CN108862259B - Graphene production method and device - Google Patents
Graphene production method and device Download PDFInfo
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- CN108862259B CN108862259B CN201810917889.8A CN201810917889A CN108862259B CN 108862259 B CN108862259 B CN 108862259B CN 201810917889 A CN201810917889 A CN 201810917889A CN 108862259 B CN108862259 B CN 108862259B
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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 discloses a graphene production method and a graphene production device, wherein the graphene production device comprises a first stirrer, a high-speed dispersion machine, a second stirrer, a reaction kettle, a cooling storage tank, a horizontal screw centrifuge, a homogenizer and a drying agent which are sequentially communicated through a pipeline.
Description
Technical Field
The invention relates to the field of graphene preparation, in particular to a graphene production method and device.
Background
Graphene (Graphene) is a two-dimensional carbon nanomaterial composed of carbon atoms in sp hybridized orbitals into a hexagonal honeycomb lattice. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future. The physicists andrelim and consanguin norworth schloff, manchester university, uk, successfully separated graphene from graphite by micromechanical exfoliation, thus collectively awarding the 2010 nobel prize for physics.
Common powder production methods of graphene include a mechanical stripping method, a redox method, SiC epitaxial growth and the like, however, these methods are generally only applicable to small-scale laboratory production, cannot be used for large-scale industrial production, and also contain a large amount of impurities, which are difficult to use. The method also has the problems of large energy loss, easy environmental pollution and the like.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a graphene production method and a graphene production device, and aims to realize the purpose of industrially producing high-purity graphene in a large scale with low energy consumption, no pollution and high efficiency.
The technical scheme of the invention is as follows:
a graphene production device comprises a first stirrer for stirring crystalline flake graphite and an intercalator to generate a graphite mixture, a high-speed disperser for dispersing the graphite mixture, a cooling storage tank for cooling the graphite mixture, a second stirrer for stirring the graphite mixture and the reaction liquid, a reaction kettle for enabling the graphite mixture and the reaction liquid to react to generate graphene raw stock, a horizontal screw centrifuge for cleaning the graphene raw stock, a homogenizer for dispersing the graphene raw stock and a dryer for drying the graphene raw stock to obtain graphene powder, the first stirrer, the high-speed dispersion machine, the cooling storage tank, the second stirrer, the reaction kettle, the horizontal screw centrifuge, the homogenizer and the dryer are sequentially communicated through pipelines.
Graphene apparatus for producing, wherein, still including the heating furnace that is used for carrying out bulking treatment to the scale graphite, the heating furnace pass through the pipeline with first mixer intercommunication.
Graphene apparatus for producing, wherein, still including the cleaning machine that is used for carrying out cleaning treatment to the scale graphite, the cleaning machine pass through the pipeline with the heating furnace intercommunication.
The graphene production device, wherein the first stirrer is a vacuum stirrer.
A graphene production method, comprising the steps of:
putting the cleaned crystalline flake graphite into a heating furnace for expansion treatment to obtain expanded crystalline flake graphite;
putting the expanded crystalline flake graphite and the intercalation agent into a first stirrer for vacuum stirring, so that the intercalation agent uniformly permeates into the expanded crystalline flake graphite to obtain a graphite mixture;
putting the graphite mixture into a high-speed disperser for dispersing treatment;
placing the graphite mixture subjected to the dispersion treatment into a cooling storage tank for cooling treatment;
placing the cooled graphite mixture and the reaction liquid into a second stirrer for stirring treatment;
placing the stirred graphite mixture and the reaction liquid into a reaction kettle for full reaction to generate graphene raw stock;
placing the graphene raw stock into a non-spiral centrifuge for centrifugal cleaning treatment;
placing the centrifuged graphene raw stock into a homogenizer for dispersion treatment;
and (4) putting the dispersed graphene raw stock into a dryer for drying treatment to obtain graphene powder.
The graphene production method comprises the following steps of putting the cleaned crystalline flake graphite into a heating furnace for expansion treatment to obtain expanded crystalline flake graphite, and specifically comprises the following steps:
and (3) putting the cleaned crystalline flake graphene into a heating furnace, setting a high-temperature grade of 1200 ℃ at 1000-plus-one and a low-temperature grade of 150 ℃ at 100-plus-one, switching the temperature grade once every 30-60min, and repeatedly carrying out high-low temperature treatment for 2-3 times to obtain the expanded crystalline flake graphite.
