CN105110318A - Graphene aqueous slurry, and preparation method thereof - Google Patents
Graphene aqueous slurry, and preparation method thereof Download PDFInfo
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- CN105110318A CN105110318A CN201510437868.2A CN201510437868A CN105110318A CN 105110318 A CN105110318 A CN 105110318A CN 201510437868 A CN201510437868 A CN 201510437868A CN 105110318 A CN105110318 A CN 105110318A
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Abstract
The invention belongs to the field of graphene material, and provides a graphene aqueous slurry, and a preparation method thereof. The graphene aqueous slurry comprises an aqueous dispersion liquid and a graphene material dispersed in the aqueous dispersion liquid, wherein the aqueous dispersion liquid contains a surfactant. The preparation method comprises following steps: graphite oxide solid or expansible graphite solid is taken as a raw material, and expansion treatment is carried out so as to prepare expanded graphite; the expanded graphite is immersed into an aqueous stripping liquid for infiltration treatment so as to obtain a mixture containing the expanded graphite; the mixture containing the expanded graphite is subjected to high-speed shearing or ultrasonic treatment so as to remove the aqueous stripping liquid so as to obtain a graphene wet material; the graphene wet material is added into the aqueous dispersion liquid, and high-speed shearing is carried out so as to obtain the graphene aqueous slurry.
Description
Technical field
The invention belongs to grapheme material field, particularly relate to a kind of Graphene water paste and preparation method thereof.
Background technology
It is a kind of novel carbon nanomaterial that Graphene is done, and it, as the nano material of current the thinnest (monoatomic thickness) in the world, has contained abundant and peculiar physical and chemical performance, as huge specific surface area (2,630m
2g
-1), higher Young's modulus (-1.0TPa), higher inherent electronic mobility (200,000cm
2v
-1s
-1), thermal conductivity (5,000Wm
-1k
-1), electroconductibility and transparency (97.7%).The above-mentioned advantage of Graphene, makes it be widely used in multiple field, as transparent conductive film, sensor, polymer composites, energy storage material, biological medicine, heat-conductive coating, protective system etc.
At present, the preparation method of Graphene mainly contains oxidation reduction process, liquid phase stripping method, mechanically peel method, gas phase synthesis method.Wherein, mechanically peel method and gas phase synthesis method can prepare zero defect graphene film, but productive rate is extremely low.Oxidation reduction process and liquid phase stripping method are the main method of current industrial production graphene powder.But there is great specific surface area due to graphene powder, adopt common furnace drying method easily to lump, cause serious lamella stacking and reunite, cause in later stage application process, Graphene is difficult to dispersion; Freeze drying process power consumption is large, efficiency is low.In addition, because fluffy graphene powder density is extremely low, easily fly upward, bring inconvenience in packed and transported and use procedure.
Summary of the invention
The object of the present invention is to provide a kind of Graphene water paste and preparation method thereof, be intended to solve lamella in existing graphene powder simultaneously and easily reunite, cause graphene dispersion and application difficult; And graphene powder density is light, packed and transported is difficult; And the unmanageable problem of Graphene size.
The present invention is achieved in that described Graphene water paste comprises aqueous liquid dispersion and is dispersed in the grapheme material in described aqueous liquid dispersion, wherein, containing tensio-active agent in described aqueous liquid dispersion.
And a kind of preparation method of Graphene water paste, comprises the following steps:
With oxidation graphite solid or expansible black lead solid for raw material, carry out expansion process, prepare expanded graphite;
Described expanded graphite is soaked in water-based stripping liquid and infiltrates process, obtain the mixture containing expanded graphite;
The described mixture containing expanded graphite is carried out high speed shear or ultrasonication, removes described water-based stripping liquid, obtain Graphene wet feed;
Described Graphene wet feed is placed in aqueous liquid dispersion, carries out high speed shear process, obtain Graphene water paste.
Graphene water paste provided by the invention, described grapheme material is dispersed in described aqueous dispersant, and containing tensio-active agent in described aqueous dispersant, described grapheme material is disperseed more even, described grapheme material size is more controlled.
