CN117735538A - Homogeneous graphene slurry and preparation method and application thereof - Google Patents
Homogeneous graphene slurry and preparation method and application thereof Download PDFInfo
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- CN117735538A CN117735538A CN202311723204.3A CN202311723204A CN117735538A CN 117735538 A CN117735538 A CN 117735538A CN 202311723204 A CN202311723204 A CN 202311723204A CN 117735538 A CN117735538 A CN 117735538A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 176
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 137
- 239000002002 slurry Substances 0.000 title claims abstract description 90
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 238000007613 slurry method Methods 0.000 title description 2
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000006185 dispersion Substances 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 38
- 238000003756 stirring Methods 0.000 claims description 36
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 229920005989 resin Polymers 0.000 claims description 18
- 239000011347 resin Substances 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000003607 modifier Substances 0.000 claims description 16
- 239000010687 lubricating oil Substances 0.000 claims description 15
- 239000003973 paint Substances 0.000 claims description 14
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000007795 chemical reaction product Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 229920001661 Chitosan Polymers 0.000 claims description 6
- 239000003292 glue Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 229920002430 Fibre-reinforced plastic Polymers 0.000 claims description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 claims description 4
- 239000011151 fibre-reinforced plastic Substances 0.000 claims description 4
- 229910001416 lithium ion Inorganic materials 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229920001690 polydopamine Polymers 0.000 claims description 3
- 239000003995 emulsifying agent Substances 0.000 claims description 2
- 239000000499 gel Substances 0.000 claims description 2
- 238000007790 scraping Methods 0.000 claims description 2
- 239000002270 dispersing agent Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 238000010907 mechanical stirring Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 238000002211 ultraviolet spectrum Methods 0.000 description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a homogeneous graphene slurry and a preparation method and application thereof, and belongs to the technical field of graphene slurry. The preparation method disclosed by the invention can prepare the homogeneous graphene slurry with good uniformity and high stability on the premise of not adding the dispersant for assistance. Compared with the existing graphene slurry preparation technology, the preparation method is simple in preparation process, does not need dispersant assistance, enables graphene to be uniformly dispersed in a solvent through repeated dispersion for many times, and the prepared graphene slurry is good in uniformity, high in stability, wide in application and easy to realize industrial serialization. And the homogeneous graphene slurry has wide application range and good application prospect.
Description
Technical Field
The invention belongs to the technical field of graphene slurry, and particularly relates to a homogeneous graphene slurry, and a preparation method and application thereof.
Background
Because graphene has excellent mechanical, electrical and heat conducting properties, the graphene is widely applied to various fields such as composite materials, heat conducting materials, large health, electronic batteries and the like. Graphene products are numerous and include reduced graphene, oxidized graphene, expanded graphite, and the like. Most of the application of the graphene material requires that graphene is dispersed in a solvent in a proper mode to obtain graphene slurry, and then the graphene slurry is subjected to a subsequent production process to obtain a product. However, because graphene is difficult to disperse in a solvent, aggregation is easy to occur, and the dispersion slurry is uneven and unstable and has low concentration, so that the preparation and application of the graphene slurry are greatly limited.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a homogeneous graphene slurry, and a preparation method and application thereof, which are used for solving the technical problems of agglomeration, instability and the like of the existing graphene slurry.
In order to achieve the above purpose, the invention is realized by adopting the following technical scheme:
the invention discloses a preparation method of homogeneous graphene slurry, which comprises the following steps:
s1: mixing a modifier, deionized water, ethanol and acetic acid to obtain a modified solution; stirring and mixing the modified solution and graphene powder to obtain a modified graphene solution; carrying out hydrothermal reaction on the modified graphene solution, obtaining a reaction product after the reaction is finished, and carrying out aftertreatment on the reaction product to obtain modified graphene powder;
s2: dispersing the modified graphene powder in a solvent, and stirring and dispersing to obtain graphene pre-dispersion slurry;
s3: and dispersing the graphene pre-dispersed slurry again to obtain the homogeneous graphene slurry.
Further, in S1, the modifier is any one of chitosan, ethylenediamine, dodecylamine, octadecylamine and polydopamine;
the mass ratio of the modifier to the ethanol to the acetic acid to the deionized water is (1-10): (5-10): (5-10): (100-200).
