CN112707390A - Graphene powder preparation method and preparation equipment - Google Patents
Graphene powder preparation method and preparation equipment Download PDFInfo
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- CN112707390A CN112707390A CN202110200487.8A CN202110200487A CN112707390A CN 112707390 A CN112707390 A CN 112707390A CN 202110200487 A CN202110200487 A CN 202110200487A CN 112707390 A CN112707390 A CN 112707390A
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- 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 a preparation method and preparation equipment of graphene powder, which comprises a series of equipment operated in a production line, wherein graphite ore is ground and sieved at the room temperature of 10-30 ℃ to obtain graphite ore powder, the graphite ore powder is added into a cavity of mechanical oscillation equipment for oscillation and acid cleaning, then three-stage cleaning, crushing and microchip stripping are carried out, and the graphite ore powder is sequentially sent into a microwave dryer, a solid-gas separator and a plasma modifier for drying, solid-gas separation and surface modification of graphene, so that the specific surface area of the graphene is increased, the wettability is increased, and finally the modified graphite powder is stored in a storage bin. The graphene powder preparation method and the preparation equipment adopt a production line type industrial processing mode, excessive participation of a chemical process is avoided, no pollution is caused to the environment, the graphene powder is subjected to ion modification, the wettability is good, the whole process is simple, and the manufacturing cost is low.
Description
Technical Field
The invention relates to the field of graphene, in particular to a preparation method and preparation equipment of graphene powder.
Background
The graphene material integrates various excellent properties, and has the unique properties of very good thermal conductivity, good mechanical strength, ultrahigh carrier mobility, excellent electrical conductivity, high light transmittance related to the number of layers and the like. Compared with semiconductor materials, the graphene has extremely high chemical stability, and embodies huge application potential in the fields of microelectronics, information technology, micro-nano sensors, new energy, environment, biomedicine and the like. Particularly, the electron mobility of the graphene material is two orders of magnitude higher than that of a silicon material, and the graphene material is expected to replace the silicon material in the semiconductor industry.
There are also many methods for preparing graphene powder, which can be classified into chemical methods and physical methods.
Wherein, the chemical method mainly comprises an oxidation-reduction method, a chemical vapor deposition method, a pyrolysis-reduction method and the like; the physical methods mainly include a micro-mechanical peeling method, a liquid phase peeling method, and the like.
The method usually needs to use toxic chemical reducing agents such as hydrazine hydrate, dimethylhydrazine, phenylhydrazine and toxic organic reagents such as aldehydes, ethers and the like, and has the disadvantages of harsh reaction conditions, complex steps, high requirements on equipment, long time consumption, uncontrollable reaction conditions, high cost and environmental pollution.
In order to solve the above problems, people are always seeking an ideal technical solution.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a graphene powder preparation method and preparation equipment which adopt a production line type industrial processing mode, avoid excessive participation of a chemical process, have no pollution to the environment, have good wettability by performing ion modification on graphene powder, and have simple whole flow and low manufacturing cost.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of graphene powder comprises the following steps:
step 1) grinding graphite ore at room temperature of 10-30 ℃, then carrying out fine screening to obtain graphite ore powder, adding the graphite ore powder into a cavity of mechanical oscillation equipment for oscillation, simultaneously adding 30-40% dilute nitric acid into the cavity of the mechanical oscillation equipment, and carrying out primary acid washing on the ore powder;
step 2) inputting the graphite slurry after acid washing into a primary cleaning and crushing device, and carrying out primary cleaning, crushing and microchip stripping on graphite powder in the graphite slurry;
step 3) inputting the graphite slurry subjected to primary cleaning, crushing and microchip stripping into a primary separator to separate liquid and graphite powder;
step 4) inputting the graphite powder obtained in the step 3) into a secondary cleaning and crushing device, and carrying out secondary cleaning, crushing and microchip stripping on the graphite powder;
step 5) inputting the graphite slurry subjected to secondary cleaning, crushing and microchip stripping into a secondary separator to separate liquid and graphite powder;
step 6) inputting the graphite powder obtained in the step 5) into a three-stage cleaning and crushing device, and carrying out three-stage cleaning, crushing and microchip stripping on the graphite powder;
step 7), inputting the graphite slurry after the three-time cleaning, crushing and microchip stripping into a three-stage separator to separate liquid and graphite powder;
step 8) inputting the graphite powder obtained in the step 7) into a microwave dryer in a vacuum environment, and drying the graphite powder to remove moisture;
step 9) inputting the dried graphite powder into a solid-gas separator in a vacuum environment to separate the graphite powder from liquid;
step 10), inputting the graphite powder obtained in the step 9) into a plasma modifying machine in a vacuum environment, modifying the surface of graphene, increasing the specific surface area of the graphene and increasing the wettability;
and 11) storing the modified graphite powder in a storage bin.
