CN109941992A - A kind of Mechanical Method removing graphene of coating and preparation method thereof - Google Patents
A kind of Mechanical Method removing graphene of coating and preparation method thereof Download PDFInfo
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- CN109941992A CN109941992A CN201910281218.1A CN201910281218A CN109941992A CN 109941992 A CN109941992 A CN 109941992A CN 201910281218 A CN201910281218 A CN 201910281218A CN 109941992 A CN109941992 A CN 109941992A
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Abstract
The present invention relates to technical field of graphene preparation, more particularly to a kind of Mechanical Method removing graphene and preparation method thereof of coating, the preparation method includes the following steps: that the surfactant of the crystalline flake graphite powder of 0.5-1.5 parts by weight and 0.05-0.15 parts by weight is dissolved in the deionized waters of 3-7 parts by weight by (1) and forms mixed solution, appropriate amount of addition agent is added, crystalline flake graphite dispersion liquid is formed by mechanical stirring；(2) crystalline flake graphite dispersion liquid is added in sand mill mechanical sand milling, forms graphene slurry；(3) graphene slurry is filtered, the surfactant residual of addition is washed with deionized；(4) filtered graphene is placed in a vacuum drying oven, is dried to Graphene powder.It is excessively light as paint filler appearance that preparation method of the invention solves existing graphene powder, with the problem of resin affinity deficiency, and reduce the dosage of resin, the graphene of coating can be suitable for large scale preparation, the cohesive force of manufactured coating and gum is more preferable.
Description
Technical field
The present invention relates to technical field of graphene preparation, and in particular to a kind of Mechanical Method removing graphene of coating and its
Preparation method.
Background technique
The industrially prepared graphene for products such as coating mostly uses greatly ultrasonic wave and high pressure abrasive condition, and technics comparing is multiple
It is miscellaneous, and graphene relatively drifts, it is insufficient with coating resin affinity.
Graphene is a kind of honeycomb flat film formed by carbon atom with sp2 hybrid form, be it is a kind of only one
The quasi- two-dimensional material of atomic layer level thickness does monoatomic layer graphite so being called.Its thickness is about 0.335nm, according to preparation
The difference of mode and there are different fluctuatings, usually in height about 1nm of vertical direction or so, horizontal direction width is about
10nm to 25nm is the base of all carbon crystals (zero dimension fullerene, one-dimensional carbon nanotube, said three-dimensional body is to graphite) in addition to diamond
This structural unit.
It is poor with the compatibility of water, organic solvent and polymer that the conjugated structure of graphene leads to it, thus increases
Its application difficulty in paint field.
Direct liquid phase removing is to make graphene is stable to be dispersed in by the interaction between solvent and graphene sheet layer
In solvent, and auxiliary agent up-stripping is then that auxiliary agent acts between solvent and lamella, so that graphene be made to be stably dispersed in solvent
In.
Summary of the invention
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide a kind of machines of coating
Tool method removes the preparation method of graphene, and it is excessively light as paint filler appearance which solves existing graphene powder
It floats, the problem with resin affinity deficiency, and reduce the dosage of resin, the graphite of coating can be suitable for large scale preparation
Alkene.
Another object of the present invention is to provide a kind of Mechanical Methods of coating to remove graphene, which removes graphite
The cohesive force of coating and gum made of alkene is more preferable.
The purpose of the invention is achieved by the following technical solution: a kind of preparation side of the Mechanical Method removing graphene of coating
Method includes the following steps:
(1) surfactant of the crystalline flake graphite powder of 0.5-1.5 parts by weight and 0.05-0.15 parts by weight is dissolved in 3-7 weight
It measures and forms mixed solution in the deionized water of part, add appropriate amount of addition agent, crystalline flake graphite dispersion liquid is formed by mechanical stirring；
(2) crystalline flake graphite dispersion liquid is added in sand mill mechanical sand milling, forms graphene slurry；
(3) graphene slurry is filtered, the surfactant residual of addition is washed with deionized；
(4) filtered graphene is placed in a vacuum drying oven, is dried to Graphene powder.
Preferably, in the step (1), the partial size of crystalline flake graphite is 8000-12000 mesh.
Preferably, in the step (1), surfactant is lauryl sodium sulfate, cetane trimethyl ammonium bromide, OP
At least one of emulsifier, triton x-100 and sodium carboxymethylcellulose.
Preferably, in the step (1), auxiliary agent is at least one of defoaming agent, dispersing agent and wetting agent.
Preferably, in the step (1), the additive amount of auxiliary agent is 0.005-0.015 parts by weight.
Preferably, in the step (1), mechanical agitation 6000-8000r/min stirs 1-3h.
Preferably, in the step (2), sand milling condition is 1000-2000r/min, and 6-10h is sanded.
Preferably, in the step (2), mill ball is zirconium pearl of the diameter in 0.8-1.0mm.
Preferably, in the step (3), vacuum drying condition is 80-100 DEG C.