Further, in S1, the graphene powder is one of graphene oxide, reduced graphene or expanded graphite; the stirring time is 2-10h, and the stirring rotating speed is 800-2000 rpm;
the post-treatment is to sequentially centrifuge, wash and dry the reaction product; the washing is carried out by adopting deionized water and ethanol; the drying temperature is 60-100 ℃ and the drying time is 10-24 hours;
the temperature of the hydrothermal reaction is 160-300 ℃ and the time is 8-24h.
Further, in S2, the solvent is any one of water, ethanol, dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide, an unsaturated resin, UV glue, paint or lubricating oil.
Further, in S2, when the graphene powder is graphene oxide, reduced graphene and expanded graphite, the mass concentrations of the graphene oxide, reduced graphene and expanded graphite in the graphene pre-dispersion slurry are 3% -10%, 0.5% -5% and 5% -15%, respectively.
Further, in S2, the modified graphene powder is dispersed in a solvent, and stirring and dispersing are performed by adopting a stirring kettle; the stirring kettle is provided with jacket cooling water to cool the system;
when the solvent is unsaturated resin, UV glue, paint or lubricating oil, a stirring kettle used for dispersing the modified graphene powder in the solvent is a doorframe-type stirrer with a scraping plate;
when the solvent is a solvent other than unsaturated resin, UV glue, paint or lubricating oil, the stirring kettle used for dispersing the modified graphene powder in the solvent is a disk turbine type or paddle type stirrer.
Further, in S2, the stirring and dispersing time is 0.5-12h, and the stirring rotating speed is 1000-2000 rpm.
Further, in S3, the fine dispersing device used for dispersing the graphene pre-dispersed slurry again is one of a high-pressure homogenizer, a high-shear emulsifying machine and a planetary dispersing machine.
The invention also discloses the homogeneous graphene slurry prepared by the preparation method.
The invention also discloses application of the homogeneous graphene slurry, wherein the homogeneous graphene slurry is used together with unsaturated resin and is used as a production raw material of fiber reinforced plastics;
the homogeneous graphene slurry is used as a preparation raw material of lithium ion battery slurry or heavy anti-corrosion paint and lubricating oil
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of homogeneous graphene slurry, which adopts a modifier, deionized water, ethanol and acetic acid as preparation raw materials of modified graphene powder, and can prepare the homogeneous graphene slurry with good uniformity and high stability on the premise of not adding dispersant assistance. Compared with the existing graphene slurry preparation technology, the preparation method is simple in preparation process, does not need dispersant assistance, enables graphene to be uniformly dispersed in a solvent through repeated dispersion for many times, and the prepared graphene slurry is good in uniformity, high in stability, wide in application and easy to realize industrial serialization.
The invention also discloses application of the homogeneous graphene slurry prepared by the preparation method, and the graphene is dispersed in unsaturated resin to obtain graphene resin slurry, and the graphene resin slurry can be used for producing fiber reinforced plastics. The graphene is dispersed in DMA, NMP, DMF and can be used in textile industry, the conductive graphene NMP slurry can be used in the field of lithium ion battery slurry, the graphene water slurry can be coated to prepare a graphene heat dissipation film or a graphene heat conduction film, graphene paint and graphene lubricating oil slurry can be used in the field of heavy anti-corrosion paint and lubricating oil, and the graphene UV adhesive slurry can be used as a UV adhesive, so that the graphene water-based graphene heat dissipation film or graphene lubricating oil slurry has wide application range and good application prospect.
