CN108726513A - A kind of preparation method of graphene dispersing solution - Google Patents
A kind of preparation method of graphene dispersing solution Download PDFInfo
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Abstract
The present invention relates to dispersion liquid technical fields, and in particular to a kind of preparation method of graphene dispersing solution includes the following steps:A, natural flake graphite is taken, graphene oxide suspension is prepared using chemistry redox method, graphene powder is obtained after carrying out ultrasound, washing, reduction and drying process;B, it takes solvent and graphene powder to be stirred to uniform, then carries out ultrasonic cleaning processing, then carry out homogenized;C, dispersant and surfactant is added, is stirred to uniform, then carries out ultrasonic cleaning processing, subsequent centrifugal treating removes bulky grain graphene particles, takes supernatant, as graphene dispersing solution.The graphene dispersing solution that the preparation method of the present invention is prepared not only has good dispersion performance and resistance to settling energy, and the chemical composition and physical pattern of graphene are not affected by destruction, therefore, the graphene dispersing solution of the application remains original performance of graphene, applicability is stronger, can be widely used for the fields such as lubrication, heat-conductive composite material.
Description
Technical field
The present invention relates to dispersion liquid technical fields, and in particular to a kind of preparation method of graphene dispersing solution.
Background technology
Graphene has shot up since 2004 are found as a nova of material supply section educational circles, although its
The time being found is also very short, but due to its perfect hexagonal crystal structure and this special construction assign it is many super excellent
Different performance, such as up to the theoretical specific surface area of 2600m2/g, the thermal conductivity of 3000W/ (m.k), the tensile strength of 1060Gpa,
The quantum hall effect etc. of perfect quantum tunneling effect and half-integer, makes it have numerous potential applications in real life
Field.The preparation method of graphene has oxidation-reduction method, mechanical stripping method, SiC epitaxial growths, chemical vapour deposition technique(CVD),
Liquid phase stripping method synthesizes from bottom to top.The graphene of redox and physics stripping is mutual due to π-π strong between lamella
Effect, makes its lamella that agglomeration easily occur, and it is limited to eventually lead to its solubility in organic solvent or water, this is just very big
Graphene applications in various fields is limited in degree.
Kinds of schemes is proposed to this researcher, to solve these problems.A kind of wherein common mode is to pass through
Chemical modification processing is carried out to graphene, to promote its dispersion performance, but this mode can lead to the chemistry of grapheme material
Composition and physical pattern etc. change.
Therefore, graphene high-efficiency how is realized on the basis of not destroying graphene uniqueness physicochemical property, is stably dispersed in
It is always industry problem urgently to be resolved hurrily in decentralized medium.
Invention content
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide a kind of graphene dispersions
The preparation method of liquid, the method overcome in the prior art to improve the chemical group that the dispersion performance of graphene destroys graphene
At the defect with physical pattern, the graphene dispersing solution that preparation method of the invention is prepared not only has good dispersibility
Energy and resistance to settling energy, and the chemical composition of graphene and physical pattern do not receive destruction, therefore, the graphene point of the application
The original performance for remaining graphene of dispersion liquid, applicability is stronger, can be widely used for the fields such as lubrication, heat-conductive composite material.
The purpose of the invention is achieved by the following technical solution:A kind of preparation method of graphene dispersing solution, including it is following
Step:A, the preparation of graphene powder:Natural flake graphite is taken, preparing graphene oxide using chemistry redox method suspends
Liquid obtains graphene powder after carrying out ultrasound, washing, reduction and drying process to graphene oxide suspension;B, major ingredient mixes:
It takes solvent and graphene powder to be stirred to uniform, ultrasonic cleaning processing then is carried out to mixed liquor, is then carried out at homogenate
Reason;C, prepared by dispersion liquid:It takes dispersant and surfactant to be added in the mixed liquor obtained in step B, is stirred to uniform,
Then ultrasonic cleaning processing is carried out to it, then carries out centrifugal treating, removed bulky grain graphene particles, take supernatant, i.e.,
For graphene dispersing solution.