Another object of the present invention is achieved through the following technical solutions: a kind of Mechanical Method removing graphene of coating, institute
Mechanical Method removing graphene is stated to be made according to preparation method described above.
The beneficial effects of the present invention are: preparation method of the invention solves existing graphene powder as paint filler
There is excessively light, the problem with resin affinity deficiency, and reduce the dosage of resin, can be suitable for applying with large scale preparation
The cohesive force of the graphene of material, manufactured coating and gum is more preferable.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of Mechanical Method removing graphene prepared by the present invention.
Specific embodiment
For the ease of the understanding of those skilled in the art, make below with reference to 1 couple of present invention of examples and drawings further
Illustrate, the content that embodiment refers to not is limitation of the invention.
Embodiment 1
A kind of preparation method of the Mechanical Method removing graphene of coating, includes the following steps:
(1) surfactant of the crystalline flake graphite powder of 1 parts by weight and 0.1 parts by weight is dissolved in the deionized water of 5 parts by weight
Middle formation mixed solution adds appropriate amount of addition agent, forms crystalline flake graphite dispersion liquid by mechanical stirring；
(2) crystalline flake graphite dispersion liquid is added in sand mill mechanical sand milling, forms graphene slurry；
(3) graphene slurry is filtered, the surfactant residual of addition is washed with deionized；
(4) filtered graphene is placed in a vacuum drying oven, is dried to Graphene powder.
In the step (1), the partial size of crystalline flake graphite is 12000 mesh.
In the step (1), surfactant is that lauryl sodium sulfate, cetane trimethyl ammonium bromide and carboxymethyl are fine
Tie up the mixture that plain sodium is formed with weight ratio 1:1:1.
In the step (1), auxiliary agent is defoaming agent.
In the step (1), the additive amount of auxiliary agent is 0.01 parts by weight.
In the step (1), mechanical agitation 6000r/min stirs 3h.
In the step (2), sand milling condition is 1000r/min, and 6h is sanded.
In the step (2), mill ball is zirconium pearl of the diameter in 0.9mm.
In the step (3), vacuum drying condition is 90 DEG C.
Embodiment 2
The present embodiment and above-described embodiment 1 the difference is that: by the crystalline flake graphite powder and 0.05 parts by weight of 0.5 parts by weight
Surfactant be dissolved in the deionized water of 3 parts by weight and form mixed solution.
In the step (1), the partial size of crystalline flake graphite is 12000 mesh.
In the step (1), surfactant is the mixing that OP emulsifier and triton x-100 are formed with weight ratio 1:1
Object.
In the step (1), auxiliary agent is the mixture that defoaming agent, ethyl alcohol, n-butanol are formed with volume ratio 1:1:1.
In the step (1), the additive amount of auxiliary agent is 0.01 parts by weight.
In the step (1), mechanical agitation 8000r/min stirs 1h.
In the step (2), sand milling condition is 2000r/min, and 6h is sanded.
In the step (2), mill ball is zirconium pearl of the diameter in 0.9mm.
In the step (3), vacuum drying condition is 90 DEG C.
Embodiment 3
The present embodiment and above-described embodiment 1 the difference is that: by the crystalline flake graphite powder and 0.15 parts by weight of 1.5 parts by weight
Surfactant be dissolved in the deionized water of 7 parts by weight and form mixed solution.
In the step (1), the partial size of crystalline flake graphite is 8000 mesh.
In the step (1), surfactant is that lauryl sodium sulfate, cetane trimethyl ammonium bromide and carboxymethyl are fine
Tie up the mixture that plain sodium is formed with weight ratio 1:1:1.
In the step (1), auxiliary agent is the mixture that defoaming agent, ethyl alcohol, n-butanol are formed with volume ratio 1:1:1.
In the step (1), the additive amount of auxiliary agent is 0.01 parts by weight.
In the step (1), mechanical agitation 8000r/min stirs 3h.
In the step (2), sand milling condition is 2000r/min, and 10h is sanded.
In the step (2), mill ball is zirconium pearl of the diameter in 0.8-1.0mm.
In the step (3), vacuum drying condition is 90 DEG C.
The scanning electron microscope (SEM) photograph of Mechanical Method prepared by the present invention removing graphene is as shown in Figure 1, preparation method solution of the invention
Existing graphene powder of having determined occurs excessively light problem with resin affinity deficiency as paint filler, and reduces tree
The dosage of rouge, can be suitable for the graphene of coating with large scale preparation, and the cohesive force of manufactured coating and gum is more preferable.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other way,
Do not depart under the premise of present inventive concept it is any obviously replace it is within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the Mechanical Method removing graphene of coating, characterized by the following steps:
(1) surfactant of the crystalline flake graphite powder of 0.5-1.5 parts by weight and 0.05-0.15 parts by weight is dissolved in 3-7 weight
It measures and forms mixed solution in the deionized water of part, add appropriate amount of addition agent, crystalline flake graphite dispersion liquid is formed by mechanical stirring；
(2) crystalline flake graphite dispersion liquid is added in sand mill mechanical sand milling, forms graphene slurry；
(3) graphene slurry is filtered, the surfactant residual of addition is washed with deionized；
(4) filtered graphene is placed in a vacuum drying oven, is dried to Graphene powder.