Drawings
FIG. 1 is an XRD pattern of graphene oxide powder modified with chitosan;
FIG. 2 is an ultraviolet spectrum of a graphene slurry of the present invention;
FIG. 3 is a graphene SMC composite material prepared using a graphene unsaturated resin slurry;
wherein: a-graphene SMC composite sample plate; b-preparing the graphene SMC composite material;
fig. 4 is a graph showing particle size distribution of graphene before and after dispersion.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
All features such as values, amounts, and concentrations that are defined herein in the numerical or percent ranges are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise indicated, "comprising," "including," "having," or similar terms encompass the meanings of "consisting of … …" and "consisting essentially of … …," e.g., "a includes a" encompasses the meanings of "a includes a and the other and" a includes a only.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The invention provides a preparation method of homogeneous graphene slurry, which comprises the following steps:
a) Uniformly mixing a modifier, deionized water, ethanol and acetic acid according to a certain proportion to obtain a modified solution;
b) Adding graphene powder into the modified solution, continuously stirring, and modifying the graphene powder to obtain a modified graphene solution;
c) Placing the modified graphene solution into a hydrothermal kettle, and performing hydrothermal reaction in a constant-temperature drying oven;
d) Centrifugal washing and drying to obtain modified graphene powder;
e) Adding the modified graphene powder into a solvent for mechanical stirring and pre-dispersing to obtain graphene pre-dispersing slurry;
f) Dispersing the pre-dispersed slurry again by using fine dispersing equipment to obtain homogeneous graphene slurry;
preferably, in the step a), the modifier is any one of chitosan, ethylenediamine, dodecylamine, octadecylamine and polydopamine. The mass ratio of the modifier to the ethanol to the acetic acid to the deionized water is (1-10): 5-10: (100-200).
Preferably, in the step b), the graphene powder is one of graphene oxide, reduced graphene and expanded graphite; the stirring and mixing time is 2-10h, and the stirring rotating speed is 800-2000 rpm.
Preferably, in step c), the hydrothermal temperature is 160-300 ℃ and the hydrothermal time is 8-24 hours.
Preferably, in step d), the supernatant is removed by centrifugation and then washed with deionized water and ethanol. The drying temperature of the graphene powder is 60-100 ℃ and the drying time is 10-24h.
Preferably, in step e), the solvent is any one of water, ethanol, DMA (dimethylacetamide), NMP (N-methylpyrrolidone), DMF (N, N-dimethylformamide), unsaturated resins, UV gel, paint, and lubricating oil.
Preferably, in the step e), the graphene powder is fed into the stirring kettle by a vacuum powder feeder; the concentration of the graphene oxide is 3% -10%, the concentration of the reduced graphene is 0.5% -5%, and the concentration of the expanded graphite is 5% -15%.
Preferably, in step e), when the mechanical stirring device uses unsaturated resin, UV glue, paint and lubricating oil as solvents, a doorframe type stirrer with a scraper is adopted to prevent the mechanical stirring device from being attached to the inner side of the kettle wall due to the high viscosity; when dispersing with other solvents, a disk turbine or paddle stirrer may be used.
Preferably, in step e), the stirring and dispersing time is 0.5-12h, and the stirring speed is 1000-2000 rpm; the stirring kettle is provided with jacket cooling water to cool the system, and the pre-dispersed material is pumped into fine dispersing equipment from a kettle bottom outlet by a diaphragm pump to perform the preparation operation of step e).
Preferably, in step f), the fine dispersing apparatus is one of a high pressure homogenizer, a high shear emulsifier, a planetary disperser; and uniformly dispersing graphene in the solvent through repeated dispersion for a plurality of times to obtain uniform graphene slurry.
The homogeneous and stable graphene slurry prepared by the method has wide application; graphene is dispersed in unsaturated resin to obtain graphene resin slurry, and the graphene resin slurry can be used for producing fiber reinforced plastics. Dispersing graphene in DMA, NMP, DMF can be used in textile industry, the conductive graphene NMP slurry can be used in the field of lithium ion battery slurry, the graphene water-based slurry can be coated to prepare a graphene heat dissipation film or a graphene heat conduction film, graphene paint and graphene lubricating oil slurry can be used in the field of heavy anti-corrosion paint and lubricating oil, and the graphene UV adhesive slurry can be used as a UV adhesive.
Preferably, the specific surface area of the reduced graphene is 300-1000m 2 The D50 is 20-80 μm.
The preparation method disclosed by the invention has the advantages of simple preparation process, no need of auxiliary dispersing agent, good uniformity, high stability and wide application, and is easy for industrial serialization.
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents are intended to fall within the scope of the claims appended hereto.
The following examples use instrumentation conventional in the art. The experimental methods, in which specific conditions are not noted in the following examples, are generally conducted under conventional conditions or under conditions recommended by the manufacturer. The following examples used various starting materials, unless otherwise indicated, were conventional commercial products, the specifications of which are conventional in the art. In the description of the present invention and the following examples, "%" means weight percent, and "parts" means parts by weight, and ratios means weight ratio, unless otherwise specified.
