CN115744889A - Method for preparing graphene powder by combining sanding and high-pressure airflow - Google Patents
Method for preparing graphene powder by combining sanding and high-pressure airflow Download PDFInfo
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- CN115744889A CN115744889A CN202211517100.2A CN202211517100A CN115744889A CN 115744889 A CN115744889 A CN 115744889A CN 202211517100 A CN202211517100 A CN 202211517100A CN 115744889 A CN115744889 A CN 115744889A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000000843 powder Substances 0.000 title claims abstract description 28
- 239000004576 sand Substances 0.000 claims abstract description 36
- 238000000227 grinding Methods 0.000 claims abstract description 20
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000003801 milling Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing graphene powder by combining sand grinding and high-pressure air flow. The preparation method provided by the invention adopts a dispersion and stripping mode combining sanding and high-pressure airflow for the first time, the prepared graphene has a complete structure, a few layers and high purity, the excellent performance of the graphene is well reserved, and the graphene can be widely applied to the fields of electronic components, sensors, rubber materials, heat conduction materials and the like. The method disclosed by the invention is simple in equipment, more beneficial to industrial conversion, environment-friendly and low in energy consumption, and can be used for preparing the graphene by a dry method, so that the original structure and characteristics of the graphene are extremely kept while the process is simplified, and the cost is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of preparation of graphene powder materials, and particularly relates to a method for preparing graphene powder by combining sand grinding and high-pressure air flow.
Background
In the prior art, a liquid phase stripping production process is adopted, graphene powder can be obtained only by drying, the drying process is time-consuming and high in energy consumption, and the problems that graphene is denatured and easy to agglomerate in the process due to high temperature are solved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for preparing graphene powder by combining sanding and high-pressure air flow. The preparation method provided by the invention adopts a dispersion and stripping mode combining sanding and high-pressure airflow for the first time, the prepared graphene has a complete structure, a few layers and high purity, the excellent performance of the graphene is well reserved, and the graphene can be widely applied to the fields of electronic components, sensors, rubber materials, heat conduction materials and the like. The method disclosed by the invention is simple in equipment, more beneficial to industrial conversion, environment-friendly and low in energy consumption, and can be used for preparing the graphene by a dry method, so that the original structure and characteristics of the graphene are extremely kept while the process is simplified, and the cost is greatly reduced.
The purpose of the invention is realized by the following technical scheme: a method for preparing graphene powder by combining sand grinding and high-pressure air flow comprises the following specific steps:
step (1), carrying out sanding pretreatment on micron-sized graphite powder by a sand mill to obtain first graphite powder;
step (2), subjecting the first graphite powder obtained in the step one to high-pressure airflow impact, stripping and dispersing to obtain a second multilayer graphene powder with 10-30 layers; the feeding speed of the high-pressure airflow impact in the step (2) is 3 to 5Kg/h, and the airflow pressure is 0.5 to 0.8Mpa;
step (3), carrying out high-pressure airflow impact, stripping and dispersion on the multilayer second graphene powder obtained in the step (2) to obtain a few-layer graphene powder with 3-10 layers; the feeding speed of the high-pressure airflow impact in the step (3) is 8-10 Kg/h, and the airflow pressure is 0.8-1.0 Mpa.
Further, in the step (1), the purity of the graphite powder is 99.90wt% -99.99 wt%, and the median particle diameter D50 is 50-100 μm.
Furthermore, the specification of the sand grinding ball used in the step (1) is one or more of 0.1 μm, 0.5 μm and 1 μm, and the sand grinding ball is matched according to different proportions.
Further, the rotation speed of the sand mill in the step (1) is 1500-3000 rpm.
Further, the total weight of the sand grinding balls in the step (1) is 1Kg.
Further, the sand milling time in the step (1) is 1-5 hours.
Further, the residence cooling time in the step (1) is 1 hour of pause cooling every 1 hour of operation.
Furthermore, in the step (1), the median particle diameter D50 of the graphite powder is 50 μm, the rotation speed of the sand mill is 3000rpm, the mass ratio of the sand milling ball to the sand milling ball is 1.
Further, the pressure of the high-pressure airflow in the step (2) is 0.8Mpa.
Further, the airflow pressure of the high-pressure airflow impact in the step (3) is 1.0Mpa.
Compared with the prior art, the invention has the following positive effects:
the preparation method of the graphene has the advantages of low cost and high purity and yield. The advantages are that:
(1) The preparation method adopts graphite as a raw material, has low price and low cost, is easy to strip into graphene, and can greatly improve the yield;
(2) The preparation method has simple requirements on equipment, convenient operation and few production steps, and is suitable for large-scale production.