2. a kind of preparation method of the Mechanical Method removing graphene of coating according to claim 1, it is characterised in that: institute
It states in step (1), the partial size of crystalline flake graphite is 8000-12000 mesh.
3. a kind of preparation method of the Mechanical Method removing graphene of coating according to claim 1, it is characterised in that: institute
It states in step (1), surfactant is lauryl sodium sulfate, cetane trimethyl ammonium bromide, OP emulsifier, the logical X- of Qula
At least one of 100 and sodium carboxymethylcellulose.
4. a kind of preparation method of the Mechanical Method removing graphene of coating according to claim 1, it is characterised in that: institute
It states in step (1), auxiliary agent is at least one of defoaming agent, dispersing agent and wetting agent.
5. a kind of preparation method of the Mechanical Method removing graphene of coating according to claim 1, it is characterised in that: institute
It states in step (1), the additive amount of auxiliary agent is 0.005-0.015 parts by weight.
6. a kind of preparation method of the Mechanical Method removing graphene of coating according to claim 1, it is characterised in that: institute
It states in step (1), mechanical agitation 6000-8000r/min, stirs 1-3h.
7. a kind of preparation method of the Mechanical Method removing graphene of coating according to claim 1, it is characterised in that: institute
It states in step (2), sand milling condition is 1000-2000r/min, and 6-10h is sanded.
8. a kind of preparation method of the Mechanical Method removing graphene of coating according to claim 1, it is characterised in that: institute
It states in step (2), mill ball is zirconium pearl of the diameter in 0.8-1.0mm.
9. a kind of preparation method of the Mechanical Method removing graphene of coating according to claim 1, it is characterised in that: institute
It states in step (3), vacuum drying condition is 80-100 DEG C.
10. a kind of Mechanical Method of coating removes graphene, it is characterised in that: the Mechanical Method removing graphene is wanted according to right
The described in any item preparation methods of 1-9 are asked to be made.
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| CN201910281218.1A CN109941992A (en) | 2019-04-09 | 2019-04-09 | A kind of Mechanical Method removing graphene of coating and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022161091A1 (en) * | 2021-01-27 | 2022-08-04 | 广东邦普循环科技有限公司 | Method for preparing graphene by mechanical exfoliation and application thereof |
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| CN104959050A (en) * | 2015-04-29 | 2015-10-07 | 北京天恒盛通科技发展有限公司 | Highly dispersed highly stable high concentration and high yield graphene dispersion liquid and preparation method thereof |
| CN105217612A (en) * | 2015-09-29 | 2016-01-06 | 北京航空航天大学 | A kind of ultrasonic assistant sand mill peels off the method preparing Graphene and the device peeling off Graphene processed |
| CN107043105A (en) * | 2017-05-25 | 2017-08-15 | 拜永孝 | A kind of method of continuous prepare with scale high-quality graphene |
| CN107381643A (en) * | 2016-12-12 | 2017-11-24 | 广东纳路纳米科技有限公司 | A kind of mechanical stripping Van der Waals stratified material prepares the universal method of two-dimensional material |
| CN107459035A (en) * | 2017-05-25 | 2017-12-12 | 拜永孝 | A kind of large-scale preparation method of the controllable high-quality graphene of lamellar spacing |
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2019
- 2019-04-09 CN CN201910281218.1A patent/CN109941992A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104959050A (en) * | 2015-04-29 | 2015-10-07 | 北京天恒盛通科技发展有限公司 | Highly dispersed highly stable high concentration and high yield graphene dispersion liquid and preparation method thereof |
| CN105217612A (en) * | 2015-09-29 | 2016-01-06 | 北京航空航天大学 | A kind of ultrasonic assistant sand mill peels off the method preparing Graphene and the device peeling off Graphene processed |
| CN107381643A (en) * | 2016-12-12 | 2017-11-24 | 广东纳路纳米科技有限公司 | A kind of mechanical stripping Van der Waals stratified material prepares the universal method of two-dimensional material |
| CN107043105A (en) * | 2017-05-25 | 2017-08-15 | 拜永孝 | A kind of method of continuous prepare with scale high-quality graphene |
| CN107459035A (en) * | 2017-05-25 | 2017-12-12 | 拜永孝 | A kind of large-scale preparation method of the controllable high-quality graphene of lamellar spacing |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022161091A1 (en) * | 2021-01-27 | 2022-08-04 | 广东邦普循环科技有限公司 | Method for preparing graphene by mechanical exfoliation and application thereof |
| GB2617023A (en) * | 2021-01-27 | 2023-09-27 | Guangdong Brunp Recycling Technology Co Ltd | Method for preparing graphene by mechanical exfoliation and application thereof |
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Application publication date: 20190628 |