Example 1
The preparation method of the homogeneous graphene slurry comprises the following steps:
s1: chitosan, deionized water, ethanol and acetic acid are mixed according to the weight ratio of 1:5:10: mixing the materials according to the mass ratio of 100 to prepare a modifier solution, and mechanically stirring the materials at the speed of 1000 revolutions per minute for 5 hours to obtain a uniform modifier solution; then adding graphene oxide powder, and stirring for 6 hours at the speed of 1200 rpm to obtain a modified graphene solution; placing the modified graphene solution into a hydrothermal kettle, performing hydrothermal reaction at 180 ℃ for 12 hours, centrifuging a reaction product after the reaction is finished, removing supernatant, washing with deionized water and ethanol for multiple times, and drying in a baking oven at 70 ℃ for 10 hours after washing to obtain modified graphene powder;
s2: adding modified graphene oxide powder into DMA (direct memory access) at a mass concentration of 5%, and mechanically stirring for 8 hours to obtain graphene pre-dispersion slurry;
s3: and dispersing the graphene pre-dispersion slurry again for 4 hours by using a planetary dispersing machine to obtain uniform and stable homogeneous graphene slurry.
Fig. 1 shows an XRD spectrum of the chitosan-modified graphene oxide powder obtained in this example, and it can be seen from the figure that after the chitosan modification is added, the crystallinity of the composite material is increased, the uniformity of the molecular chain is increased, the regularity is improved, and the dispersion performance of the graphene oxide is increased.
Example 2
The preparation method of the homogeneous graphene slurry comprises the following steps:
s1: ethylenediamine, deionized water, ethanol and acetic acid according to the weight ratio of 1:10:5:120, preparing a modifier solution after mixing, and mechanically stirring for 8 hours at the speed of 1200 revolutions per minute to obtain a uniform modifier solution; then adding expanded graphite, and stirring for 5 hours at the speed of 1200 rpm to obtain a modified graphene solution; placing the modified graphene solution into a hydrothermal kettle, performing hydrothermal reaction at 220 ℃ for 8 hours, centrifuging a reaction product after the reaction is finished, removing supernatant, washing with deionized water and ethanol for multiple times, and drying in an oven at 80 ℃ for 18 hours after washing to obtain modified graphene powder;
s2: adding the modified expanded graphite into NMP at a mass concentration of 15%, and mechanically stirring for 10 hours to obtain graphene pre-dispersion slurry;
s3: and dispersing the graphene pre-dispersed slurry again for 4 hours by using a high-shear emulsifying machine to obtain uniform and stable homogeneous graphene slurry.
FIG. 2 is a UV spectrum of a 15% expanded graphite NMP slurry; the purple curve is one day of preparation, and the red curve is one month of preparation, so that the absorbance reduction amplitude is small, and the slurry is still stable under long-term placement.
Example 3
The preparation method of the homogeneous graphene slurry comprises the following steps:
s1: mixing dodecyl amine, deionized water, ethanol and acetic acid according to a ratio of 2:5:5:150, preparing a modifier solution after mixing, and mechanically stirring at a speed of 1500 rpm for 4 hours to obtain a uniform modifier solution; then adding reduced graphene, and stirring for 5 hours at the speed of 1600 rpm to obtain a modified graphene solution; placing the modified graphene solution into a hydrothermal kettle, performing hydrothermal reaction at 250 ℃ for 6 hours, centrifuging a reaction product after the reaction is finished, removing supernatant, washing with deionized water and ethanol for multiple times, and drying in a baking oven at 90 ℃ for 15 hours after washing to obtain modified graphene powder;
s2: adding the modified graphene oxide powder into unsaturated polyester resin at a mass concentration of 1.5%, and mechanically stirring for 10 hours to obtain graphene pre-dispersion slurry;
s3: and (3) dispersing the graphene pre-dispersion slurry again for 4 hours by using a high-pressure homogenizer to obtain uniform and stable homogeneous graphene slurry.