The graphene production method comprises the step of preparing an intercalation agent, wherein the intercalation agent comprises 60-80% of hydrogen peroxide and 20-40% of a mixture formed by carbonate peroxide and a nonionic coupling agent.
The graphene production method comprises the steps of stirring at the vacuum stirring speed of 1000-1500r/min for 15-30 min.
The graphene production method is characterized in that the temperature of the cooling treatment is lower than 15 ℃.
The graphene production method comprises the following steps of 25-45% of ethylenediamine tetraacetic acid ammonia, 25-45% of propylenediamine tetrapotassium tetraacetate and 20-40% of water in percentage by weight.
Has the advantages that: the graphene production device provided by the invention comprises a first stirrer, a high-speed disperser, a cooling storage tank, a second stirrer, a reaction kettle, a horizontal screw centrifuge, a homogenizer and a drying agent which are sequentially communicated through a pipeline, and the device has the advantages of simple structure and low cost, and can realize large-scale industrial production of high-purity graphene with low energy consumption, no pollution and high efficiency.
Drawings
Fig. 1 is a schematic structural diagram of a preferred embodiment of a graphene production apparatus according to the present invention.
Fig. 2 is a flowchart of a preferred embodiment of a graphene production method according to the present invention.
Detailed Description
The invention provides a method and a device for producing graphene, and the invention is further described in detail below in order to make the purpose, the technical scheme and the effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, fig. 1 is a schematic structural diagram of a preferred embodiment of a graphene production apparatus according to the present invention, as shown in the figure, wherein the graphene production apparatus includes a first stirrer 10 for stirring flake graphite and an intercalating agent to generate a graphite mixture, a high-speed disperser 20 for dispersing the graphite mixture, a second stirrer 30 for stirring the graphite mixture and a reaction solution, a reaction kettle 40 for reacting the graphite mixture and the reaction solution to generate a graphene raw slurry, a cooling storage tank 50 for cooling the graphene raw slurry, a horizontal decanter centrifuge 60 for cleaning the cooled graphene raw slurry, a homogenizer 70 for dispersing the graphene raw slurry, and a dryer 80 for drying the graphene raw slurry to obtain a graphene powder, the first stirrer 10, the high-speed disperser 20, the second stirrer 30, the reaction kettle 40, the cooling storage tank 50, the horizontal decanter centrifuge 60, the homogenizer 70, and the dryer 80 are sequentially communicated through a pipeline.
The graphene production device in the embodiment has a simple structure and low cost; the graphene production device in the embodiment can realize large-scale industrial production of high-purity graphene with low energy consumption, no pollution and high efficiency.
Preferably, a water pump is provided on each pipe.
In a preferred embodiment, the device further comprises a heating furnace 11 for expanding the scale graphite, and the heating furnace is communicated with the first stirrer through a pipeline. The flake graphite is puffed by the heating furnace, so that the puffed flake graphite can easily permeate the intercalation agent.
In a preferred real-time mode, the device further comprises a cleaning machine 12 for cleaning the scale graphite, and the cleaning machine is communicated with the heating furnace through a pipeline. Through the cleaning machine washs scale graphite, clears away the various impurity of the inside, guarantees the purity of scale graphite, the graphite that the scale graphite was mined out for graphite ore is smashed the graphite product of screening out according to certain size, and corresponding graphite alkene product can be produced to the scale graphite of different sizes.
In a preferred embodiment, the first stirrer is a vacuum stirrer, and the expanded crystalline flake graphite and the intercalating agent are stirred in a vacuum state, so that the intercalating agent can be uniformly permeated into the expanded crystalline flake graphite, and subsequent reaction can be facilitated.
