried out oxidation processes by step a.；
Graphite after the process of step a is carried out expansion process by step b.；
Graphite after the process of step b is carried out oxidation processes by step c. again；
Graphite after the process of step c is carried out high temperature reduction expansion and obtains reexpansion graphite by step d..
4. the preparation method of single-layer graphene dispersion liquid as claimed in claim 3 is it is characterised in that in described step a, in oxygen
During change is processed, the mass ratio 25:1～45:1 of wherein graphite and oxidant, the oxidant of employing includes: sulphuric acid, nitric acid, permanganic acid
One or more of potassium, potassium chlorate, hydrogen peroxide, hypochlorous acid, nitrous acid.
5. the preparation method of single-layer graphene dispersion liquid as claimed in claim 3 is it is characterised in that in described step d, described
The temperature that high temperature reduction expands is 600～1800 DEG C.
6. the single-layer graphene of the preparation method preparation of single-layer graphene dispersion liquid described in a kind of any one by claim 1-5
Dispersion liquid is it is characterised in that include: the Graphene of 1～10wt%, 0.01～5wt% dispersant；Described graphene dispersing solution
Concentration is 10～60mg ml-1, a diameter of 200 nanometers～10 microns of Graphene；Described dispersant is DBSA
Sodium, Polyvinylpyrrolidone, sodium cholate, polystyrene, one or more of cetyl trimethylammonium bromide.
7. single-layer graphene dispersion liquid as claimed in claim 6 is it is characterised in that also include: water or solvent, described solvent bag
Include: Ketocyclopentane, Ketohexamethylene, piperidines -1- formaldehyde, vinyl pyrrolidone, 1,3- dimethyl -2- imidazoline, bromobenzene, benzonitrile, benzene
Benzoin methyl acid, n, n- dimethyl propylene thiazolinyl urea ketone, n- ethyl-2-pyrrolidone, n- methyl pyrrolidone, dimethylamino acetyl
Amine, cyclohexyl pyrrolidone, benzyl oxide, isopropanol, n- octylpyrrolidone, dioxolanes, ethyl acetate, 1- quinoline, Benzoinum
Aldehyde, ethanolamine, ethyl phthalate, n- dodecyl pyrrolidone, pyridine, dimethyl phthalate, ethanol, acetone, vinyl acetate,
Ethylene glycol, toluene, heptane, pentane, hexane, Methanamide, dimethylformamide, dimethyl sulfoxide, dichlorobenzene, chloroform, tetrahydrochysene
One or more of furan.
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|---|---|---|---|---|
| WO2016101208A1 (en) * | 2014-12-25 | 2016-06-30 | 北京航空航天大学 | Single-layer graphene dispersion liquid and preparation method therefor |
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| CN101993061A (en) * | 2009-08-19 | 2011-03-30 | 中国科学院金属研究所 | Method for preparing high-quality graphene with controllable layer number |
| CN103935997A (en) * | 2014-05-10 | 2014-07-23 | 由伟 | Method for producing graphene based on sodium dodecylbenzene sulfonate |
| CN104151582B (en) * | 2014-07-17 | 2017-03-29 | 哈尔滨工业大学 | A kind of preparation method of Graphene polyimides conduction black film |
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