CN105110318B - A kind of graphene water paste and preparation method thereof - Google Patents
A kind of graphene water paste and preparation method thereof Download PDFInfo
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Abstract
The present invention is applied to grapheme material field, provide a kind of graphene water paste and preparation method thereof, the graphene water paste includes aqueous liquid dispersion and the grapheme material being dispersed in the aqueous liquid dispersion, wherein, contain surfactant in the aqueous liquid dispersion.The preparation method of the graphene water paste comprises the following steps：Using oxidation graphite solid or expansible graphite solid as raw material, expansion process is carried out, prepares expanded graphite；The expanded graphite is soaked in into infiltration in water-based stripper to handle, obtains the mixture containing expanded graphite；The mixture containing expanded graphite is subjected to high speed shear or ultrasonication, the water-based stripper is removed, obtains graphene wet feed；The graphene wet feed is placed in aqueous liquid dispersion, high speed shear processing is carried out, obtains graphene water paste.
Description
Technical field
The invention belongs to grapheme material field, more particularly to a kind of graphene water paste and preparation method thereof.
Background technology
It is a kind of new carbon nanomaterial that graphene, which is made, its nanometer as current most thin in the world (monoatomic thickness)
Material, abundant and peculiar physical and chemical performance is contained, such as huge specific surface area (2,630m2·g-1), higher Young's modulus
(- 1.0TPa), higher inherent electron mobility (200,000cm2·v-1·s-1), thermal conductivity (5,000Wm-1·K-1), lead
Electrical and transparency (97.7%).The above-mentioned advantage of graphene so that it is widely used in multiple fields, as electrically conducting transparent is thin
Film, sensor, polymer composites, energy storage material, biological medicine, heat-conductive coating, anticorrosive paint etc..
At present, the preparation method of graphene mainly has oxidation-reduction method, liquid phase stripping method, mechanical stripping method, vapor- phase synthesis
Method.Wherein, mechanical stripping method and gas phase synthesis method can prepare zero defect graphene film, but yield is extremely low.Oxidation-reduction method and
Liquid phase stripping method is the main method of current industrial production graphene powder.Have yet with graphene powder and greatly compare table
Area, easily lumpd using common furnace drying method, cause serious lamella to stack and reunite, cause in later stage application process, stone
Black alkene is difficult to disperse；Freeze drying process power consumption is big, efficiency is low.Further, since fluffy graphene powder density is extremely low, Workflow
Raise, brought inconvenience during packed and transported and use.
The content of the invention
It is an object of the invention to provide a kind of graphene water paste and preparation method thereof, it is intended to while solve existing stone
Lamella easily reunites, causes graphene dispersion and application difficult in black alkene powder；And Graphene powder volume density is light, packaging fortune
Defeated difficulty；And graphene size it is unmanageable the problem of.
The present invention is achieved in that the graphene water paste includes aqueous liquid dispersion and is dispersed in described water-based point
Grapheme material in dispersion liquid, wherein, contain surfactant in the aqueous liquid dispersion.
And a kind of preparation method of graphene water paste, comprise the following steps：
Using oxidation graphite solid or expansible graphite solid as raw material, expansion process is carried out, prepares expanded graphite；
The expanded graphite is soaked in into infiltration in water-based stripper to handle, obtains the mixture containing expanded graphite；
The mixture containing expanded graphite is subjected to high speed shear or ultrasonication, removes the water-based stripper,
Obtain graphene wet feed；
The graphene wet feed is placed in aqueous liquid dispersion, high speed shear processing is carried out, obtains graphene water paste.
Graphene water paste provided by the invention, the grapheme material are dispersed in the aqueous dispersion, and institute
State and contain surfactant in aqueous dispersion so that the grapheme material is scattered more uniformly, the grapheme material chi
It is very little more controllable.