The chemistry redox method of use includes using preparations such as Hummers methods, Staudenmaier methods and Brodie methods
Graphene oxide, and use reducing agent(Hydrazine and its derivative, sodium borohydride, green reducing agent etc.)Reduction, soda acid reduction, solvent
Thermal reduction etc. prepares graphene, and improved method on the basis of such method.
Ultrasound, washing, reduction and drying process in the step A are specially:Graphene oxide suspension is surpassed
Then sonication, ultrasonic time 2.5-3.5h use deionized water to carry out repeatedly washing into graphene oxide suspension
Property, then graphene oxide suspension is diluted to 1mg/ml, it is ultrasonically treated 2.5-3.5h again, uses at hydrazine hydrate reduction later
The graphene oxide in graphene oxide suspension is managed, deionized water is reused and repeatedly wash to neutrality, finally freeze
Drying process obtains graphene powder.
The usage amount of solvent in the step B is 100 parts by weight, and the usage amount of graphene powder is 0.5-1 parts by weight.
The equipment for being cleaned by ultrasonic processing in the step B is supersonic wave cleaning machine, and the equipment of time 2h, homogenized are
Refiner, Homogenization time 40-50min, refiner rotating speed are 16000-28000rpm.
The dosage of dispersant in the step C is 0.2-0.3 parts by weight, and the dosage of surfactant is 0.2-0.3 weights
Measure part.
Mixing time in the step C is 25-35min, and whipping temp is 70-80 DEG C, is cleaned by ultrasonic what processing used
Equipment is supersonic wave cleaning machine, ultrasonic time 25-35min, and the rotating speed of centrifuge is 1000-5000rpm when centrifugal treating.
The solvent is one or more kinds of mixtures in NMP, DMF, PMA, gamma-butyrolacton, EA.
Preferably, the solvent is NMP or DMF.
More preferably, further include secondary solvent n-butanol.When two kinds of solvents of selection are immiscible, positive fourth can be selected
Alcohol dissolves each other as secondary solvent auxiliary.
The dispersant is one or more kinds of mixtures in PVP, SDBS, PVA, CMC.
The surfactant is to be mixed by Tween 80, sorbester p17, oleic acid.
The average grain diameter of graphene particles in the graphene dispersing solution is 1.06 um-2.6 um, the graphite flakes
Mesh number be 500 mesh, 5000 mesh, 10000 mesh or 12000 mesh.
Preferably, the average grain diameter of the graphene particles in the graphene dispersing solution is 1.3 um, the graphite flakes
Mesh number be 500 mesh or 10000 mesh.
The beneficial effects of the present invention are:The present invention removes graphene sheet layer by being homogenized and being ultrasonically treated preliminary refinement,
Then dispersant is used(Macromolecule dispersing agent)Dispersion degree of the graphene in related solvents is further increased with surfactant,
Finally centrifugation removal graphene particles inferior, obtain having certain density graphene dispersing solution, overcome and are in the prior art
It improves the dispersion performance of graphene and destroys the chemical composition of graphene and the defect of physical pattern, preparation method system of the invention
Standby obtained graphene dispersing solution not only has good dispersion performance and resistance to settling energy, and the chemical composition and object of graphene
Reason pattern does not receive destruction, good stability, therefore, the original property for remaining graphene of the graphene dispersing solution of the application
Can, applicability is stronger, can be widely used for the fields such as lubrication, heat-conductive composite material.
Specific implementation mode
For the ease of the understanding of those skilled in the art, with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying refers to not is limitation of the invention.
