CN106185895A - A kind of graphene dispersion liquid and preparation method thereof - Google Patents
A kind of graphene dispersion liquid and preparation method thereof Download PDFInfo
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- CN106185895A CN106185895A CN201610525644.1A CN201610525644A CN106185895A CN 106185895 A CN106185895 A CN 106185895A CN 201610525644 A CN201610525644 A CN 201610525644A CN 106185895 A CN106185895 A CN 106185895A
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Abstract
The invention belongs to graphene dispersing solution preparing technical field, relate to a kind of graphene dispersion liquid and preparation method thereof, preparation method includes prepared by dispersant solution, one time high shear liquid phase is peeled off and secondary high-pressure three processing steps of stripping: first dissolves the dispersant into and prepares dispersant solution in solvent, then graphite raw material is joined in dispersant solution, carry out a high shear liquid phase by high shear force and peel off the graphite slurry once peeled off, the graphite slurry once peeled off is applied the pressure of 10～400MPa again, then micro slit it is passed to, with broken valve generation strong collision, the graphite slurry once peeled off is carried out secondary stripping by powerful shearing force and impact force, make the dispersion of graphene uniform in a solvent, prepare uniform graphene dispersing solution；The graphene dispersing solution quality prepared is high, and uniform and stable property is good, production process environmental protection, reduces environmental pollution, and production technology is simple, it is easy to industrialization large-scale production, and yield is high, low cost, and applied environment is friendly.
Description
Technical field:
The invention belongs to graphene dispersing solution preparing technical field, relate to a kind of side preparing high-quality graphene dispersion liquid
Method, peels off the graphene dispersing solution of directly prepared high stability especially by a high shear liquid phase stripping and secondary high-pressure
Environmental protection method.
Background technology:
The two dimensional crystal that Graphene is made up of one layer of carbon atom, be in the world known to the thinnest, the hardest nanometer material
Material, it is almost fully transparent, only absorbs the light of 2.3%；Heat conductivity is up to 5300W/m K, higher than CNT and gold
Hard rock, under room temperature, its electron mobility is more than 15000cm2/ V s, and resistivity only about 10-8Ω m, for world resistivity
Minimum material, scientist even foretells that Graphene " will thoroughly change 21 century ", it is most likely that starts one and have swepts the globe
Subversiveness new technique new industrial revolution.The physicist An Deliegaimu of Univ Manchester UK in 2004 and Constant
Ding Nuowoxiao love successfully isolates Graphene from graphite, common acquisition Nobel Prize in physics in 2010；Since stone
Since ink alkene is found, the preparation method of Graphene is always the study hotspot of scientists, the most relatively common Graphene
Preparation method has mechanical stripping method, oxidation-reduction method, chemical vapour deposition technique and epitaxial growth method etc., epitaxial growth method and chemistry
Vapour deposition process all can obtain high quality monolayer Graphene, but both complex process, yielding poorly, cost is high, to graphite-based
The end, requires higher, is not suitable for industrialization large-scale production；Oxidation-reduction method is relatively suitable for large-scale production, but needs in production process
Consuming a large amount of concentrated sulphuric acid and heavy metallic salt, cause cost of sewage disposal to increase, environmental pollution is serious, and graphite oxidation
Process can introduce substantial amounts of defect, thus destroys the crystal structure of Graphene, causes the disappearance of electric property；And the adhesive tape of routine
Although mechanical stripping method can obtain the high quality monolayer Graphene of sheet, but efficiency is the lowest, is not suitable for batch production；As super
, easily there is the situation that dispersion is uneven in graphene dispersing solution prepared by the traditional handicrafts such as sound method, and dispersion liquid is placed the most just
Settling, it is uneven that this in use can cause Graphene to disperse in the material, causes the effect of Graphene to give a discount greatly
, even there is retroaction in button.Therefore, explore and seek a kind of environmental protection method preparing high-quality graphene dispersion liquid, pass through
One time high shear liquid phase is peeled off and the graphene dispersing solution of the prepared high stability of secondary high-pressure stripping, reduces environmental pollution, is suitable to
Batch production.
Summary of the invention:
It is an object of the invention to the shortcoming overcoming prior art to exist, propose one and prepare high-quality graphene dispersion liquid
Environmental protection method, to solve the uneven problem of graphene dispersing solution prepared, overcome existing complex manufacturing, yield
The defect that low and cost is high, improves and produces the present situation that environment causes severe contamination.