A kind of preparation method of graphene water paste provided by the invention, oxidation graphite solid or expansible graphite are consolidated
After body carries out expansion process, the expanded graphite of different expansion multiplying powers is can obtain, it is strict that the expanded graphite is placed in into surface tension
After fully being soaked in the water-based stripper of control, high speed shear or ul-trasonic irradiation, the surface of the water-based stripper are carried out
Power makes the nanoscale twins of expansion sufficiently be dissociated and disperseed, so as to effectively prevent the accumulation of graphene sheet layer and reunion,
Improve dispersive property when graphene uses.After the high speed shear or ultrasonication, the graphene wet feed is again
Disperse in a solvent, in the presence of surfactant, through high speed shear, ball milling, sand milling or ul-trasonic irradiation, to can obtain highly concentrated
The controllable graphene water paste of degree, size.The preparation method technique of graphene water paste of the present invention is simple and environmentally-friendly, can be real
It is prepared by the batch of the existing graphene water paste；And by controlling the oxygen content of raw material and peeling off dispersing technology, it can control
The size of graphene in the graphene water paste, so as to solve the difficult control of graphene size, graphene powder is easily reunited, close
The problems such as degree is light, packed and transported is difficult, difficult scattered.Graphene water paste prepared by the inventive method, can be applied to conductive and heat-conductive
The fields such as coating, anticorrosive paint, battery/ultracapacitor.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of graphene in the graphene water paste that the embodiment of the present invention 3 provides；
Fig. 2 is the infrared spectrogram of graphene in the graphene water paste that the embodiment of the present invention 3 provides.
Embodiment
In order that technical problems, technical solutions and advantageous effects to be solved by the present invention are more clearly understood, below in conjunction with
Drawings and Examples, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used
To explain the present invention, it is not intended to limit the present invention.
The embodiments of the invention provide a kind of graphene water paste, the graphene water paste includes aqueous liquid dispersion
And the grapheme material in the aqueous liquid dispersion is dispersed in, wherein, contain surfactant in the aqueous liquid dispersion.
As a preferred embodiment, counted using the gross mass of the graphene water paste as 100%, the graphene
Weight/mass percentage composition is 0.1-10%.Specifically, the weight/mass percentage composition of the graphene can be 0.1%, 0.2%, 0.5%,
0.8%th, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%.Graphene-structured in the graphene water paste
Can be single-layer graphene or a small number of layer graphene microplates, but thickness is in Nano grade.
As another preferred embodiment, the surface tension of the aqueous liquid dispersion is 40-50mN/m.Suitable surface
Force value, it is ensured that the grapheme material is not reunited, so as to obtain the scattered graphene water paste being more uniformly distributed.
Graphene water paste provided in an embodiment of the present invention, the grapheme material are dispersed in the aqueous dispersion
In, and containing surfactant in the aqueous dispersion so that the grapheme material is scattered more uniformly, the graphene
Scantling is more controllable.
Accordingly, also a kind of preparation method of graphene water paste of the embodiment of the present invention comprises the following steps：
S01. using oxidation graphite solid or expansible graphite solid as raw material, expansion process is carried out, prepares expanded graphite；
S02. the expanded graphite is soaked in into infiltration in water-based stripper to handle, obtains the mixture containing expanded graphite；
S03. the mixture containing expanded graphite is subjected to high speed shear or ultrasonication, removes the stripper,
Obtain graphene wet feed；
S04. the graphene wet feed is placed in aqueous liquid dispersion, carries out high speed shear processing, it is water-based to obtain graphene
Slurry.
Specifically, in above-mentioned steps S01, the embodiment of the present invention uses oxidation graphite solid or expansible graphite solid conduct
Raw material.The selection of the oxidation graphite solid or expansible graphite solid is unrestricted, can voluntarily prepare or market purchase obtains
.Specifically, the graphite oxide can use the Hummers methods of current relative maturity, Brodie methods, Staudenmaier methods or
Its modified technique is synthesized；The expansible graphite uses commercially available high purity product.