Embodiment 1
A kind of preparation method of graphene dispersing solution, includes the following steps:A, the preparation of graphene powder:Graphite flakes are taken, are adopted
Graphene oxide suspension is prepared with Hummers methods, ultrasound, washing, reduction and drying are carried out to graphene oxide suspension
Graphene powder is obtained after processing;B, major ingredient mixes:Solvent and graphene powder is taken to be stirred to uniform, then to mixed liquor
Ultrasonic cleaning processing is carried out, homogenized is then carried out;C, prepared by dispersion liquid:Take dispersant and surfactant that step B is added
In in obtained mixed liquor, be stirred to uniform, ultrasonic cleaning processing then carried out to it, centrifugal treating is then carried out, goes
Except bulky grain graphene particles, supernatant, as graphene dispersing solution are taken.
Ultrasound, washing, reduction and drying process in the step A are specially:Graphene oxide suspension is surpassed
Then sonication, ultrasonic time 2.5h use deionized water to carry out repeatedly washing to neutrality to graphene oxide suspension, then
Graphene oxide suspension is diluted to 1mg/ml, is ultrasonically treated 2.5h again, uses hydrazine hydrate reduction processing oxidation stone later
Graphene oxide in black alkene suspension reuses deionized water and carries out repeatedly washing to neutrality, last freeze-drying process
Obtain graphene powder.
The usage amount of solvent in the step B is 100 parts by weight, and the usage amount of graphene powder is 0.5 parts by weight.
The equipment for being cleaned by ultrasonic processing in the step B is supersonic wave cleaning machine, and the equipment of time 2h, homogenized are
Refiner, Homogenization time 40min, refiner rotating speed are 16000rpm.
The dosage of dispersant in the step C is 0.2 parts by weight, and the dosage of surfactant is 0.2 parts by weight.
Mixing time in the step C is 25min, and whipping temp is 70 DEG C, be cleaned by ultrasonic the equipment that processing uses for
Supersonic wave cleaning machine, ultrasonic time 25-35min, the rotating speed of centrifuge is 1000-5000rpm when centrifugal treating.
The solvent is NMP.
The dispersant is PVP.
The surfactant is to be mixed by Tween 80, sorbester p17, oleic acid.
The average grain diameter of graphene particles in the graphene dispersing solution is 1.06 um, the mesh number of the graphite flakes
For 500 mesh.
Embodiment 2
A kind of preparation method of graphene dispersing solution, includes the following steps:A, the preparation of graphene powder:Graphite flakes are taken, are adopted
Graphene oxide suspension is prepared with Hummers methods, ultrasound, washing, reduction and drying are carried out to graphene oxide suspension
Graphene powder is obtained after processing;B, major ingredient mixes:Solvent and graphene powder is taken to be stirred to uniform, then to mixed liquor
Ultrasonic cleaning processing is carried out, homogenized is then carried out;C, prepared by dispersion liquid:Take dispersant and surfactant that step B is added
In in obtained mixed liquor, be stirred to uniform, ultrasonic cleaning processing then carried out to it, centrifugal treating is then carried out, goes
Except bulky grain graphene particles, supernatant, as graphene dispersing solution are taken.
Ultrasound, washing, reduction and drying process in the step A are specially:Graphene oxide suspension is surpassed
Then sonication, ultrasonic time 2.8h use deionized water to carry out repeatedly washing to neutrality to graphene oxide suspension, then
Graphene oxide suspension is diluted to 1mg/ml, is ultrasonically treated 2.8h again, uses hydrazine hydrate reduction processing oxidation stone later
Graphene oxide in black alkene suspension reuses deionized water and carries out repeatedly washing to neutrality, last freeze-drying process
Obtain graphene powder.
The usage amount of solvent in the step B is 100 parts by weight, and the usage amount of graphene powder is 0.6 parts by weight.
The equipment for being cleaned by ultrasonic processing in the step B is supersonic wave cleaning machine, and the equipment of time 2h, homogenized are
Refiner, Homogenization time 42min, refiner rotating speed are 18000rpm.
The dosage of dispersant in the step C is 0.22 parts by weight, and the dosage of surfactant is 0.22 parts by weight.
Mixing time in the step C is 28min, and whipping temp is 72 DEG C, be cleaned by ultrasonic the equipment that processing uses for
Supersonic wave cleaning machine, ultrasonic time 28min, the rotating speed of centrifuge is 2000rpm when centrifugal treating.
