CN113184837A - Oily graphene dispersion liquid and preparation method thereof - Google Patents
Oily graphene dispersion liquid and preparation method thereof Download PDFInfo
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- CN113184837A CN113184837A CN202110529020.8A CN202110529020A CN113184837A CN 113184837 A CN113184837 A CN 113184837A CN 202110529020 A CN202110529020 A CN 202110529020A CN 113184837 A CN113184837 A CN 113184837A
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- organic solvent
- methylimidazole
- dispersion liquid
- graphite
- graphene dispersion
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
Abstract
The invention provides an oily graphene dispersion liquid and a preparation method thereof. The oily graphene dispersion liquid comprises graphite and an organic solvent, the flake graphite and the organic solvent form the oily graphene dispersion liquid, the graphite in the oily graphene dispersion liquid is one or more of graphite powder, flake graphite, artificial graphite, expandable graphite and expanded graphite, and the organic solvent comprises an organic solvent I and an organic solvent II. The preparation method provided by the invention is simple, high in stripping efficiency, good in product quality, low in energy consumption, easy for large-scale production, wide in application prospect, and capable of being used as a conductive additive to be applied to the fields of graphene electric heating films, lithium batteries, supercapacitors, conductive coatings, graphene heat dissipation materials and the like.
Description
Technical Field
The invention relates to the technical field of graphene, and particularly relates to an oily graphene dispersion liquid and a preparation method thereof.
Background
Graphene has excellent mechanical, electronic, optical and thermal properties, and has been widely used in the fields of nanoelectronics, energy storage, catalysis, biosensors, and the like. In practical application, however, the two-dimensional graphene sheets are very easy to agglomerate, and are difficult to disperse uniformly in the composite material, so that the original characteristics of graphene are greatly weakened. Therefore, graphene needs to be dispersed in an organic solvent or a surfactant aqueous solution, and single-layer dispersion of graphene is achieved by electrostatic repulsion or intermolecular force. The uniform and stable dispersion liquid is an important condition for application and research of graphene in various fields, but the graphene dispersion liquid reported at present is low in concentration and low in single-layer content, and development of graphene is limited.
Therefore, it is necessary to provide a novel oily graphene dispersion and a preparation method thereof to solve the above technical problems.
Disclosure of Invention
In order to solve the technical problems, the invention provides an oily graphene dispersion liquid and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
the oily graphene dispersion liquid comprises graphite and an organic solvent, wherein the scale graphite and the organic solvent form the oily graphene dispersion liquid, and the graphite in the oily graphene dispersion liquid is one or more of graphite powder, scale graphite, artificial graphite, expandable graphite and expanded graphite.
As a further scheme of the invention: the organic solvent consists of an organic solvent I and an organic solvent II.
As a further scheme of the invention: the first organic solvent is chloroform, dimethyl sulfoxide, benzene, N-methyl pyrrolidone, N-dimethylformamide, ethylene glycol, glycerol and tetrahydrofuran.
As a further scheme of the invention: the organic solvent II is an ionic liquid, and the ionic liquid is 1, 3-dimethylimidazole iodide, 1, 3-dimethylimidazole methyl sulfate, 1, 3-dimethylimidazole dimethyl phosphate, 1-ethyl-3-methylimidazole bromide, 1-ethyl-3-methylimidazole iodide, 1-ethyl-3-methylimidazole methyl sulfate, 1-ethyl-3-methylimidazole dimethyl phosphate, 1-ethyl-3-methylimidazole tetrafluoroborate, 1-ethyl-3-methylimidazole hexafluorophosphate, 1-ethyl-3-methylimidazole trifluoromethanesulfonate, 1-ethyl-3-methylimidazole acetate, 1-benzyl-3-methylimidazole bromide, 1-methylimidazole, 1-benzyl-3-methylimidazole chloride, 1-benzyl-3-methylimidazole hexafluorophosphate, 1-benzyl-3-methylimidazole tetrafluoroborate, 1-allyl-3-methylimidazole chloride, 1-allyl-3-methylimidazole bromide, 1-allyl-3-methylimidazole iodide, N-ethylpyridine bromide, N-ethylpyridine iodide, N-ethylpyridine tetrafluoroborate, N-ethylpyridine hexafluorophosphate, N-butylpyridine chloride, N-butylpyridine bromide, N-butylpyridine tetrafluoroborate, and N-butylpyridine hexafluorophosphate.
As a further scheme of the invention: the volume ratio of the organic solvent I to the organic solvent II is as follows: 60:40-95: 5.
The preparation method of the oily graphene dispersion liquid comprises the following specific steps:
the method comprises the following steps: the organic solvent I and the organic solvent II are prepared according to the volume ratio: mixing at a ratio of 60:40-95:5 to obtain an organic solvent;
step two: premixing graphite and an organic solvent under the action of dispersing equipment;
step three: and dispersing the obtained premixed solution by a high-pressure micro-jet homogenizer to obtain the oily graphene dispersion liquid with high purity.