To achieve these goals, the environmental protection preparation method of the high-quality graphene dispersion liquid that the present invention relates to includes
Prepared by dispersant solution, a high shear liquid phase is peeled off and secondary high-pressure three processing steps of stripping:
(1), prepared by dispersant solution: dissolves the dispersant into and prepares dispersant solution, the weight of described dispersant in solvent
Amount degree is the 0.1～20% of solvent；Described dispersant be dodecylbenzene sodium sulfonate, sodium lauryl sulphate,
Dodecyl sodium sulfate, cetyl trimethylammonium bromide, benzalkonium chloride, benzalkonium bromide, polyvinylpyrrolidone, sulfomethylated lignin
One or more mixture mixed in any proportion in acid sodium, Polyethylene Glycol or chitosan；Described solvent be deionized water,
Ethanol, N-N-dimethylformamide, toluene, N-Methyl pyrrolidone, ether, chloroform, acetone, oxolane, pyridine, pyrrole
Cough up or one or more mixture mixed in any proportion in dimethyl sulfoxide；
(2), a high shear liquid phase is peeled off: is joined by graphite raw material in the dispersant solution that step (1) prepares, then leads to
Cross high shear force and carry out the graphite slurry that a high shear liquid phase stripping is once peeled off；The weight percent of described graphite raw material
Than 0.1～30% that content is solvent；Described graphite raw material be crystalline flake graphite, spherical graphite, expansible graphite, expanded graphite,
One or more mixture mixed in any proportion in graphite oxide or highly directional cracking graphite；Described high shear forces power
Use for the one or more combination in homogenizer, ball mill, sand mill, mulser or colloid mill；
(3), secondary high-pressure is peeled off: the graphite slurry once peeled off first obtained step (2) applies 10～400MPa
Pressure, is then passed to micro slit, when high-pressure fluid can be produced by the instantaneous normal pressure of being down to of supertension when by micro slit
The raw speed times over velocity of sound, last and broken valve generation strong collision, the graphite slurry once peeled off is by powerful shearing force
Carry out secondary stripping with impact force, make the dispersion of graphene uniform in a solvent, prepare uniform graphene dispersing solution by material
Mouth is collected；The width of described micro slit is 0.1～20mm；Described broken valve material is metal alloy, diamond or nitride
Pottery；It is 1～20 time that described high-voltage secondary peels off number of times.
Compared with prior art, the graphene dispersing solution quality obtained through twice stripping is high, uniform and stable property for the present invention
Good；Production process environmental protection, reduces environmental pollution；Production technology is simple, it is easy to industrialization large-scale production, and yield is high, becomes
This is low, and applied environment is friendly.
Accompanying drawing illustrates:
Fig. 1 is the structural principle schematic diagram that graphite slurry carries out secondary high-pressure stripping system.
Detailed description of the invention:
Below by specific embodiment and combine accompanying drawing the invention will be further described.
Embodiment 1:
The environmental protection method preparing high-quality graphene dispersion liquid involved by the present embodiment includes dispersant solution system
Standby, a high shear liquid phase is peeled off and secondary high-pressure three processing steps of stripping:
(1), prepared by dispersant solution: join in 1000g deionized water solvent by 1g sodium lauryl sulphate dispersant,
Fully dissolve and prepare dispersant solution.
(2), a high shear liquid phase is peeled off: 10g graphite raw material crystalline flake graphite joins the dispersant that step (1) prepares
In solution, then carry out ball-milling treatment by ball mill, under high shear, carry out a high shear liquid phase stripping obtain one
The graphite slurry of secondary stripping.
(3), secondary high-pressure is peeled off: carrying out in secondary high-pressure stripping system, first obtain step (2) once peels off
Graphite slurry 2 applies the pressure of 100MPa by piston 1, is then passed to the slit 3 of 1mm width, when high-pressure graphite slurry
Fluid can be produced the speed times over velocity of sound by the instantaneous normal pressure of being down to of supertension when by slit 3, finally impinges upon nitride
On the broken valve 4 of ceramic material, the graphite slurry once peeled off is carried out secondary stripping, secondary by powerful shearing force and impact force
Stripping is carried out 1 time, makes the dispersion of graphene uniform in a solvent, prepares high-quality uniform graphene dispersing solution by material mouth
5 collect, and are stood by prepared graphene dispersing solution and the most substantially settle for 2 months.
Embodiment 2:
The environmental protection method preparing high-quality graphene dispersion liquid involved by the present embodiment includes dispersant solution system
Standby, a high shear liquid phase is peeled off and secondary high-pressure three processing steps of stripping:
(1), prepared by dispersant solution: 2g dodecylbenzene sodium sulfonate dispersant is joined 1000g N-N-dimethyl methyl
In amide solvent, fully dissolve and prepare dispersant solution；
(2), a high shear liquid phase is peeled off: 50g graphite raw material graphite oxide joins the dispersant that step (1) prepares
In solution, then carry out sanded treatment by sand mill, under high shear, carry out a high shear liquid phase stripping obtain one
The graphite slurry of secondary stripping；
(3), secondary high-pressure peels off: the graphite slurry once peeled off that first obtains step (2) applies the pressure of 200MPa,
Then the slit of 0.5mm width it is passed to, when high-pressure fluid can be produced by the instantaneous normal pressure of being down to of supertension when by slit
Times over the speed of velocity of sound, finally impinging upon on the broken valve of metal alloy material, the graphite slurry once peeled off is by powerful
Shearing force and impact force carry out secondary stripping, and circulation secondary is peeled off 20 times, makes the dispersion of graphene uniform in a solvent, thus makes
Obtain high-quality uniform graphene dispersing solution；Prepared graphene dispersing solution is stood and within 3 months, the most substantially settles.