(3) The graphene prepared by the preparation method provided by the invention has the advantages of complete structure, few layers and high purity, and the excellent performance of the graphene is well reserved.
Drawings
FIG. 1 is a schematic view of a sander apparatus.
FIG. 2 is a schematic view of a high pressure gas flow apparatus.
Figure 3 is a SEM image of a single sander treatment process.
Fig. 4 is a SEM image of a single high pressure gas stream treatment process.
Fig. 5 is an SEM image of graphene prepared in example 4.
Fig. 6 is a fixed carbon content analysis of the graphene prepared in example 4.
In the figure: the method comprises the following steps of 1, 2, 3, 4, 5, 7, 8, 9 and 10.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
FIG. 1 is a schematic diagram of a sand mill device, wherein a cavity of the sand mill is opened, a certain amount of micron-sized graphite powder 1 is poured into the cavity, the cavity is closed, a cavity cooling circulation device is opened, and the rotating speed, the operating time and the staying cooling time are set. The technological process mainly controls the rotation speed, the running time and the staying and cooling time of the sand mill.
FIG. 2 is a schematic view of a high-pressure airflow separation device, wherein materials are automatically sucked into a high-pressure airflow chamber through a hopper under the condition of negative pressure, the high-pressure airflow is impacted, stripped and dispersed and then is output to a charging basket in a reduced pressure mode, and the feeding speed and the airflow pressure are mainly controlled in the process flow.
The method for preparing the graphene powder by combining sand grinding and high-pressure airflow comprises the following specific steps:
step (1), carrying out sanding pretreatment on micron-sized graphite powder 1 through a sand mill 2 to obtain first graphite powder 3;
step (2), performing high-pressure airflow impact, stripping and dispersion on the first graphite powder obtained in the step one to obtain a multilayer second graphene powder 6 with 10-30 layers; the feeding speed of the high-pressure airflow impact in the step (2) is 3-5 Kg/h, and the airflow pressure is 0.5-0.8 Mpa;
step (3), carrying out high-pressure airflow impact, stripping and dispersion on the multilayer second graphene powder obtained in the step (2) to obtain a few-layer graphene powder 10 with 3-10 layers; the feeding speed of the high-pressure airflow impact in the step (3) is 8-10 Kg/h, and the airflow pressure is 0.8-1.0 Mpa.
Graphite powder in the following examples was purchased from Qingdao rock-ocean carbon materials, inc.
Example 1
After comprehensive analysis and comparison, the following results are obtained: the optimal scheme is that when the size of the raw material is 50 μm, the rotating speed is 3000rpm, the sand grinding ball is 0.1 μm, and the sand grinding time is 3 hours.
Example 2
After adjusting the proportion of the sanding balls according to the results of example 1, it follows: the scheme is optimal when the mass ratio of the sand milling ball (0.1 μm/0.5 μm/1.0 μm) is 1.
Example 3
When the feeding amount does not reach the upper limit of the equipment treatment, the effect is better when the gas flow pressure is larger.
Example 4
When the feeding amount does not reach the upper limit of the equipment treatment, the effect is better when the airflow pressure is higher.
Referring to fig. 5 and 6, SEM spectra and fixed carbon content analysis of the graphenes prepared in examples 1-4 are shown. Compared with the SEM spectrum (shown in figure 3) of a single sand mill treatment process and the SEM spectrum (shown in figure 4) of a single high-pressure gas flow treatment process, the graphene obtained by integrating the embodiments 1 to 4 has high purity and a good sheet structure.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (10)
1. A method for preparing graphene powder by combining sanding and high-pressure airflow is characterized by comprising the following steps: the method comprises the following specific steps:
step (1), carrying out sanding pretreatment on the micron-sized graphite powder through a sanding machine to obtain first graphite powder;
step (2), performing high-pressure airflow impact, stripping and dispersion on the first graphite powder obtained in the step one to obtain a plurality of layers of second graphene powder with 10-30 layers; the feeding speed of the high-pressure airflow impact in the step (2) is 3-5 Kg/h, and the airflow pressure is 0.5-0.8 Mpa;
step (3), carrying out high-pressure airflow impact, stripping and dispersion on the multilayer second graphene powder obtained in the step (2) to obtain a few-layer graphene powder with 3-10 layers; the feeding speed of the high-pressure airflow impact in the step (3) is 8-10 Kg/h, and the airflow pressure is 0.8-1.0 Mpa.