The solvent is DMF.
The dispersant is SDBS.
The surfactant is to be mixed by Tween 80, sorbester p17, oleic acid.
The average grain diameter of graphene particles in the graphene dispersing solution is 1.5 um, and the mesh number of the graphite flakes is
5000 mesh.
Embodiment 3
A kind of preparation method of graphene dispersing solution, includes the following steps:A, the preparation of graphene powder:Graphite flakes are taken, are adopted
Graphene oxide suspension is prepared with Hummers methods, ultrasound, washing, reduction and drying are carried out to graphene oxide suspension
Graphene powder is obtained after processing;B, major ingredient mixes:Solvent and graphene powder is taken to be stirred to uniform, then to mixed liquor
Ultrasonic cleaning processing is carried out, homogenized is then carried out;C, prepared by dispersion liquid:Take dispersant and surfactant that step B is added
In in obtained mixed liquor, be stirred to uniform, ultrasonic cleaning processing then carried out to it, centrifugal treating is then carried out, goes
Except bulky grain graphene particles, supernatant, as graphene dispersing solution are taken.
Ultrasound, washing, reduction and drying process in the step A are specially:Graphene oxide suspension is surpassed
Then sonication, ultrasonic time 3h use deionized water to carry out repeatedly washing to neutrality to graphene oxide suspension, then will
Graphene oxide suspension is diluted to 1mg/ml, is ultrasonically treated 3h again, uses hydrazine hydrate reduction to handle graphene oxide later
Graphene oxide in suspension reuses deionized water and repeatedly wash to neutrality, and last freeze-drying process obtains
Graphene powder.
The usage amount of solvent in the step B is 100 parts by weight, and the usage amount of graphene powder is 0.7 parts by weight.
The equipment for being cleaned by ultrasonic processing in the step B is supersonic wave cleaning machine, and the equipment of time 2h, homogenized are
Refiner, Homogenization time 45min, refiner rotating speed are 20000rpm.
The dosage of dispersant in the step C is 0.25 parts by weight, and the dosage of surfactant is 0.25 parts by weight.
Mixing time in the step C is 30min, and whipping temp is 75 DEG C, be cleaned by ultrasonic the equipment that processing uses for
Supersonic wave cleaning machine, ultrasonic time 30min, the rotating speed of centrifuge is 3000rpm when centrifugal treating.
The solvent is the mixture that PMA and gamma-butyrolacton form.
The dispersant is PVA.
The surfactant is to be mixed by Tween 80, sorbester p17, oleic acid.
The average grain diameter of graphene particles in the graphene dispersing solution is 1.8 um, and the mesh number of the graphite flakes is
10000 mesh.
Embodiment 4
A kind of preparation method of graphene dispersing solution, includes the following steps:A, the preparation of graphene powder:Graphite flakes are taken, are adopted
Graphene oxide suspension is prepared with Hummers methods, ultrasound, washing, reduction and drying are carried out to graphene oxide suspension
Graphene powder is obtained after processing;B, major ingredient mixes:Solvent and graphene powder is taken to be stirred to uniform, then to mixed liquor
Ultrasonic cleaning processing is carried out, homogenized is then carried out;C, prepared by dispersion liquid:Take dispersant and surfactant that step B is added
In in obtained mixed liquor, be stirred to uniform, ultrasonic cleaning processing then carried out to it, centrifugal treating is then carried out, goes
Except bulky grain graphene particles, supernatant, as graphene dispersing solution are taken.
Ultrasound, washing, reduction and drying process in the step A are specially:Graphene oxide suspension is surpassed
Then sonication, ultrasonic time 3.2h use deionized water to carry out repeatedly washing to neutrality to graphene oxide suspension, then
Graphene oxide suspension is diluted to 1mg/ml, is ultrasonically treated 3.2h again, uses hydrazine hydrate reduction processing oxidation stone later
Graphene oxide in black alkene suspension reuses deionized water and carries out repeatedly washing to neutrality, last freeze-drying process
Obtain graphene powder.