Embodiment 3:
The environmental protection method preparing high-quality graphene dispersion liquid involved by the present embodiment includes dispersant solution system
Standby, a high shear liquid phase is peeled off and secondary high-pressure three processing steps of stripping:
(1), prepared by dispersant solution: 10g dodecylbenzene sodium sulfonate dispersant is joined 1000g tetrahydrofuran solvent
In, fully dissolve and prepare dispersant solution；
(2), a high shear liquid phase is peeled off: 100g graphite raw material expansible graphite joins prepared the dividing of step (1)
In dispersant solution, then carry out high-speed stirred process by homogenizer, under high shear, carry out a high shear liquid
Peel off the graphite slurry once peeled off mutually；
(3), secondary high-pressure peels off: the graphite slurry once peeled off that first obtains step (2) applies the pressure of 150MPa,
Then the slit of 0.3mm width it is passed to, when high-pressure fluid can be produced by the instantaneous normal pressure of being down to of supertension when by slit
Times over the speed of velocity of sound, finally impinging upon on the broken valve of diamond material, the graphite slurry once peeled off is cut by powerful
Shear force and impact force carry out secondary stripping, and circulation secondary is peeled off and carried out 5 times, makes the dispersion of graphene uniform in a solvent, thus
Prepare high-quality uniform graphene dispersing solution.Prepared graphene dispersing solution is stood and within 3 months, the most substantially settles.
Claims (1)
1. a graphene dispersion liquid and preparation method thereof, it is characterised in that its preparation method include dispersant solution prepare, one second highest
Shear liquid phase to peel off and secondary high-pressure three processing steps of stripping:
(1), prepared by dispersant solution: dissolves the dispersant into and prepares dispersant solution, the weight hundred of described dispersant in solvent
Proportion by subtraction content is the 0.1～20% of solvent；Described dispersant be dodecylbenzene sodium sulfonate, sodium lauryl sulphate, 12
Sodium alkyl sulfonate, cetyl trimethylammonium bromide, benzalkonium chloride, benzalkonium bromide, polyvinylpyrrolidone, lignin sulfonic acid
One or more mixture mixed in any proportion in sodium, Polyethylene Glycol or chitosan；Described solvent is deionized water, second
Alcohol, N-N-dimethylformamide, toluene, N-Methyl pyrrolidone, ether, chloroform, acetone, oxolane, pyridine, pyrroles
Or the mixture that one or more in dimethyl sulfoxide mix in any proportion；
(2), a high shear liquid phase is peeled off: is joined by graphite raw material in the dispersant solution that step (1) prepares, then passes through height
Shearing force carries out a high shear liquid phase and peels off the graphite slurry once peeled off；The percentage by weight of described graphite raw material contains
Amount is the 0.1～30% of solvent；Described graphite raw material is crystalline flake graphite, spherical graphite, expansible graphite, expanded graphite, oxidation
One or more mixture mixed in any proportion in graphite or highly directional cracking graphite；Described high shear forces power is high
One or more combination in speed blender, ball mill, sand mill, mulser or colloid mill uses；
(3), secondary high-pressure peels off: the graphite slurry once peeled off that first obtains step (2) applies the pressure of 10～400MPa,
Then micro slit it is passed to, when high-pressure fluid can be produced several times by the instantaneous normal pressure of being down to of supertension when by micro slit
In the speed of velocity of sound, last and broken valve generation strong collision, the graphite slurry once peeled off is by powerful shearing force and collision
Power carries out secondary stripping, makes the dispersion of graphene uniform in a solvent, prepares uniform graphene dispersing solution and is collected by material mouth；
The width of described micro slit is 0.1～20mm；Described broken valve material is metal alloy, diamond or nitride ceramics；Institute
Stating high-voltage secondary and peeling off number of times is 1～20 time.
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| CN106542527A (en) * | 2017-01-06 | 2017-03-29 | 成都新柯力化工科技有限公司 | A kind of method of mechanical stripping grading system for graphene microchip dispersion liquid |
| CN106587027A (en) * | 2017-01-05 | 2017-04-26 | 苏州高通新材料科技有限公司 | Method for rapidly preparing small-dimensional graphene |
| CN106744862A (en) * | 2017-03-20 | 2017-05-31 | 青岛科技大学 | A kind of large stretch of layer graphene aqueous dispersions and preparation method thereof |
| CN106829928A (en) * | 2017-01-26 | 2017-06-13 | 北京清烯科技有限公司 | The preparation method of large-area graphene |
| CN107827102A (en) * | 2017-11-27 | 2018-03-23 | 内蒙古碳烯石墨新材料有限公司 | A kind of method for preparing graphene |
| CN108117069A (en) * | 2018-01-23 | 2018-06-05 | 杭州高烯科技有限公司 | A kind of method for concentration and device of sheet graphene oxide solution |
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