The graphene resin slurry is used for adding auxiliary glass fiber and the like to prepare the graphene SMC composite material, and the graphene SMC composite material is shown in figure 3. The particle size of the sample before and after dispersion of graphene is shown in fig. 4. It can be seen that the particle size of the dispersed graphene powder is greatly reduced.
The specific surface area of the reduced graphene used in the above embodiment is 300-1000m 2 The D50 is 20-80 μm.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. The preparation method of the homogeneous graphene slurry is characterized by comprising the following steps of:
s1: mixing a modifier, deionized water, ethanol and acetic acid to obtain a modified solution; stirring and mixing the modified solution and graphene powder to obtain a modified graphene solution; carrying out hydrothermal reaction on the modified graphene solution, obtaining a reaction product after the reaction is finished, and carrying out aftertreatment on the reaction product to obtain modified graphene powder;
s2: dispersing the modified graphene powder in a solvent, and stirring and dispersing to obtain graphene pre-dispersion slurry;
s3: and dispersing the graphene pre-dispersed slurry again to obtain the homogeneous graphene slurry.
2. The preparation method of the homogeneous graphene slurry according to claim 1, wherein in S1, the modifier is any one of chitosan, ethylenediamine, octadecylamine and polydopamine;
the mass ratio of the modifier to the ethanol to the acetic acid to the deionized water is (1-10): (5-10): (5-10): (100-200).
3. The method for preparing a homogeneous graphene slurry according to claim 1, wherein in S1, the graphene powder is one of graphene oxide, reduced graphene or expanded graphite; the stirring time is 2-10h, and the stirring rotating speed is 800-2000 rpm;
the post-treatment is to sequentially centrifuge, wash and dry the reaction product; the washing is carried out by adopting deionized water and ethanol; the drying temperature is 60-100 ℃ and the drying time is 10-24 hours;
the temperature of the hydrothermal reaction is 160-300 ℃ and the time is 8-24h.
4. The method for preparing a homogeneous graphene slurry according to claim 3, wherein in S2, the solvent is any one of water, ethanol, dimethylacetamide, N-methylpyrrolidone, N-dimethylformamide, an unsaturated resin, UV gel, paint or lubricating oil.
5. The preparation method of the homogeneous graphene slurry according to claim 4, wherein in S2, when graphene powder is graphene oxide, reduced graphene and expanded graphite respectively, the mass concentration of the graphene oxide, reduced graphene and expanded graphite in the graphene pre-dispersion slurry is 3% -10%, 0.5% -5% and 5% -15%, respectively.
6. The preparation method of the homogeneous graphene slurry according to claim 5, wherein in S2, the modified graphene powder is dispersed in a solvent and stirred and dispersed by a stirred tank; the stirring kettle is provided with jacket cooling water to cool the system;
when the solvent is unsaturated resin, UV glue, paint or lubricating oil, a stirring kettle used for dispersing the modified graphene powder in the solvent is a doorframe-type stirrer with a scraping plate;
when the solvent is a solvent other than unsaturated resin, UV glue, paint or lubricating oil, the stirring kettle used for dispersing the modified graphene powder in the solvent is a disk turbine type or paddle type stirrer.
7. The method for preparing a homogeneous graphene slurry according to claim 6, wherein in S2, the stirring and dispersing time is 0.5-12h, and the stirring speed is 1000-2000 rpm.
8. The method for preparing a homogeneous graphene slurry according to claim 1, wherein in S3, the fine dispersing device used for dispersing the graphene pre-dispersed slurry again is one of a high-pressure homogenizer, a high-shear emulsifier and a planetary dispersing machine.
9. A homogeneous graphene slurry, characterized in that the homogeneous graphene slurry is prepared by the preparation method of the homogeneous graphene slurry according to any one of claims 1 to 8.
10. The use of a homogeneous graphene slurry according to claim 9, wherein the homogeneous graphene slurry is used in combination with an unsaturated resin as a raw material for the production of fiber reinforced plastics;
the homogeneous graphene slurry is used as a preparation raw material of lithium ion battery slurry or heavy anti-corrosion paint and lubricating oil.
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| CN202311723204.3A CN117735538A (en) | 2023-12-14 | 2023-12-14 | Homogeneous graphene slurry and preparation method and application thereof |
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