2. The method for preparing the graphene powder by combining sand grinding and high-pressure air flow according to claim 1, wherein the method comprises the following steps: in the step (1), the purity of the graphite powder is 99.90wt% -99.99 wt%, and the median particle diameter D50 is 50-100 μm.
3. The method for preparing the graphene powder by combining sand grinding and high-pressure air flow according to claim 1, wherein the method comprises the following steps: the specification of the sand grinding ball used in the step (1) is one or more of 0.1 μm, 0.5 μm and 1 μm, which are matched according to different proportions.
4. The method for preparing graphene powder by combining sand grinding and high-pressure air flow according to claim 1, wherein the method comprises the following steps: the rotation speed of the sand mill in the step (1) is 1500-3000 rpm.
5. The method for preparing graphene powder by combining sand grinding and high-pressure air flow according to claim 1, wherein the method comprises the following steps: the total weight of the sand grinding balls in the step (1) is 1Kg.
6. The method for preparing the graphene powder by combining sand grinding and high-pressure air flow according to claim 1, wherein the method comprises the following steps: the sand milling time in the step (1) is 1-5 hours.
7. The method for preparing graphene powder by combining sand grinding and high-pressure air flow according to claim 1, wherein the method comprises the following steps: the staying cooling time in the step (1) is 1 hour of pause cooling every 1 hour of operation.
8. The method for preparing graphene powder by combining sand grinding and high-pressure air flow according to claim 1, wherein the method comprises the following steps: in the step (1), the median particle diameter D50 of the graphite powder is 50 μm, the rotation speed of a sand mill is 3000rpm, the mass ratio of a sand milling ball to the graphite powder is 1.
9. The method for preparing the graphene powder by combining sand grinding and high-pressure air flow according to claim 1, wherein the method comprises the following steps: and (3) the air flow pressure of the high-pressure air flow impact in the step (2) is 0.8Mpa.
10. The method for preparing the graphene powder by combining sand grinding and high-pressure air flow according to claim 1, wherein the method comprises the following steps: and (4) the air flow pressure of the high-pressure air flow impact in the step (3) is 1.0Mpa.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103332670A (en) * | 2013-06-21 | 2013-10-02 | 重庆交通大学 | Method for preparing graphene oxide |
| CN205500791U (en) * | 2016-04-08 | 2016-08-24 | 成都新柯力化工科技有限公司 | Shear complete sets who peels off hierarchical preparation graphite alkene in succession |
| CN110066589A (en) * | 2019-05-17 | 2019-07-30 | 张志广 | A kind of graphene zinc-copper multicomponent alloy anticorrosive paint and preparation method thereof |
| CN111048780A (en) * | 2019-12-18 | 2020-04-21 | 武汉低维材料研究院有限公司 | Graphene conductive agent for lithium ion battery and preparation method thereof |
| CN112225208A (en) * | 2020-11-09 | 2021-01-15 | 牛思婷 | Sand mill for preparing graphene through industrialized layered grinding and stripping |
| US20210291320A1 (en) * | 2018-06-28 | 2021-09-23 | Robert Bosch Gmbh | Sanding Block for Manual Use, and System Comprising a Sanding Block and an Abrasive Article |
-
2022
- 2022-11-30 CN CN202211517100.2A patent/CN115744889A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103332670A (en) * | 2013-06-21 | 2013-10-02 | 重庆交通大学 | Method for preparing graphene oxide |
| CN205500791U (en) * | 2016-04-08 | 2016-08-24 | 成都新柯力化工科技有限公司 | Shear complete sets who peels off hierarchical preparation graphite alkene in succession |
| US20210291320A1 (en) * | 2018-06-28 | 2021-09-23 | Robert Bosch Gmbh | Sanding Block for Manual Use, and System Comprising a Sanding Block and an Abrasive Article |
| CN110066589A (en) * | 2019-05-17 | 2019-07-30 | 张志广 | A kind of graphene zinc-copper multicomponent alloy anticorrosive paint and preparation method thereof |
| CN111048780A (en) * | 2019-12-18 | 2020-04-21 | 武汉低维材料研究院有限公司 | Graphene conductive agent for lithium ion battery and preparation method thereof |
| CN112225208A (en) * | 2020-11-09 | 2021-01-15 | 牛思婷 | Sand mill for preparing graphene through industrialized layered grinding and stripping |
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