The high-pressure micro-jet homogenizer is circulated for 10 to 200 times under the pressure of 100-300 Mpa.
The dispersing equipment is one or more of an ultrasonic cell crusher, a sand mill, a ball mill and a high-speed shearing emulsifying machine.
Compared with the related art, the oily graphene dispersion liquid and the preparation method thereof provided by the invention have the following beneficial effects:
the preparation method provided by the invention is simple, high in stripping efficiency, good in product quality, low in energy consumption, easy for large-scale production, and wide in application prospect, and can be used as a conductive additive to be applied to the fields of graphene electric heating films, lithium batteries, supercapacitors, conductive coatings, graphene heat dissipation materials and the like.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The first embodiment is as follows:
in the embodiment of the invention, the oily graphene dispersion liquid comprises graphite and an organic solvent, wherein the scale graphite and the organic solvent form the oily graphene dispersion liquid, and the graphite in the oily graphene dispersion liquid is one or more of graphite powder, scale graphite, artificial graphite, expandable graphite and expanded graphite.
Further, the organic solvent is composed of an organic solvent I and an organic solvent II.
Further, the organic solvent I is chloroform, dimethyl sulfoxide, benzene, N-methyl pyrrolidone, N-dimethylformamide, ethylene glycol, glycerol and tetrahydrofuran.
Further, the second organic solvent is ionic liquid, the ionic liquid is one or more of 1, 3-dimethylimidazole iodide, 1, 3-dimethylimidazole methyl sulfate, 1, 3-dimethylimidazole dimethyl phosphate, 1-ethyl-3-methylimidazole bromide, 1-ethyl-3-methylimidazole iodide, 1-ethyl-3-methylimidazole methyl sulfate, 1-ethyl-3-methylimidazole dimethyl phosphate, 1-ethyl-3-methylimidazole tetrafluoroborate, 1-ethyl-3-methylimidazole hexafluorophosphate, 1-ethyl-3-methylimidazole trifluoromethanesulfonate and 1-ethyl-3-methylimidazole acetate.
Further, the volume ratio of the organic solvent I to the organic solvent II is as follows: 60:40-95: 5.
The preparation method of the oily graphene dispersion liquid comprises the following specific steps:
the method comprises the following steps: the organic solvent I and the organic solvent II are prepared according to the volume ratio: mixing at a ratio of 60:40-95:5 to obtain an organic solvent;
step two: premixing graphite and an organic solvent under the action of dispersing equipment;
step three: and dispersing the obtained premixed solution by a high-pressure micro-jet homogenizer to obtain the oily graphene dispersion liquid with high purity.
The high-pressure micro-jet homogenizer is circulated for 10 to 200 times under the pressure of 100-300 Mpa.
The dispersing equipment is one or more of an ultrasonic cell crusher, a sand mill, a ball mill and a high-speed shearing emulsifying machine.
Example two:
in the embodiment of the invention, the oily graphene dispersion liquid comprises graphite and an organic solvent, wherein the scale graphite and the organic solvent form the oily graphene dispersion liquid, and the graphite in the oily graphene dispersion liquid is one or more of graphite powder, scale graphite, artificial graphite, expandable graphite and expanded graphite.
Further, the organic solvent is composed of an organic solvent I and an organic solvent II.
Further, the organic solvent I is chloroform, dimethyl sulfoxide, benzene, N-methyl pyrrolidone, N-dimethylformamide, ethylene glycol, glycerol and tetrahydrofuran.
Further, the organic solvent II is an ionic liquid, and the ionic liquid is 1-benzyl-3-methylimidazole bromide, 1-benzyl-3-methylimidazole chloride, 1-benzyl-3-methylimidazole hexafluorophosphate, 1-benzyl-3-methylimidazole tetrafluoroborate, 1-allyl-3-methylimidazole chloride, 1-allyl-3-methylimidazole bromide, 1-allyl-3-methylimidazole iodide, N-ethylpyridine bromide, N-ethylpyridine iodide, N-ethylpyridine tetrafluoroborate, N-ethylpyridine hexafluorophosphate, N-butylpyridine chloride, N-butylpyridine bromide, N-butylpyridine tetrafluoroborate, N-butylpyridine tetrafluoroborate, N-propylpyridine, N-ethylpyridine, N-propylpyridine, N-methyl-ethyl-methyl-ethyl-methyl-ethyl-methyl-ethyl-methyl-ethyl-methyl-ethyl-methyl-ethyl-methyl-ethyl-propyl-ethyl-propyl-ethyl-, One or more of N-butylpyridinium hexafluorophosphate.
Further, the volume ratio of the organic solvent I to the organic solvent II is as follows: 60:40-95: 5.