The preparation method of a kind of Graphene water paste provided by the invention, after oxidation graphite solid or expansible black lead solid are carried out expansion process, the expanded graphite of different expansion multiplying power can be obtained, described expanded graphite is placed in water-based stripping liquid that surface tension strictly controls fully wetting after, carry out high speed shear or ul-trasonic irradiation, the surface tension of described water-based stripping liquid makes the nanoscale twins of expansion be dissociated fully and disperse, thus the heap sum that effectively prevent graphene sheet layer is reunited, improve dispersing property when Graphene uses.After described high speed shear or ultrasonication, described Graphene wet feed disperses in a solvent again, under the effect of tensio-active agent, through high speed shear, ball milling, sand milling or ul-trasonic irradiation, can obtain the Graphene water paste that high density, size are controlled.Preparation method's technique of Graphene water paste of the present invention is simple, environmental protection, can realize the batch preparation of described Graphene water paste; And pass through the oxygen level and the stripping dispersing technology that control raw material, the size of Graphene in described Graphene water paste can be controlled, thus solve the problem such as the control of Graphene size difficulty, graphene powder is easily reunited, density is light, packed and transported is difficult, difficult dispersion.Graphene water paste prepared by the inventive method, can be applicable to the fields such as conductive and heat-conductive coating, protective system, battery/ultracapacitor.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of Graphene in the Graphene water paste that provides of the embodiment of the present invention 3;
Fig. 2 is the infrared spectrogram of Graphene in the Graphene water paste that provides of the embodiment of the present invention 3.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiments provide a kind of Graphene water paste, described Graphene water paste comprises aqueous liquid dispersion and is dispersed in the grapheme material in described aqueous liquid dispersion, wherein, containing tensio-active agent in described aqueous liquid dispersion.
As a preferred embodiment, in the total mass of described Graphene water paste for 100%, the mass percentage of described Graphene is 0.1-10%.Concrete, the mass percentage of described Graphene can be 0.1%, 0.2%, 0.5%, 0.8%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%.In described Graphene water paste, graphene-structured can be single-layer graphene or minority layer graphene microplate, but thickness is all in Nano grade.
As another preferred embodiment, the surface tension of described aqueous liquid dispersion is 40-50mN/m.Suitable surface tension value, can ensure that described grapheme material is not reunited, thus obtains disperseing more uniform Graphene water paste.
The Graphene water paste that the embodiment of the present invention provides, described grapheme material is dispersed in described aqueous dispersant, and containing tensio-active agent in described aqueous dispersant, make described grapheme material disperse more even, described grapheme material size is more controlled.
Accordingly, the preparation method of the embodiment of the present invention also a kind of Graphene water paste comprises the following steps:
S01. with oxidation graphite solid or expansible black lead solid for raw material, carry out expansion process, prepare expanded graphite;
S02. described expanded graphite is soaked in water-based stripping liquid and infiltrates process, obtain the mixture containing expanded graphite;
S03. the described mixture containing expanded graphite is carried out high speed shear or ultrasonication, remove described stripping liquid, obtain Graphene wet feed;
S04. described Graphene wet feed is placed in aqueous liquid dispersion, carries out high speed shear process, obtain Graphene water paste.
Concrete, in above-mentioned steps S01, the embodiment of the present invention adopts oxidation graphite solid or expansible black lead solid as raw material.Selecting of described oxidation graphite solid or expansible black lead solid is unrestricted, can prepare voluntarily or market is bought and obtained.Concrete, described graphite oxide can adopt the Hummers method of current relative maturity, Brodie method, Staudenmaier method or its improving technique to synthesize; Described expansible black lead adopts commercially available high purity product.
