CN102583335A - Preparation method of graphene uniform dispersion - Google Patents
Preparation method of graphene uniform dispersion Download PDFInfo
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Abstract
The invention relates to a preparation method of graphene uniform dispersion, belonging to the technical field of new nano materials. The preparation method comprises the following steps of: (1) preparing aqueous surfactant solution with the concentration of 0.2-20g/L; (2) mixing raw graphite powder with the aqueous surfactant solution according to the concentration of 1-100g/L, forming suspension and adding the suspension into a high-pressure reactor with strirring; (3) adjusting the rotating speed of the high-pressure reactor to be 50-300rpm and the temperature in the reactor to be 100-300 DEG C, carrying out heat preservation treatment on the raw graphite powder for 5-24 hours and then taking out paste; (4) carrying out 1000-2000rpm centrifugation on the paste for 15-45 minutes, and obtaining supernatant solution which is the dispersion with one-layer and multilayer graphene. The preparation method has the advantages that the aqueous surfactant solution used in the preparation process can be recycled without exhaust emission; the used materials are non-corrosive, non-toxic, non-flammable and non-explosive products; the process can not cause large damage to the protogenic conjugated structure of the graphene; and the low cost can be realized, and the graphene dispersion with excellent dispersity and stability can be prepared.
Description
Technical field
What the present invention relates to is the nanometer new material technology field, specifically is a kind of preparation method of Graphene homodisperse liquid.
Background technology
Since coming to light from Graphene in 2004, just enjoyed generally favor from physics and field of materials investigator always.Graphene is a kind of by the tightly packed bi-dimensional cellular shape crystalline network blacking that forms of monolayer carbon atom.Although Graphene has only a carbon atomic layer thickness, and be the thinnest a kind of in the known materials, however unusual rigid.Graphene also is the outstanding material of present known conductive property simultaneously.In addition, Graphene also has the performance of many excellences, like high heat conductance, huge specific surface area or the like.Because the property of Graphene, it has wide practical use at aspects such as electronics, optics, magnetics, biomedicine, transmitter, energy storage.In order Graphene to be applied in above-mentioned field, the problem that at first will solve is can prepare high-quality Graphene and realize scale operation.
The preparation method of grapheme material mainly contains micromechanics and peels off method (adhesive tape method), oxidation-reduction method, chemical Vapor deposition process (CVD) etc.; Wherein the adhesive tape method is owing to can obtain purity and the Graphene of structural integrity the best; In fundamental researchs such as microstructure and conduction, heat conductivility, be used widely, but this method productive rate is extremely low.Oxidation-reduction method can be produced grapheme material in batches; Though this grapheme material surface oxy radical (like hydroxyl, epoxy group(ing), carboxyl and carbonyl etc.) can't thoroughly be eliminated; Influence its conductivity, but be suitable for preparing lightweight, high-intensity polymer composites.Because oxidation stage uses strong oxidizers such as oleum, nitric acid, potassium permanganate; Reduction phase has used poisonous, inflammable and explosive strong reductants such as Hydrazine Hydrate 80, sodium Metal 99.5 and potassium, Resorcinol, Peng Qinghuana; This method will run into serious wastewater treatment, problem such as fire-proof and explosion-proof in the scale prodn process, complex procedures and cost of material height also will make production cost face the challenge simultaneously.The CVD method can be than the preparation individual layer or the low number of plies grapheme material of big area (centimeter scale); At the device manufacturing method mask very big application potential is arranged; But the graphene film size still is limited by the size of transition metal substrate (Cu, Ni, Ru etc.); And the film shifting process is complicated, and the stability that how to keep product performance will be the key that devices in batches is made.Consider from industrial feasibility, but the working method of grapheme material need possess characteristics such as low cost, pollution-free, the simple continuous batch production of technology.
Summary of the invention
The objective of the invention is to overcome the problem that exists in the prior art, a kind of simple to operate, with low cost, method of being easy to prepare in a large number Graphene is provided.
The present invention with the graphite raw material powder under high temperature and high pressure environment in water phase surfactant mixture hot soarfing from the preparation Graphene.