The oxygen content of graphite oxide raw material is higher, and specific surface area is bigger during expansion, finally peels off obtained graphene product
Thinner, specific surface area is bigger, and slurry is more black；The preparation of graphite oxide typically uses Fine particle processing, and feed particles are to product
Performance impact is little.As a particular preferred embodiment, the granular size of the graphite oxide is 200-1000 mesh, oxygen content
It is Strong oxdiative intercalation product for 30-50%.Similar with graphite oxide, expansible graphite oxygen content is higher, and product is thinner, compares table
Area is bigger, and paste color is deeper；The preparation of expansible graphite typically uses flaky graphite, and expansible graphite raw materials size
It is little to final products performance impact.As another preferred embodiment, the granular size of the expansible graphite is 30-200
Mesh, oxygen content 5-15%, it is weak oxide intercalation product.Of course it is to be understood that raw material described in the embodiment of the present invention can also be adopted
The moderate oxidation intercalation product prepared with similar expansible graphite synthesis technique, as particular preferred embodiment, in described
Oxygen content etc. degree oxidation intercalation product is 15-30%.In the embodiment of the present invention, using different raw materials, difference will be obtained
The graphene water paste of thickness.
In the embodiment of the present invention, in order to obtain the preferable expanded graphite of expansion effect, the expansion process is preferably using height
Temperature expansion or microwave expansion are realized.As particular preferred embodiment, the temperature of the high-temperature expansion is 200-1100 DEG C, during expansion
Between be 3s-60s；Or the power of the microwave expansion is 500-2800W, Bulking Time 3-600s.
Because expanded graphite specific surface area it is relatively low when, peeling effect is poor, and more crystalline flake graphite piece is remained in product, influences to starch
The using effect of material.As the presently preferred embodiments, specific surface area of the raw material after the expansion process is not less than 20m2/g。
In above-mentioned steps S02, the addition of water-based stripper described in the embodiment of the present invention, the expanded graphite can be caused to fill
Decompose from and it is scattered, so as to effectively prevent the reunion of graphene sheet layer, and then dispersive property when improving its use.It is of the invention real
Apply in example, suitable surface tension value, it is ensured that the expanded graphite is in optimal and peeled off in environment, so as to obtain preferably
Peeling effect, and then the graphene for preventing from subsequently obtaining is reunited.As the presently preferred embodiments, the surface of the water-based stripper
Tension force is 40-50mN/m.Further, in order to ensure the effect of the infiltration processing so that the expanded graphite fully dissociates,
Scattered, the content of the expanded graphite and the water-based stripper is than there is strict limitation.As the presently preferred embodiments, the expansion
The content ratio of graphite and the water-based stripper is 1g：(50-1000) ml, concretely 1g:50ml、1g:100ml、1g:
200ml、1g:300ml、1g:400ml、1g:500ml、1g:600ml、1g:700ml、1g:800ml、1g:900ml、1g:
1000ml。
The solvent of water-based stripper described in the embodiment of the present invention can select organic solvent or inorganic solvent, the water-based stripping
Chaotropic can be made up of one or more solvents.As the presently preferred embodiments, in the water-based stripper solvent be individually selected from from
Sub- water, ammoniacal liquor, formic acid, acetic acid, methanol, ethanol, glycerine, acetone, normal propyl alcohol, n-octyl alcohol, isooctanol, dimethyl sulfoxide, acetonitrile,
At least one of dimethylformamide, dioxane, tetrahydrofuran.
As particular preferred embodiment, in order that the water-based stripper is obtained in above-mentioned surface tension range, the water
Property stripper is optionally added surfactant.As particular preferred embodiment, the surface in the water-based stripper is lived
Property agent be selected from neopelex, polyvinylpyrrolidone, sodium lignin sulfonate, sodium taurocholate, stearic acid, tricresyl phosphate fourth
Acid, silane coupler, TBAB, sodium citrate, cetyl trimethylammonium bromide, polyoxyethylene laurel ether, tween
80th, triton X-100, dibutyltin oxide, Disperbyk-163, lysine, it is poly- between sub- phenylethylene derivative, DsPE,
At least one of DNA, polyvinyl alcohol.The dosage of the surfactant by the water-based stripper solvent species and dosage
Determine, preferably make the surface tension of the stripper in 40-50mN/m scopes.