The oxygen level of graphite oxide raw material is higher, and during expansion, specific surface area is larger, and finally peel off the graphene product obtained thinner, specific surface area is larger, and slurry is more black; The preparation of graphite oxide generally adopts Fine particle processing, and feed particles is little on product performance impact.As a concrete preferred embodiment, the granular size of described graphite oxide is 200-1000 order, and oxygen level is 30-50%, is Strong oxdiative intercalation product.Similar with graphite oxide, expansible black lead oxygen level is higher, and product is thinner, and specific surface area is larger, and paste color is darker; The preparation of expansible black lead generally adopts flaky graphite, and expansible black lead raw materials size is little to the finished product performance impact.As another preferred embodiment, the granular size of described expansible black lead is 30-200 order, and oxygen level is 5-15%, is weak oxide intercalation product.Of course it is to be understood that the moderate oxidation intercalation product that raw material described in the embodiment of the present invention also can adopt similar expansible black lead synthesis technique to prepare, as concrete preferred embodiment, the oxygen level of described moderate oxidation intercalation product is 15-30%.In the embodiment of the present invention, adopt different raw materials, will the Graphene water paste of different thickness be obtained.
In the embodiment of the present invention, in order to obtain the good expanded graphite of expansion effect, described expansion process preferably adopts high-temperature expansion or microwave expansion to realize.As concrete preferred embodiment, the temperature of described high-temperature expansion is 200-1100 DEG C, and Bulking Time is 3s-60s; Or the power of described microwave expansion is 500-2800W, Bulking Time is 3-600s.
Because of expanded graphite specific surface area lower time, peeling effect is poor, and in product, residual more crystalline flake graphite sheet, affects the result of use of slurry.As preferred embodiment, the specific surface area of described raw material after described expansion process is not less than 20m
2/ g.
In above-mentioned steps S02, the interpolation of water-based stripping liquid described in the embodiment of the present invention, can make described expanded graphite fully dissociate and disperse, thus effectively prevent the reunion of graphene sheet layer, and then improves dispersing property when it uses.In the embodiment of the present invention, suitable surface tension value, can ensure that described expanded graphite is in best stripping in environment, thus obtain good peeling effect, and then prevent the follow-up Graphene obtained from reuniting.As preferred embodiment, the surface tension of described water-based stripping liquid is 40-50mN/m.Further, in order to ensure the described effect infiltrating process, make described expanded graphite fully dissociate, disperse, the content of described expanded graphite and described water-based stripping liquid is than there being strict restriction.As preferred embodiment, described expanded graphite and described water-based stripping liquid content than being 1g:(50-1000) ml, specifically can be 1g:50ml, 1g:100ml, 1g:200ml, 1g:300ml, 1g:400ml, 1g:500ml, 1g:600ml, 1g:700ml, 1g:800ml, 1g:900ml, 1g:1000ml.
Described in the embodiment of the present invention, the solvent of water-based stripping liquid can select organic solvent or inorganic solvent, and described water-based stripping liquid can by one or more solvent compositions.As preferred embodiment, in described water-based stripping liquid, solvent is selected from least one in deionized water, ammoniacal liquor, formic acid, acetic acid, methyl alcohol, ethanol, glycerol, acetone, n-propyl alcohol, n-Octanol, isooctyl alcohol, methyl-sulphoxide, acetonitrile, dimethyl formamide, dioxane, tetrahydrofuran (THF) individually.
As concrete preferred embodiment, in order to make described water-based stripping liquid in above-mentioned surface tension range, described water-based stripping liquid optionally adds tensio-active agent.As concrete preferred embodiment, the tensio-active agent in described water-based stripping liquid be selected from Sodium dodecylbenzene sulfonate, polyvinylpyrrolidone, sodium lignosulfonate, Sodium cholic acid, stearic acid, tricresyl phosphate butyric acid, silane coupling agent, Tetrabutyl amonium bromide, Trisodium Citrate, cetyl trimethylammonium bromide, polyoxyethylene laurel ether, tween 80, triton X-100, dibutyltin oxide, Disperbyk-163, Methionin, poly-between sub-phenylethylene derivative, DsPE, DNA, at least one in polyvinyl alcohol.The consumption of described tensio-active agent is determined by the kind of described water-based stripping liquid solvent and consumption, preferably makes the surface tension of described stripping liquid in 40-50mN/m scope.