The usage amount of solvent in the step B is 100 parts by weight, and the usage amount of graphene powder is 0.8 parts by weight.
The equipment for being cleaned by ultrasonic processing in the step B is supersonic wave cleaning machine, and the equipment of time 2h, homogenized are
Refiner, Homogenization time 48min, refiner rotating speed are 25000rpm.
The dosage of dispersant in the step C is 0.28 parts by weight, and the dosage of surfactant is 0.28 parts by weight.
Mixing time in the step C is 32min, and whipping temp is 78 DEG C, be cleaned by ultrasonic the equipment that processing uses for
Supersonic wave cleaning machine, ultrasonic time 32min, the rotating speed of centrifuge is 4000rpm when centrifugal treating.
The solvent is the mixture formed in gamma-butyrolacton and EA.
It further include secondary solvent n-butanol.
The dispersant is the mixture formed in PVA and CMC.
The surfactant is to be mixed by Tween 80, sorbester p17, oleic acid.
The average grain diameter of graphene particles in the graphene dispersing solution is 2.2 um, and the mesh number of the graphite flakes is
12000 mesh.
Embodiment 5
A kind of preparation method of graphene dispersing solution, includes the following steps:A, the preparation of graphene powder:Graphite flakes are taken, are adopted
Graphene oxide suspension is prepared with Hummers methods, ultrasound, washing, reduction and drying are carried out to graphene oxide suspension
Graphene powder is obtained after processing;B, major ingredient mixes:Solvent and graphene powder is taken to be stirred to uniform, then to mixed liquor
Ultrasonic cleaning processing is carried out, homogenized is then carried out;C, prepared by dispersion liquid:Take dispersant and surfactant that step B is added
In in obtained mixed liquor, be stirred to uniform, ultrasonic cleaning processing then carried out to it, centrifugal treating is then carried out, goes
Except bulky grain graphene particles, supernatant, as graphene dispersing solution are taken.
Ultrasound, washing, reduction and drying process in the step A are specially:Graphene oxide suspension is surpassed
Then sonication, ultrasonic time 3.5h use deionized water to carry out repeatedly washing to neutrality to graphene oxide suspension, then
Graphene oxide suspension is diluted to 1mg/ml, is ultrasonically treated 3.5h again, uses hydrazine hydrate reduction processing oxidation stone later
Graphene oxide in black alkene suspension reuses deionized water and carries out repeatedly washing to neutrality, last freeze-drying process
Obtain graphene powder.
The usage amount of solvent in the step B is 100 parts by weight, and the usage amount of graphene powder is 1 parts by weight.
The equipment for being cleaned by ultrasonic processing in the step B is supersonic wave cleaning machine, and the equipment of time 2h, homogenized are
Refiner, Homogenization time 50min, refiner rotating speed are 28000rpm.
The dosage of dispersant in the step C is 0.3 parts by weight, and the dosage of surfactant is 0.3 parts by weight.
Mixing time in the step C is 35min, and whipping temp is 80 DEG C, be cleaned by ultrasonic the equipment that processing uses for
Supersonic wave cleaning machine, ultrasonic time 35min, the rotating speed of centrifuge is 5000rpm when centrifugal treating.
The solvent is the mixture of NMP, DMF and PMA composition.
It further include secondary solvent n-butanol.
The dispersant is the mixture of PVP, SDBS and PVA composition.
The surfactant is to be mixed by Tween 80, sorbester p17, oleic acid.