The preparation method of the oily graphene dispersion liquid comprises the following specific steps:
the method comprises the following steps: the organic solvent I and the organic solvent II are prepared according to the volume ratio: mixing at a ratio of 60:40-95:5 to obtain an organic solvent;
step two: premixing graphite and an organic solvent under the action of dispersing equipment;
step three: and dispersing the obtained premixed solution by a high-pressure micro-jet homogenizer to obtain the oily graphene dispersion liquid with high purity.
The high-pressure micro-jet homogenizer is circulated for 10 to 200 times under the pressure of 100-300 Mpa.
The dispersing equipment is one or more of an ultrasonic cell crusher, a sand mill, a ball mill and a high-speed shearing emulsifying machine.
According to the invention, the graphene is stripped by selecting the composite organic solvent through a liquid phase stripping method, and the obtained graphene dispersion liquid has high single-layer rate and concentration and good dispersion stability.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. The oily graphene dispersion liquid is characterized by comprising graphite and an organic solvent, wherein the scale graphite and the organic solvent form the oily graphene dispersion liquid, and the graphite in the oily graphene dispersion liquid is one or more of graphite powder, scale graphite, artificial graphite, expandable graphite and expanded graphite.
2. The oily graphene dispersion liquid according to claim 1, wherein the organic solvent is composed of a first organic solvent and a second organic solvent.
3. The oily graphene dispersion liquid according to claim 1, wherein the first organic solvent is chloroform, dimethyl sulfoxide, benzene, N-methylpyrrolidone, N-dimethylformamide, ethylene glycol, glycerol, tetrahydrofuran.
4. The oily graphene dispersion liquid according to claim 1, wherein the organic solvent II is an ionic liquid, and the ionic liquid is 1, 3-dimethylimidazole iodide, 1, 3-dimethylimidazole methyl sulfate, 1, 3-dimethylimidazole dimethyl phosphate, 1-ethyl-3-methylimidazole bromide, 1-ethyl-3-methylimidazole iodide, 1-ethyl-3-methylimidazole methyl sulfate, 1-ethyl-3-methylimidazole dimethyl phosphate, 1-ethyl-3-methylimidazole tetrafluoroborate, 1-ethyl-3-methylimidazole hexafluorophosphate, 1-ethyl-3-methylimidazole trifluoromethanesulfonate, 1-ethyl-3-methylimidazole acetate, or a mixture thereof, One or more of 1-benzyl-3-methylimidazole bromide, 1-benzyl-3-methylimidazole chloride, 1-benzyl-3-methylimidazole hexafluorophosphate, 1-benzyl-3-methylimidazole tetrafluoroborate, 1-allyl-3-methylimidazole chloride, 1-allyl-3-methylimidazole bromide, 1-allyl-3-methylimidazole iodide, N-ethylpyridine bromide, N-ethylpyridine iodide, N-ethylpyridine tetrafluoroborate, N-ethylpyridine hexafluorophosphate, N-butylpyridine chloride, N-butylpyridine bromide, N-butylpyridine tetrafluoroborate, and N-butylpyridine hexafluorophosphate.
5. The oily graphene dispersion liquid according to any one of claims 2 to 4, wherein the volume ratio of the first organic solvent to the second organic solvent is: 60:40-95: 5.
6. The method for preparing the oily graphene dispersion liquid according to claim 1, which comprises the following specific steps:
the method comprises the following steps: the organic solvent I and the organic solvent II are prepared according to the volume ratio: mixing at a ratio of 60:40-95:5 to obtain an organic solvent;
step two: premixing graphite and an organic solvent under the action of dispersing equipment;
step three: and dispersing the obtained premixed solution by a high-pressure micro-jet homogenizer to obtain the oily graphene dispersion liquid with high purity.
7. The method for preparing the oily graphene dispersion liquid according to claim 6, wherein the high-pressure micro-jet homogenizer is cycled for 10-200 times under a pressure of 100-300 MPa.
8. The method for preparing the oily graphene dispersion liquid according to claim 6, wherein the dispersing equipment is one or more of an ultrasonic cell crusher, a sand mill, a ball mill and a high-speed shearing emulsifying machine.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110529020.8A CN113184837A (en) | 2021-05-14 | 2021-05-14 | Oily graphene dispersion liquid and preparation method thereof |
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| CN202110529020.8A CN113184837A (en) | 2021-05-14 | 2021-05-14 | Oily graphene dispersion liquid and preparation method thereof |
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| CN113184837A true CN113184837A (en) | 2021-07-30 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114873584A (en) * | 2022-05-08 | 2022-08-09 | 苏州烯之韵科技有限公司 | Oily graphene dispersion liquid with strong dispersion stability and high monolayer rate and preparation method thereof |
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2021
- 2021-05-14 CN CN202110529020.8A patent/CN113184837A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114873584A (en) * | 2022-05-08 | 2022-08-09 | 苏州烯之韵科技有限公司 | Oily graphene dispersion liquid with strong dispersion stability and high monolayer rate and preparation method thereof |
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