Infiltrate process described in the embodiment of the present invention and preferably can adopt the wetting realization of stirring, further, described expanded graphite stirs or soaks infiltrating time in described water-based stripping liquid is 0.5-4h.
In above-mentioned steps S03, under the condition that above-mentioned water-based stripping liquid infiltrates, particularly surface tension is under the condition of 40-50mN/m, adopt shear dissociate or ultrasonic dissociate auxiliary, dissociating fast of described expanded graphite, it is large that its single prepares output, can realize expanded graphite in 1 hour and dissociate fast, meet industrial production demand.
Concrete, in described high speed shear or ultrasonication, peel off power and splitting time is very big to graphene sheet layer size impact, superpower, to peel off for a long time, the water paste of small size, the thin Graphene of lamella can be obtained; On the contrary, the stripping of low power, short period of time, can obtain the water paste of big size graphene.In the embodiment of the present invention, in described high speed shear or ultrasonication, the rotating speed of described high speed shear is 2000-40000rpm, and shear time is 10-400min; Or described ultrasonic power is 50-3000W, ultrasonic treatment time is 10-600min.By adjusting stripping power and the splitting time of described high speed shear or ultrasonication, the Graphene wet feed that size is controlled can be obtained.
In the embodiment of the present invention, remove described water-based stripping liquid and obtain Graphene wet feed, one or more realizations of natural subsidence, centrifuging, air press filtration, vacuum filtration can be taked.
In above-mentioned steps S04, for obtaining Graphene water paste, need the dispersion treatment again in a solvent of Graphene filter cake wet feed in SO3, described solvent is at least one in deionized water or dehydrated alcohol, further, for obtaining high-stability graphene water paste, certain tensio-active agent can be added in solvent, concrete preferably Sodium dodecylbenzene sulfonate, polyvinylpyrrolidone, sodium lignosulfonate, Sodium cholic acid, stearic acid, tricresyl phosphate butyric acid, silane coupling agent, Tetrabutyl amonium bromide, Trisodium Citrate, cetyl trimethylammonium bromide, polyoxyethylene laurel ether, tween 80, triton X-100, dibutyltin oxide, Disperbyk-163, Methionin, sub-phenylethylene derivative between poly-, DsPE, DNA, at least one in polyvinyl alcohol.As preferred embodiment, the surface tension of described aqueous liquid dispersion is 40-50mN/m, is beneficial to the dispersion of grapheme material.
By described Graphene wet feed and aqueous liquid dispersion, carrying out high speed shear, ball milling, sand milling or ultrasonication further makes graphene microchip be uniformly dispersed, the rotating speed of described high speed shear, shear time, described ultrasonic power, ultrasonic treatment time all can refer to the optimum configurations of above-mentioned steps S03, the rotating speed of described ball milling is 100-1000rpm, and Ball-milling Time is 2-48h; The rotating speed of described sand milling is 500-5000rpm, and the sand milling time is 2-48h.
The preparation method of the Graphene water paste that the embodiment of the present invention provides, has the following advantages:
The first, the embodiment of the present invention is using graphite oxide or expansible black lead as raw material, and cheaper starting materials is easy to get, and the technique that the embodiment of the present invention prepares Graphene water paste simply, is easily controlled, and can realize the batch preparation of described Graphene water paste;
Second, after oxidation graphite solid or expansible black lead solid are carried out expansion process by the embodiment of the present invention, the expanded graphite of different expansion multiplying power can be obtained, described expanded graphite is placed in water-based stripping liquid that surface tension strictly controls fully wetting after, carry out high speed shear or ul-trasonic irradiation, the surface tension of described water-based stripping liquid makes the graphite flake layer of expansion obtain fully, dissociates efficiently and disperse, thus the heap sum that effectively prevent graphene sheet layer is reunited, improve dispersing property when Graphene uses.
3rd, the embodiment of the present invention water-based stripping liquid that uses surface tension to be 40-50mN/m, to dissociate or under the ultrasonic booster action dissociated, it is large that single prepares output, can realize expanded graphite in 1 hour and dissociate fast in shearing; The embodiment of the present invention uses the aqueous liquid dispersion that surface tension is 40-50mN/m, makes the stable performance of Graphene water paste, meets suitability for industrialized production and application demand.