Based on the above apparatus, the present invention further provides a graphene production method, wherein as shown in fig. 2, the method includes the steps of:
s10, placing the cleaned crystalline flake graphite into a heating furnace for expansion treatment to obtain expanded crystalline flake graphite;
s20, putting the expanded crystalline flake graphite and the intercalation agent into a first stirrer for vacuum stirring, so that the intercalation agent uniformly permeates into the expanded crystalline flake graphite to obtain a graphite mixture;
s30, placing the graphite mixture into a high-speed dispersion machine for dispersion treatment;
s40, putting the graphite mixture subjected to the dispersion treatment and the reaction liquid into a second stirrer for stirring treatment;
s50, placing the stirred graphite mixture and the reaction liquid into a reaction kettle for full reaction to generate graphene raw stock;
s50, placing the graphene raw stock into a cooling storage tank for cooling treatment;
s70, placing the cooled graphene raw stock into a non-spiral centrifuge for centrifugal cleaning;
s80, placing the centrifuged graphene raw stock into a homogenizer for dispersion treatment;
and S90, placing the dispersed graphene raw stock into a dryer for drying treatment to obtain graphene powder.
In a preferred embodiment, the cleaned crystalline flake graphene is placed into a heating furnace, a high temperature range of 1000-. The embodiment utilizes the principle of expansion with heat and contraction with cold to repeatedly carry out high-low temperature treatment on the flake graphite, so that the flake graphite is puffed, and the subsequent intercalation agent is convenient to permeate.
Preferably, the switching time of the temperature gear can be adjusted according to the size of the flake graphite, and if the flake graphite is large in size, the interval time can be properly prolonged by 20%.
In a preferred embodiment, the expanded crystalline flake graphite and the intercalator are put into a first stirrer for vacuum stirring, the rotating speed of the vacuum stirring is 1000-1500r/min, the vacuum stirring time is 15-30min, and the intercalator is uniformly permeated into the expanded crystalline flake graphite under the stirring condition to obtain the graphite mixture.
Preferably, the intercalating agent comprises 60-80% of hydrogen peroxide and 20-40% of a mixture of carbonate peroxide and a nonionic coupling agent. The reaction liquid comprises 25-45% of ethylenediamine tetraacetic acid ammonia, 25-45% of propylenediamine tetra-potassium acetate and 20-40% of water in percentage by weight.
Specifically, the flake graphite can be regarded as formed by stacking single-layer graphene together through van der waals force between layers, the intercalator serving as a small molecular reagent can be uniformly inserted into gaps between the layers of the flake graphite, after a reaction liquid is added, the reaction liquid serving as another chemical reagent with a smaller molecular structure can also be inserted into the gaps between the layers of the flake graphite, and when the reaction liquid is contacted with the intercalator, a chemical reaction can be generated so that the single-layer graphene in the flake graphite overcomes the van der waals force between the layers, and then the single-layer graphene is separated from the flake graphite to form the graphene sheet.
In a preferred embodiment, the flake graphite mixture mixed with the intercalation agent is extracted and placed in a high-speed disperser for dispersion intercalation.
In a preferred embodiment, the flake graphite mixture with the intercalation agent is extracted from the cooling storage tank into the second stirrer, and the reaction solution is added to the second stirrer, stirred for about 5 minutes, and then placed into the reaction kettle. After the reaction liquid and the graphite mixture are fully reacted, the generated graphene raw stock floats on the surface of the reaction kettle, impurities are dissolved in water or sink to the water bottom, the reaction liquid containing the impurities at the lower part of the reaction kettle is discharged, and the remaining graphene raw stock is obtained.
Further, the dispersed crystalline flake graphite mixture is pumped into a cooling storage tank for cooling storage, and the temperature of the cooling treatment is preferably lower than 15 ℃. Because the intercalation agent and the reaction liquid are subjected to chemical reaction, force is generated, heat is also generated, and the overall temperature of the reaction system is increased. Since a single graphene sheet is very small, it moves violently at high temperatures and, in some cases, may stick to other graphene sheets. For this reason, the present invention must reduce the temperature after the reaction, thereby reducing the chance of the graphene sheets re-polymerizing together.
In a preferred embodiment, the graphene raw stock is extracted from the reaction kettle and is cleaned by a horizontal screw centrifuge, so that impurities in the graphene raw stock are further removed, and the purity of the graphene is further improved. And dispersing the cleaned graphene raw stock by using a homogenizer, and finally drying the dispersed graphene raw stock by using a heating dryer or a spray dryer to obtain the most graphene powder.