Infiltration processing described in the embodiment of the present invention can be preferably using stirring wetting realization, further, the expansion stone
It is 0.5-4h that ink stirs or soaked infiltrating time in the water-based stripper.
In above-mentioned steps S03, under conditions of above-mentioned water-based stripper infiltration, particularly surface tension is 40-50mN/m
Under conditions of, yield is prepared using the auxiliary of shearing dissociation or ultrasound dissociation, the quick dissociation of the expanded graphite, its single
Greatly, it may be implemented in expanded graphite in 1 hour quickly to dissociate, meet industrial production demand.
Specifically, in the high speed shear or ultrasonication, power and splitting time are peeled off to graphene sheet layer size
Influence very big, high power, the prolonged water paste peeled off, the thin graphene of small size, lamella can be obtained；On the contrary, low-power,
The stripping of short time, the water paste of big size graphene can be obtained.In the embodiment of the present invention, the high speed shear or ultrasonic wave
In processing, the rotating speed of the high speed shear is 2000-40000rpm, shear time 10-400min；Or the ultrasonic power
For 50-3000W, ultrasonic treatment time 10-600min.By the stripping work(for adjusting the high speed shear or ultrasonication
Rate and splitting time, the controllable graphene wet feed of size can be obtained.
In the embodiment of the present invention, remove the water-based stripper and obtain graphene wet feed, natural subsidence can be taken, centrifuged
Filter, air press filtration, one or more of realizations of vacuum filtration.
In above-mentioned steps S04, to obtain graphene water paste, it is necessary to by graphene filter cake wet feed in SO3 in a solvent
Again decentralized processing, the solvent is at least one of deionized water or absolute ethyl alcohol, further, to obtain high stability
Graphene water paste, certain surfactant can be added into solvent, be particularly preferred as neopelex, poly- second
Alkene pyrrolidone, sodium lignin sulfonate, sodium taurocholate, stearic acid, tricresyl phosphate butyric acid, silane coupler, TBAB, lemon
Sour sodium, cetyl trimethylammonium bromide, polyoxyethylene laurel ether, Tween 80, triton X-100, dibutyltin oxide,
Disperbyk-163, lysine, it is poly- between at least one of sub- phenylethylene derivative, DsPE, DNA, polyvinyl alcohol.As
Preferred embodiment, the surface tension of the aqueous liquid dispersion is 40-50mN/m, in favor of disperseing for grapheme material.
By the graphene wet feed and aqueous liquid dispersion, high speed shear, ball milling, sand milling or ultrasonication are further carried out
Graphene microchip is set to be uniformly dispersed, when the rotating speed of the high speed shear, shear time, the ultrasonic power, ultrasonication
Between can refer to above-mentioned steps S03 parameter setting, the rotating speed of the ball milling is 100-1000rpm, Ball-milling Time 2-48h；
The rotating speed of the sand milling is 500-5000rpm, and the sand milling time is 2-48h.
The preparation method of graphene water paste provided in an embodiment of the present invention, there is advantages below：
First, the embodiment of the present invention is using graphite oxide or expansible graphite as raw material, and raw material is cheap and easy to get, and the present invention
The technique that embodiment prepares graphene water paste is simple, easily-controllable, prepared by the batch that the graphene water paste can be achieved；
Second, after oxidation graphite solid or expansible graphite solid are carried out expansion process by the embodiment of the present invention, it can obtain
The expanded graphite of different expansion multiplying powers, the expanded graphite is placed in the water-based stripper that surface tension strictly controls and fully moistened
After wet, carrying out high speed shear or ul-trasonic irradiation, the surface tension of the water-based stripper is filled the graphite flake layer of expansion
Divide, efficiently dissociate and disperse, so as to effectively prevent the accumulation of graphene sheet layer and reunion, improve when graphene uses
Dispersive property.
3rd, the embodiment of the present invention is using the water-based stripper that surface tension is 40-50mN/m, in shearing dissociation or ultrasound
Under the booster action of dissociation, single preparation yield is big, may be implemented in expanded graphite in 1 hour and quickly dissociates；The embodiment of the present invention
Using surface tension be 40-50mN/m aqueous liquid dispersion, make graphene water paste stable performance, meet industrialized production and
Application demand.