4th, the preparation method of Graphene water paste described in the embodiment of the present invention, the size of described graphene sheet layer by feed change oxygen level, thus solves Graphene size problem rambunctious.
5th, described in the embodiment of the present invention, water-based stripping liquid is recyclable, and reuse after allotment, minimum to environmental hazard, described Graphene water paste is environment-friendly size.
Graphene water paste prepared by embodiment of the present invention method, can be applicable to the fields such as conductive and heat-conductive coating, protective system, battery/ultracapacitor.
Be described below in conjunction with specific embodiment.
Experimental example 1
A kind of Graphene water paste and preparation method thereof, comprises the following steps:
S11. get the expansible black lead that 14g particle diameter is 80 orders, oxygen level 10%, in 1000 DEG C of high-temperature expansion stoves, carry out expansion process, prepare 10g expanded graphite;
S12. described expanded graphite to be soaked in the deionized water volume percent being placed in 3L be 15% ammoniacal liquor and mass concentration is 4 × 10
-4stir moistening 1h in the mixing stripping liquid of the n-Octanol composition of kg/kg, obtain the mixture containing expanded graphite;
S13. the described mixture containing expanded graphite is carried out 800W ul-trasonic irradiation 4h, after centrifuging, obtain Graphene filter cake;
S14. described Graphene filter cake is scattered in 190g deionized water, add PVP reconciliation statement surface tension within the scope of 40-50mN/m, sand milling 6h in nanometer sand mill, obtain the Graphene water paste of weight percentage about 5%, wherein Graphene average platelet is of a size of 1 μm.
Experimental example 2
A kind of Graphene water paste and preparation method thereof, comprises the following steps:
S21. get the expansible black lead that 14g particle diameter is 150 orders, oxygen level 10%, in industrial microwave oven, carry out expansion process, prepare 10g expanded graphite;
S22. being soaked in by described expanded graphite and being placed in 1L volume percent be 15% ammoniacal liquor and mass concentration is 4 × 10
-4stir moistening 1h in the mixing stripping liquid of the n-Octanol composition of kg/kg, obtain the mixture containing expanded graphite;
S23. the described mixture containing expanded graphite is carried out 1000W ul-trasonic irradiation 3h, after vacuum filtration, obtain Graphene filter cake;
S24. described Graphene filter cake is scattered in 90g dehydrated alcohol, add Trisodium Citrate reconciliation statement surface tension within the scope of 40-50mN/m, shear dispersion treatment 3h, obtain the ethanol slurry of the Graphene of weight percentage about 10%, wherein Graphene average platelet is of a size of 15 μm.
Experimental example 3
A kind of Graphene water paste and preparation method thereof, comprises the following steps:
S31. get the expansible black lead that 15g particle diameter is 80 orders, oxygen level 5%, in 1000 DEG C of high-temperature expansion stoves, carry out expansion process, prepare 10g expanded graphite;
S32. being soaked in by described expanded graphite and being placed in 2L volume percent be 12% ammoniacal liquor and mass concentration is 3 × 10
-4stir moistening 0.5h in the mixing stripping liquid of the isooctyl alcohol composition of kg/kg, obtain the mixture containing expanded graphite;
S33. the described mixture containing expanded graphite is carried out 2800W ul-trasonic irradiation 1h, after air press filtration, obtain Graphene filter cake;
S34. described Graphene filter cake is scattered in 990g deionized water, add silane coupling agent reconciliation statement surface tension within the scope of 40-50mN/m, ultrasonic disperse process 2h, obtain the Graphene water paste of weight percentage about 1%, wherein Graphene average platelet is of a size of 20 μm.
In Graphene water paste prepared by the embodiment of the present invention, as shown in Figure 1, its infrared spectrogram as shown in Figure 2 for the scanning electron microscope (SEM) photograph of Graphene.