Basically, in the step 4), the step 6) and the step 8), the graphite powder is conveyed by matching a vacuum conveying pump and an atmospheric pressure conveying pump respectively.
Basically, in the step 8), the step 9) and the step 10), the microwave dryer, the solid-gas separator and the plasma modifier are arranged in the same vacuum environment, and the vacuum environment is provided by using a vacuum pump as a power source.
On the basis, the working frequency of the primary cleaning and crushing device is 20-45KHz, and the working time is 5-45 minutes; the working frequency of the secondary cleaning and crushing device is 30K-80KHz, and the working time is 5-30 minutes; the working frequency of the three-stage cleaning and crushing device is 50K-120KHz, and the working time is 5-40 minutes.
A graphene powder preparation device comprises a primary normal pressure conveying pump, a primary cleaning and crushing device, a primary separator, a first vacuum conveying pump, a secondary normal pressure conveying pump, a secondary cleaning and crushing machine, a secondary separator, a second vacuum conveying pump, a tertiary normal pressure conveying pump, a tertiary cleaning and crushing machine, a tertiary separator, a third vacuum conveying pump, a microwave dryer, a vacuum pump, a solid-gas separator, a plasma modifier and a storage bin, wherein the primary normal pressure conveying pump, the primary cleaning and crushing device, the primary separator, the first vacuum conveying pump, the secondary normal pressure conveying pump, the secondary cleaning and crushing machine, the secondary separator, the second vacuum conveying pump, the tertiary normal pressure conveying pump, the tertiary cleaning and crushing machine, the tertiary separator, the third vacuum conveying pump, the microwave dryer, the solid-gas separator, the plasma modifier and the storage bin are sequentially connected, the vacuum pump is connected with a vacuum chamber and provides a vacuum environment for the vacuum chamber, and the microwave dryer, the solid-gas separator and the plasma modifier are all arranged in the vacuum chamber.
On the basis, the working frequency of the primary cleaning and crushing device is 20-45KHz, and the working time is 5-45 minutes; the working frequency of the secondary cleaning and crushing device is 30K-80KHz, and the working time is 5-30 minutes; the working frequency of the three-stage cleaning and crushing device is 50K-120KHz, and the working time is 5-40 minutes.
Compared with the prior art, the method has outstanding substantive characteristics and remarkable progress, and particularly, the method takes the graphite ore powder as the raw material, obtains a pure graphene powder product with higher wettability through acid washing, three-stage crushing and microchip stripping, three-stage separation and purification, microwave drying, solid-gas separation and ion modification, greatly reduces pollution compared with a production mode of a pure chemical method, has higher industrialization degree compared with the traditional graphene powder product limited to laboratory production, can realize flow line production, meets industrial requirements to a certain degree, simplifies the used equipment and flow, reduces the production difficulty, and greatly reduces the cost.
Drawings
Fig. 1 is a schematic view of the overall structure of the graphene powder preparation apparatus according to the present invention.
Fig. 2 to 4 are schematic structural diagrams of each part of the graphene powder preparation apparatus according to the present invention.
In the figure: 1. a primary normal pressure delivery pump; 2. a primary cleaning and crushing device; 3. a first-stage separator; 4. a first vacuum transfer pump; 5. a secondary normal pressure delivery pump; 6. a secondary cleaning and crushing machine; 7. a secondary separator; 8. a second vacuum transfer pump; 9. a three-stage normal pressure delivery pump; 10. a third stage cleaning and crushing machine; 11. a three-stage separator; 12. a third vacuum transfer pump; 13. a microwave dryer; 14. a vacuum pump; 15. a solid-gas separator; 16. a plasma modifier; 17. a storage bin.
Detailed Description
The technical solution of the present invention is further described in detail by the following embodiments.