4th, the preparation method of graphene water paste described in the embodiment of the present invention, the size of the graphene sheet layer can
By feed change oxygen content, so as to solve graphene size problem rambunctious.
5th, water-based stripper described in the embodiment of the present invention is recyclable, is reused after formulated, to environmental hazard pole
Small, the graphene water paste is environment-friendly size.
Graphene water paste prepared by present invention method, can be applied to conductive and heat-conductive coating, anticorrosive paint, electricity
The fields such as pond/ultracapacitor.
Illustrated with reference to specific embodiment.
Experimental example 1
A kind of graphene water paste and preparation method thereof, comprises the following steps：
S11. 14g particle diameters are taken to be carried out for 80 mesh, the expansible graphite of oxygen content 10% in 1000 DEG C of high-temperature expansion stoves swollen
Swollen processing, 10g expanded graphites are prepared；
S12. it is 15% ammoniacal liquor and quality the expanded graphite to be soaked in into percent by volume in the deionized water for be placed in 3L
Concentration is 4 × 10-4Stirring moistening 1h, obtains the mixture containing expanded graphite in the mixing stripper of kg/kg n-octyl alcohol composition；
S13. the mixture containing expanded graphite is subjected to 800W ul-trasonic irradiation 4h, after centrifugal filtration, obtains stone
Black alkene filter cake；
S14. the graphene filter cake is scattered in 190g deionized waters, adds PVP and adjust surface tension in 40-50mN/m
In the range of, 6h is sanded in nanometer sand mill, obtains the graphene water paste of weight percentage about 5%, wherein graphene
Average platelet size is 1 μm.
Experimental example 2
A kind of graphene water paste and preparation method thereof, comprises the following steps：
S21. 14g particle diameters are taken to be carried out for 150 mesh, the expansible graphite of oxygen content 10% in industrial microwave oven at expansion
Reason, is prepared 10g expanded graphites；
S22. the expanded graphite is soaked in and is placed in that 1L percents by volume are 15% ammoniacal liquor and mass concentration is 4 × 10- 4Stirring moistening 1h, obtains the mixture containing expanded graphite in the mixing stripper of kg/kg n-octyl alcohol composition；
S23. the mixture containing expanded graphite is subjected to 1000W ul-trasonic irradiation 3h, after vacuum filtration, obtains stone
Black alkene filter cake；
S24. the graphene filter cake is scattered in 90g absolute ethyl alcohols, adds sodium citrate and adjust surface tension in 40-
In the range of 50mN/m, decentralized processing 3h is sheared, obtains the ethanol slurry of the graphene of weight percentage about 10%, wherein graphite
Alkene average platelet size is 15 μm.
Experimental example 3
A kind of graphene water paste and preparation method thereof, comprises the following steps：
S31. 15g particle diameters are taken to be carried out for 80 mesh, the expansible graphite of oxygen content 5% in 1000 DEG C of high-temperature expansion stoves swollen
Swollen processing, 10g expanded graphites are prepared；
S32. the expanded graphite is soaked in and is placed in that 2L percents by volume are 12% ammoniacal liquor and mass concentration is 3 × 10- 4Stirring moistening 0.5h, obtains the mixture containing expanded graphite in the mixing stripper of kg/kg isooctanol composition；
S33. the mixture containing expanded graphite is subjected to 2800W ul-trasonic irradiation 1h, after air press filtration, obtains stone
Black alkene filter cake；
S34. the graphene filter cake is scattered in 990g deionized waters, adds silane coupler regulation surface tension and exist
In the range of 40-50mN/m, ultrasonic disperse processing 2h, the graphene water paste of weight percentage about 1%, wherein graphite are obtained
Alkene average platelet size is 20 μm.
As shown in Figure 1, its is red for the scanning electron microscope (SEM) photograph of graphene in graphene water paste prepared by the embodiment of the present invention
External spectrum figure is as shown in Figure 2.