Step of the present invention is:
(1) prepares water phase surfactant mixture according to the concentration of 0.2～20g/L;
(2) the graphite raw material powder is mixed by 1～100g/L concentration with water phase surfactant mixture, form suspension-s, and add the autoclave that has whipping appts;
(3) conditioned reaction still mixing speed is 50～300rpm, regulates 100～300 ℃ of temperature in the kettle, and psia corresponding in the reaction kettle is 0.1～8.6MPa, and insulation is handled after 5～24 hours and taken out slurry to the graphite raw material powder under high temperature and high pressure environment;
(4) slurry being carried out high speed centrifugation separates; Centrifugal rotational speed is 1000～2000rpm; Centrifugal 15～45min makes unstripped graphite granule or the many Graphenes of the number of plies precipitate through centrifugal action, and upper solution promptly is the mixed dispersion liquid of individual layer and number layer graphene.
Graphite raw material powder of the present invention is artificial synthetic graphite powder, natural graphite powder, high temperature pyrolysis Graphite Powder 99 or expansible black lead powder.
Tensio-active agent of the present invention is polyethers P-123, Tween-80, polyoxyethylene octyl phenyl ether X-100.Vinylpyrrolidone polymer, Tween-85, X 2073, sodium lauryl sulphate, nonionic and ASs such as Sodium desoxycholate.
The autoclave that the described preparation facilities of wood invention stirs for band.
Advantage of the present invention is: 1, the prices of raw and semifnished materials are cheap; The tensio-active agent reusable edible can be realized low cost, scale prodn continuous, in enormous quantities; 2, there are not waste water, exhaust gas emission in the production process, starting material non-corrosiveness, murder by poisoning or the inflammable explosive article of use; 3, do not use strong oxidizer, the graphene conductive conjugated structure is not produced considerable damage, can be used for preparing the functional materials of high conduction performance; 4, the Graphene dispersion liquid of preparation is peeled off well dispersiveness and excellent in stability.
Description of drawings
Fig. 1 is the Graphite Powder 99 XRD figure;
Fig. 2 is the XRD figure of the Graphene of preparation in the instance 1;
Fig. 3 is the TEM photo of the Graphene of preparation in the instance 1;
Fig. 4 is the TEM photo of the Graphite Powder 99 do not peeled away fully in the Comparative Examples 1.
The schema that Fig. 5 implements for this patent
Embodiment
Get 1g expansible black lead powder; Add in the Tween-80 aqueous solution of 1000mL 0.2g/L, autoclave is warming up to 200 ℃, keep mixing speed 200rpm to carry out the hydro-thermal insulation and handled 6 hours; Slurries 1000rpm spinning 20min obtains upper solution and is the Graphene dispersion liquid then.Leave standstill 2 hours no sedimentation phenomenon under this dispersion liquid room temperature, show to have good stability.002 and 004 peak is the greying characteristic peak among Fig. 1,2, and the relative graphite of 002 and 004 peak intensity of Graphene reduces a lot of explanation graphite and effectively peeled off number of plies reduction; The little surperficial conjugated structure of 001 characteristic peak explanation degree of oxidation that graphite oxide does not appear in 10.6 ° of positions in the XRD figure of Graphene destroys few.
Embodiment 2
Get 10g high temperature pyrolysis Graphite Powder 99; Add in the sodium dodecyl benzene sulfonate aqueous solution of 1000mL 2g/L, autoclave is warming up to 160 ℃, keep mixing speed 180rpm to carry out the hydro-thermal insulation and handled 10 hours; Slurries 1500rpm spinning 40min then; Obtain upper solution and be the Graphene dispersion liquid, leave standstill 2 hours no sedimentation phenomenon under this dispersion liquid room temperature, show to have good stability.The products obtained therefrom XRD figure is similar with embodiment 1, and 002 and 004 peak intensity of Graphene compares the graphite reduction a lot, and 001 characteristic peak of graphite oxide does not appear in 10.6 ° of positions.
Embodiment 3
Get 100g expansible black lead powder; Add in the polyethers P-123 aqueous solution of 1000mL 20g/L, autoclave is warming up to 180 ℃, keep mixing speed 160rpm to carry out hydrothermal treatment consists 16 hours; Slurries 2000rpm spinning 30min then; Obtain upper solution and be the Graphene dispersion liquid, leave standstill 2 hours no sedimentation phenomenon under the room temperature, show that dispersion stability is good.The products obtained therefrom XRD figure is similar with embodiment 1, and 002 and 004 peak intensity of Graphene compares the graphite reduction a lot, and 001 characteristic peak of graphite oxide does not appear in 10.6 ° of positions.