Experimental example 4
A kind of Graphene water paste and preparation method thereof, comprises the following steps:
S41. get the expansible black lead that 15g particle diameter is 150 orders, oxygen level 15%, in industrial microwave oven, carry out expansion process, prepare 10g expanded graphite;
S42. being soaked in by described expanded graphite and being placed in 4L volume percent be 12% ammoniacal liquor and mass concentration is 3 × 10
-4stir moistening 0.5h in the mixing stripping liquid of the isooctyl alcohol composition of kg/kg, obtain the mixture containing expanded graphite;
S43. the described mixture containing expanded graphite is carried out high speed shear effect 2h, after vacuum filtration, obtain Graphene filter cake;
S44. described Graphene filter cake is scattered in 90g dehydrated alcohol, add stearic acid reconciliation statement surface tension within the scope of 40-50mN/m, carry out high speed ball milling 4h, obtain the Graphene ethanol slurry of weight percentage about 10%, wherein Graphene average platelet is of a size of 3 μm.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a Graphene water paste, is characterized in that, described Graphene water paste comprises aqueous liquid dispersion and is dispersed in the grapheme material in described aqueous liquid dispersion, wherein, containing tensio-active agent in described aqueous liquid dispersion.
2. Graphene water paste as claimed in claim 1, it is characterized in that, in the total mass of described Graphene water paste for 100%, the mass percentage of described Graphene is 0.1-10%.
3. Graphene water paste as claimed in claim 1, it is characterized in that, the surface tension of described aqueous liquid dispersion is 40-50mN/m.
4. a preparation method for Graphene water paste as described in as arbitrary in claims 1-3, comprises the following steps:
With oxidation graphite solid or expansible black lead solid for raw material, carry out expansion process, prepare expanded graphite;
Described expanded graphite is soaked in water-based stripping liquid and infiltrates process, obtain the mixture containing expanded graphite;
The described mixture containing expanded graphite is carried out high speed shear or ultrasonication, removes described water-based stripping liquid, obtain Graphene wet feed;
Described Graphene wet feed is placed in aqueous liquid dispersion, carries out high speed shear process, obtain Graphene water paste.
5. the preparation method of Graphene water paste as claimed in claim 4, is characterized in that, containing tensio-active agent in described water-based stripping liquid and/or described aqueous liquid dispersion.
6. the preparation method of Graphene water paste as claimed in claim 5, it is characterized in that, the surface tension of described water-based stripping liquid and/or described aqueous liquid dispersion is 40-50mN/m.
7. the preparation method of Graphene water paste as claimed in claim 5, it is characterized in that, described tensio-active agent be Sodium dodecylbenzene sulfonate, polyvinylpyrrolidone, sodium lignosulfonate, Sodium cholic acid, stearic acid, tricresyl phosphate butyric acid, silane coupling agent, Tetrabutyl amonium bromide, Trisodium Citrate, cetyl trimethylammonium bromide, polyoxyethylene laurel ether, tween 80, triton X-100, dibutyltin oxide, Disperbyk-163, Methionin, poly-between sub-phenylethylene derivative, DsPE, at least one in polyvinyl alcohol.
8. the preparation method of Graphene water paste as claimed in claim 4, is characterized in that, described expanded graphite through high speed shear or ultrasonication, wherein,
The rotating speed of described high speed shear is 2000-40000rpm, and shear time is 10-400min; Or
Described ultrasonic power is 50-3000W, and ultrasonic treatment time is 30-600min.
9. the preparation method of Graphene water paste as described in as arbitrary in claim 4 or 8, it is characterized in that, described Graphene wet feed is being placed in after aqueous liquid dispersion carries out high speed shear process, also comprise ball milling, sand milling or ultrasonication, wherein, the rotating speed of described ball-milling processing is 100-1000rpm, and Ball-milling Time is 2-48h; And/or the rotating speed of described sanded is 500-5000rpm, the sand milling time is 2-48h.
10. the preparation method of Graphene water paste as claimed in claim 4, is characterized in that, the content of described expanded graphite and described water-based stripping liquid is than being 1g:(50-5000) ml.
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