The average grain diameter of graphene particles in the graphene dispersing solution is 2.6 um, and the mesh number of the graphite flakes is
12000 mesh.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other manner,
Any obvious replacement is not departed under the premise of present inventive concept within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of graphene dispersing solution, it is characterised in that:Include the following steps:A, the preparation of graphene powder:
Graphite flakes are taken, graphene oxide suspension is prepared using chemistry redox method, graphene oxide suspension is surpassed
Graphene powder is obtained after sound, washing, reduction and drying process;B, major ingredient mixes:Solvent is taken to be stirred with graphene powder
To uniform, ultrasonic cleaning processing then is carried out to mixed liquor, then carries out homogenized;C, prepared by dispersion liquid:Take dispersant and
Surfactant is added in the mixed liquor obtained in step B, is stirred to uniform, then carries out ultrasonic cleaning processing to it,
Centrifugal treating is then carried out, bulky grain graphene particles is removed, takes supernatant, as graphene dispersing solution.
2. a kind of preparation method of graphene dispersing solution according to claim 1, it is characterised in that:In the step A
Ultrasound, washing, reduction and drying process are specially:Graphene oxide suspension is ultrasonically treated, ultrasonic time 2.5-
Then 3.5h uses deionized water to carry out repeatedly washing to graphene oxide suspension and suspends to neutrality, then by graphene oxide
Liquid is diluted to 1mg/ml, is ultrasonically treated 2.5-3.5h again, uses later in hydrazine hydrate reduction processing graphene oxide suspension
Graphene oxide, reuse deionized water carry out repeatedly washing to neutrality, last freeze-drying process obtains Graphene powder
Body.
3. a kind of preparation method of graphene dispersing solution according to claim 1, it is characterised in that:In the step B
The usage amount of solvent is 100 parts by weight, and the usage amount of graphene powder is 0.5-1 parts by weight.
4. a kind of preparation method of graphene dispersing solution according to claim 1, it is characterised in that:Surpass in the step B
The equipment of sound cleaning treatment is supersonic wave cleaning machine, and the equipment of time 2h, homogenized are refiner, Homogenization time 40-
50min, refiner rotating speed are 16000-28000rpm.
5. a kind of preparation method of graphene dispersing solution according to claim 1, it is characterised in that:In the step C
The dosage of dispersant is 0.2-0.3 parts by weight, and the dosage of surfactant is 0.2-0.3 parts by weight.
6. a kind of preparation method of graphene dispersing solution according to claim 1, it is characterised in that:In the step C
Mixing time is 25-35min, and whipping temp is 70-80 DEG C, is cleaned by ultrasonic the equipment for handling and using for supersonic wave cleaning machine, surpasses
The sound time is 25-35min, and the rotating speed of centrifuge is 1000-5000rpm when centrifugal treating.
7. a kind of preparation method of graphene dispersing solution according to claim 1, it is characterised in that:The solvent be NMP,
One or more kinds of mixtures in DMF, PMA, gamma-butyrolacton, EA.
8. a kind of preparation method of graphene dispersing solution according to claim 1, it is characterised in that:The dispersant is
One or more kinds of mixtures in PVP, SDBS, PVA, CMC.
9. a kind of preparation method of graphene dispersing solution according to claim 1, it is characterised in that:The surfactant
To be mixed by Tween 80, sorbester p17, oleic acid.
10. a kind of preparation method of graphene dispersing solution according to claim 1, it is characterised in that:The graphene point
The average grain diameter of graphene particles in dispersion liquid is 1.06 um-2.6 um, and the mesh number of the graphite flakes is 500 mesh, 5000
Mesh, 10000 mesh or 12000 mesh.
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CN109817385A (en) * | 2018-12-28 | 2019-05-28 | 常州碳森石墨烯科技有限公司 | A kind of preparation method that environment-friendly type graphene conductive carbon is starched and its application on flexible heating film |
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CN111470502A (en) * | 2020-04-14 | 2020-07-31 | 南通强生石墨烯科技有限公司 | Graphene disinfectant and preparation method thereof |
CN111470502B (en) * | 2020-04-14 | 2023-03-31 | 南通强生石墨烯科技有限公司 | Graphene disinfectant and preparation method thereof |
CN114873586A (en) * | 2022-04-26 | 2022-08-09 | 油湃能源环保科技(天津)有限公司 | Preparation method of graphene material dispersion liquid |
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