As shown in fig. 1-4, a graphene powder preparation apparatus includes a primary atmospheric pressure delivery pump 1, a primary cleaning and crushing device 2, a primary separator 3, a first vacuum delivery pump 4, a secondary atmospheric pressure delivery pump 5, a secondary cleaning and crushing machine 6, a secondary separator 7, a second vacuum delivery pump 8, a tertiary atmospheric pressure delivery pump 9, a tertiary cleaning and crushing machine 10, a tertiary separator 11, a third vacuum delivery pump 12, a microwave dryer 13, a vacuum pump 14, a solid-gas separator 15, a plasma modifier 16 and a storage bin 17, wherein the primary atmospheric pressure delivery pump 1, the primary cleaning and crushing device 2, the primary separator 3, the first vacuum delivery pump 4, the secondary atmospheric pressure delivery pump 5, the secondary cleaning and crushing machine 6, the secondary separator 7, the second vacuum delivery pump 8, the tertiary atmospheric pressure delivery pump 9, the tertiary cleaning and crushing machine 10, the tertiary separator 11, The third vacuum transfer pump 12, the microwave dryer 13, the solid-gas separator 15, the plasma modifier 17 and the storage bin 17 are sequentially connected, the vacuum pump 14 is connected with a vacuum chamber and provides a vacuum environment for the vacuum chamber, and the microwave dryer 13, the solid-gas separator 15 and the plasma modifier 17 are all arranged in the vacuum chamber.
Wherein the working frequency of the first-stage cleaning and crushing device is 20-45KHz, and the working time is 5-45 minutes; the working frequency of the secondary cleaning and crushing device is 30K-80KHz, and the working time is 5-30 minutes; the working frequency of the three-stage cleaning and crushing device is 50K-120KHz, and the working time is 5-40 minutes.
A preparation method of graphene powder comprises the following steps:
step 1) grinding graphite ore at room temperature of 10-30 ℃, then finely screening the ground graphite ore, controlling the mesh number to be 500 meshes to obtain graphite ore powder, adding the graphite ore powder into a cavity of mechanical oscillation equipment for oscillation, simultaneously adding 30-40% dilute nitric acid into the cavity of the mechanical oscillation equipment, carrying out primary acid washing on the ore powder, and removing Al in the ore powder by acid washing2O3And water-insoluble metal oxides such as (aluminum oxide), MgO (magnesium oxide), CaO (calcium oxide), and CuO (copper oxide). At the same time, the graphite slurry is subjected to primary microchip stripping and particle crushing. The duration of the whole crushing and stripping process is about 5-45 minutes.
And 2) inputting the pickled graphite slurry into a primary cleaning and crushing device, and carrying out primary cleaning, crushing and microchip stripping on graphite powder in the graphite slurry, wherein the multi-stage cleaning and crushing device is made of corrosion-resistant materials.
And 3) inputting the graphite slurry subjected to primary cleaning, crushing and microchip stripping into a primary separator, separating liquid and graphite powder, wherein the separated slurry retains graphite microchip, and inorganic salt and water are separated out. And (4) purifying and separating the separated solution again, recycling part of the solution, and performing harmless treatment on part of the solution to form inorganic salt slag. The step realizes the harmlessness of the waste liquid treatment process.
And 4) inputting the graphite powder obtained in the step 3) into a secondary cleaning and crushing device, and carrying out secondary cleaning, crushing and microchip stripping on the graphite powder.
And 5) inputting the graphite slurry subjected to secondary cleaning, crushing and microchip stripping into a secondary separator, separating liquid and graphite powder, separating graphite microchip and inorganic salt and water dissolved in water, refining and separating the waste water solution, recycling the separated water, and recycling the inorganic salt to form purified slag for other purposes.
And 6) inputting the graphite powder obtained in the step 5) into a three-stage cleaning and crushing device, and carrying out three-stage cleaning, crushing and microchip stripping on the graphite powder.
And 7) inputting the graphite slurry subjected to the three-time cleaning, crushing and microchip stripping into a three-stage separator to separate liquid and graphite powder.
And 8) inputting the graphite powder obtained in the step 7) into a microwave dryer in a vacuum environment, drying the graphite powder, and removing moisture, wherein the microwave heating time and intensity are controllable. In this example, the duration is 1-15 minutes.
Step 9) inputting the dried graphite powder into a solid-gas separator in a vacuum environment to separate the graphite powder from liquid;
and step 10) inputting the graphite powder obtained in the step 9) into a plasma modifying machine in a vacuum environment, wherein the specific surface area of the modified graphene powder is obviously increased compared with the original specific surface area, the surface energy of the graphene powder is reduced, and the wettability of the graphite powder is enhanced. The graphene powder is easy to disperse and not easy to agglomerate. And obtaining the graphene powder.
And 11) storing the modified graphite powder in a storage bin, and then sealing and packaging by a packaging machine.
In the step 4), the step 6) and the step 8), the graphite powder is conveyed by matching a vacuum transfer pump and an atmospheric pressure delivery pump respectively, and in the step 8), the step 9) and the step 10), the microwave dryer, the solid-gas separator and the plasma modifier are arranged in the same vacuum environment, and the vacuum environment is provided by taking a vacuum pump as a power source.
Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present invention and not to limit the same; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.
Claims (6)
1. A preparation method of graphene powder is characterized by comprising the following steps: the method comprises the following steps:
step 1) grinding graphite ore at room temperature of 10-30 ℃, then carrying out fine screening to obtain graphite ore powder, adding the graphite ore powder into a cavity of mechanical oscillation equipment for oscillation, simultaneously adding 30-40% dilute nitric acid into the cavity of the mechanical oscillation equipment, and carrying out primary acid washing on the ore powder;
step 2) inputting the graphite slurry after acid washing into a primary cleaning and crushing device, and carrying out primary cleaning, crushing and microchip stripping on graphite powder in the graphite slurry;
step 3) inputting the graphite slurry subjected to primary cleaning, crushing and microchip stripping into a primary separator to separate liquid and graphite powder;
step 4) inputting the graphite powder obtained in the step 3) into a secondary cleaning and crushing device, and carrying out secondary cleaning, crushing and microchip stripping on the graphite powder;
step 5) inputting the graphite slurry subjected to secondary cleaning, crushing and microchip stripping into a secondary separator to separate liquid and graphite powder;
step 6) inputting the graphite powder obtained in the step 5) into a three-stage cleaning and crushing device, and carrying out three-stage cleaning, crushing and microchip stripping on the graphite powder;
step 7), inputting the graphite slurry after the three-time cleaning, crushing and microchip stripping into a three-stage separator to separate liquid and graphite powder;
step 8) inputting the graphite powder obtained in the step 7) into a microwave dryer in a vacuum environment, and drying the graphite powder to remove moisture;
step 9) inputting the dried graphite powder into a solid-gas separator in a vacuum environment to separate the graphite powder from liquid;
step 10), inputting the graphite powder obtained in the step 9) into a plasma modifying machine in a vacuum environment, modifying the surface of graphene, increasing the specific surface area of the graphene and increasing the wettability;
and 11) storing the modified graphite powder in a storage bin.
2. The method for preparing graphene powder according to claim 1, wherein: and in the steps 4), 6) and 8), the graphite powder is conveyed by matching a vacuum conveying pump and a normal pressure conveying pump respectively.
3. The method for preparing graphene powder according to claim 1 or 2, wherein: in the steps 8), 9) and 10), the microwave dryer, the solid-gas separator and the plasma modifier are arranged in the same vacuum environment, and the vacuum environment is provided by a vacuum pump as a power source.
4. The method for preparing graphene powder according to claim 3, wherein: the working frequency of the first-stage cleaning and crushing device is 20-45KHz, and the working time is 5-45 minutes; the working frequency of the secondary cleaning and crushing device is 30K-80KHz, and the working time is 5-30 minutes; the working frequency of the three-stage cleaning and crushing device is 50K-120KHz, and the working time is 5-40 minutes.
5. A graphite alkene powder preparation equipment which characterized in that: comprises a primary normal pressure conveying pump, a primary cleaning and crushing device, a primary separator, a first vacuum conveying pump, a secondary normal pressure conveying pump, a secondary cleaning and crushing machine, a secondary separator, a second vacuum conveying pump, a tertiary normal pressure conveying pump, a tertiary cleaning and crushing machine, a tertiary separator, a third vacuum conveying pump, a microwave dryer, a vacuum pump, a solid-gas separator, a plasma modifier and a storage bin, wherein the primary normal pressure conveying pump, the primary cleaning and crushing device, the primary separator, the first vacuum conveying pump, the secondary normal pressure conveying pump, the secondary cleaning and crushing machine, the secondary separator, the second vacuum conveying pump, the tertiary normal pressure conveying pump, the tertiary cleaning and crushing machine, the tertiary separator, the third vacuum conveying pump, the microwave dryer, the solid-gas separator, the plasma modifier and the storage bin are sequentially connected, the vacuum pump is connected with a vacuum chamber and provides a vacuum environment for the vacuum chamber, the microwave dryer, the solid-gas separator and the plasma modifier are all arranged in the vacuum chamber.
6. The graphene powder preparation apparatus according to claim 5, wherein: the working frequency of the first-stage cleaning and crushing device is 20-45KHz, and the working time is 5-45 minutes; the working frequency of the secondary cleaning and crushing device is 30K-80KHz, and the working time is 5-30 minutes; the working frequency of the three-stage cleaning and crushing device is 50K-120KHz, and the working time is 5-40 minutes.
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