In summary, the graphene production device provided by the invention comprises a first stirrer, a high-speed disperser, a second stirrer, a reaction kettle, a cooling storage tank, a horizontal screw centrifuge, a homogenizer and a drying agent which are sequentially communicated through a pipeline, and the device has the advantages of simple structure, low cost and capability of realizing large-scale industrial production of high-purity graphene with low energy consumption, no pollution and high efficiency.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (3)
1. The utility model provides a graphite alkene production method based on graphite alkene apparatus for producing, a serial communication port, graphite alkene apparatus for producing is including being used for stirring the first mixer that generates graphite mixture with scale graphite and intercalant, be used for with graphite mixture carries out the high speed dispersion machine that disperses, be used for with graphite mixture and reaction liquid carry out the second mixer that stirs, be used for making graphite mixture and reaction liquid react and generate the reation kettle of graphite alkene magma, be used for with graphite alkene magma carries out refrigerated cooling storage tank, be used for right the graphite alkene magma after the cooling treatment carries out abluent horizontal decanter centrifuge, be used for right the homogenizer that graphite alkene magma disperses and be used for right the desiccator that graphite alkene magma carries out the drying and obtains the graphite alkene powder, first mixer, high speed dispersion machine, second mixer, reation kettle, The cooling storage tank, the horizontal screw centrifuge, the homogenizer and the dryer are communicated in sequence through pipelines; the graphene production method comprises the following steps:
placing the cleaned crystalline flake graphite into a heating furnace for expansion treatment, setting a high-temperature grade of 1000-plus-one at 1200 ℃ and a low-temperature grade of 100-plus-one at 150 ℃, switching the temperature grade once every 30-60min, and repeatedly performing high-low temperature treatment for 2-3 times to obtain expanded crystalline flake graphite;
putting the expanded crystalline flake graphite and an intercalator into a first stirrer for vacuum stirring, so that the intercalator uniformly permeates into the expanded crystalline flake graphite to obtain a graphite mixture, wherein the intercalator comprises 60-80% of hydrogen peroxide and 20-40% of a mixture formed by carbonate peroxide and a nonionic couplant, the vacuum stirring speed is 1000-1500r/min, and the vacuum stirring time is 15-30 min;
putting the graphite mixture into a high-speed disperser for dispersing treatment;
placing the graphite mixture subjected to dispersion treatment and reaction liquid into a second stirrer for stirring treatment, wherein the reaction liquid comprises 25-45% of ammonium ethylenediamine tetraacetate, 25-45% of potassium propylenediamine tetraacetate and 20-40% of water in percentage by weight;
placing the stirred graphite mixture and the reaction liquid into a reaction kettle for full reaction, after the reaction liquid and the graphite mixture are fully reacted, floating the generated graphene raw stock on the surface of the reaction kettle, dissolving impurities into water or sinking to the bottom of the water, discharging the reaction liquid containing the impurities at the lower part of the reaction kettle, and obtaining the remaining graphene raw stock;
putting the graphene raw stock into a cooling storage tank for cooling treatment, wherein the temperature of the cooling treatment is lower than 15 ℃;
placing the cooled graphene raw stock into a horizontal screw centrifuge for centrifugal cleaning;
placing the centrifuged graphene raw stock into a homogenizer for dispersion treatment;
and (4) putting the dispersed graphene raw stock into a dryer for drying treatment to obtain graphene powder.
2. The graphene production method according to claim 1, wherein the graphene production apparatus further comprises a heating furnace for puffing crystalline flake graphite, and the heating furnace is communicated with the first stirrer through a pipeline.
3. The graphene production method according to claim 2, wherein the graphene production apparatus further comprises a cleaning machine for cleaning scale graphite, and the cleaning machine is communicated with the heating furnace through a pipeline.
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| IT201800010845A1 (en) * | 2018-12-05 | 2020-06-05 | Gea Mech Equipment Italia S P A | HIGH PRESSURE HOMOGENIZING VALVE AND PRODUCTION PROCESS OF CARBON-BASED NANOSTRUCTURED MATERIALS, IN PARTICULAR GRAPHENE AND CARBON NANOTUBES |
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