Experimental example 4
A kind of graphene water paste and preparation method thereof, comprises the following steps：
S41. 15g particle diameters are taken to be carried out for 150 mesh, the expansible graphite of oxygen content 15% in industrial microwave oven at expansion
Reason, is prepared 10g expanded graphites；
S42. the expanded graphite is soaked in and is placed in that 4L percents by volume are 12% ammoniacal liquor and mass concentration is 3 × 10- 4Stirring moistening 0.5h, obtains the mixture containing expanded graphite in the mixing stripper of kg/kg isooctanol composition；
S43. the mixture containing expanded graphite is subjected to high speed shear effect 2h, after vacuum filtration, obtains graphite
Alkene filter cake；
S44. the graphene filter cake is scattered in 90g absolute ethyl alcohols, adds stearic acid and adjust surface tension in 40-
In the range of 50mN/m, high speed ball milling 4h is carried out, obtains the graphene ethanol slurry of weight percentage about 10%, wherein graphene
Average platelet size is 3 μm.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (4)
1. a kind of graphene water paste, it is characterised in that the graphene water paste includes aqueous liquid dispersion and is dispersed in
Grapheme material in the aqueous liquid dispersion,
The graphene water paste is prepared by following step：
Using oxidation graphite solid or expansible graphite solid as raw material, expansion process is carried out, prepares expanded graphite；
The expanded graphite is soaked in into infiltration in water-based stripper to handle, obtains the mixture containing expanded graphite；
The mixture containing expanded graphite is subjected to high speed shear or ultrasonication, the water-based stripper is removed, obtains
Graphene wet feed；
The graphene wet feed is placed in aqueous liquid dispersion, after carrying out high speed shear processing, carries out ball milling, sand milling or ultrasonic wave
Processing, obtains graphene water paste, the rotating speed of the ball-milling treatment is 100-1000rpm, Ball-milling Time 2-48h；And/or
The rotating speed of the sanded treatment is 500-5000rpm, and the sand milling time is 2-48h,
Wherein, surfactant is contained in the water-based stripper, the aqueous liquid dispersion, and the surfactant is wooden
Plain sodium sulfonate, stearic acid, tricresyl phosphate butyric acid, silane coupler, TBAB, sodium citrate, polyoxyethylene laurel ether, tell
Temperature 80, triton X-100, dibutyltin oxide, Disperbyk-163, lysine, it is poly- between sub- phenylethylene derivative, DsPE,
At least one of polyvinyl alcohol；
The water-based stripper, the surface tension of the aqueous liquid dispersion are 40-50mN/m.
2. graphene water paste as claimed in claim 1, it is characterised in that using the gross mass of the graphene water paste as
100% meter, the weight/mass percentage composition of the graphene is 0.1-10%.
3. graphene water paste as claimed in claim 1, it is characterised in that the expanded graphite is through high speed shear or ultrasonic wave
Processing, wherein,
The rotating speed of the high speed shear is 2000-40000rpm, shear time 10-400min；Or
The ultrasonic power is 50-3000W, ultrasonic treatment time 30-600min.
4. graphene water paste as claimed in claim 1, it is characterised in that the expanded graphite and the water-based stripper
Content ratio is 1g：(50-5000)ml.
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| CN101704520B (en) * | 2009-11-05 | 2012-05-23 | 华侨大学 | Method for producing graphene |
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| US9914108B2 (en) * | 2011-07-19 | 2018-03-13 | The Australian National University | Exfoliating laminar material by ultrasonication in surfactant |
| CN102583335B (en) * | 2012-01-19 | 2014-03-12 | 常州大学 | Preparation method of graphene uniform dispersion |
| CN103373724B (en) * | 2012-04-17 | 2015-05-20 | 安炬科技股份有限公司 | Method for preparing graphene composite material |
| CN104387446B (en) * | 2014-10-11 | 2017-07-07 | 中国石油大学(华东) | A kind of graphene dispersion agent and the preparation method of graphene dispersing solution |
| CN104495826B (en) * | 2014-12-25 | 2017-01-18 | 北京航空航天大学 | Single-layer graphene dispersion liquid and preparation method thereof |
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