Comparative Examples 1
Get 10g high temperature pyrolysis Graphite Powder 99, add in the 1000mL water, closed reactor is warming up to 160 ℃, keep mixing speed 180rpm to carry out hydrothermal treatment consists 10 hours, then slurries 1500rpm spinning 40min.It is obvious to leave standstill sedimentation in 2 hours under this dispersion liquid room temperature.
Comparative Examples 2
Get 1g expansible black lead powder, add in the Tween-80 aqueous solution of 1000mL 0.2g/L, at room temperature keep mixing speed 200rpm to handle 6 hours, then slurries 1000rpm spinning 20min.It is obvious to leave standstill sedimentation in 2 hours under this dispersion liquid room temperature.
Comparative Examples 3
Get 10g high temperature pyrolysis Graphite Powder 99; Add in the tetrabutyl ammonium fluoride aqueous solution of 1000mL 2g/L; Autoclave is warming up to 160 ℃; Keep mixing speed 180rpm to carry out the hydro-thermal insulation and handled 10 hours, slurries 1500rpm spinning 40min then, it is obvious to leave standstill sedimentation in 2 hours under this dispersion liquid room temperature.
With above-mentioned foundation desirable embodiment of the present invention is enlightenment, and through above-mentioned description, the related work personnel can carry out various change and modification fully in the scope that does not depart from this invention technological thought.The technical scope of this invention is not limited to the content on the specification sheets, must confirm its technical scope according to the claim scope.
Claims (4)
1. the preparation method of a Graphene homodisperse liquid the steps include:
(1) preparation water phase surfactant mixture, concentration is 0.2～20g/L;
(2) the graphite raw material powder is mixed by 1～100g/L concentration with water phase surfactant mixture, form suspension-s, and add the autoclave of band whipping appts;
(3) conditioned reaction still rotating speed is 50～300rpm, and regulating temperature in the kettle is 100～300 ℃, and psia corresponding in the reaction kettle is 0.1～8.6MPa.Insulation is handled after 5～24 hours and is taken out slurry to the graphite raw material powder under high temperature and high pressure environment;
(4) slurry being carried out high speed centrifugation separates; Centrifugal rotational speed is 1000～2000rpm; Centrifugation time 15～45min makes unstripped graphite granule or the many Graphenes of the number of plies precipitate through centrifugal action, and upper solution promptly is the dispersion liquid of individual layer and number layer graphene.
2. the preparation method of a kind of Graphene homodisperse liquid according to claim 1 is characterized in that described graphite raw material powder is artificial synthetic graphite powder, natural graphite powder, high temperature pyrolysis Graphite Powder 99 or expansible black lead powder.
3. the preparation method of homodisperse liquid according to claim 1 is characterized in that tensio-active agent is nonionic and AS.
4. the preparation method of homodisperse liquid according to claim 1 is characterized in that tensio-active agent is polyethers P-123, Tween-80; Polyoxyethylene octyl phenyl ether X-100, Vinylpyrrolidone polymer, Tween-85; X 2073, sodium lauryl sulphate, Sodium desoxycholate.
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| CN102992312A (en) * | 2012-12-12 | 2013-03-27 | 哈尔滨工业大学 | Preparation method of graphene monomer complex |
| CN103254455A (en) * | 2013-04-23 | 2013-08-21 | 中国科学院上海光学精密机械研究所 | Preparation method of graphene-thickening polymer composite film |
| CN103466608A (en) * | 2013-09-11 | 2013-12-25 | 中南大学 | Ball milling preparation method of graphene |
| CN103771402A (en) * | 2013-12-30 | 2014-05-07 | 华南农业大学 | Graphene preparation method |
| CN104505513A (en) * | 2014-09-15 | 2015-04-08 | 宁波维科电池股份有限公司 | Lithium ion battery graphene conductive agent and preparation method thereof |
| CN105110318A (en) * | 2015-07-23 | 2015-12-02 | 深圳市国创新能源研究院 | Graphene aqueous slurry, and preparation method thereof |
| CN105253862A (en) * | 2014-07-15 | 2016-01-20 | 中国科学院过程工程研究所 | Method for large-scale preparation of graphene-like boron nitride nano-sheets through high temperature liquid-phase peeling |
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Address after: 215500 5th floor, building 4, 68 Lianfeng Road, Changfu street, Changshu City, Suzhou City, Jiangsu Province Patentee after: Changshu intellectual property operation center Co.,Ltd. Address before: No.13 caodang Road, Changshu City, Suzhou City, Jiangsu Province Patentee before: Changshu intellectual property operation center Co.,Ltd. |
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