CN108862259A - A kind of graphene production method and device - Google Patents
A kind of graphene production method and device Download PDFInfo
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- CN108862259A CN108862259A CN201810917889.8A CN201810917889A CN108862259A CN 108862259 A CN108862259 A CN 108862259A CN 201810917889 A CN201810917889 A CN 201810917889A CN 108862259 A CN108862259 A CN 108862259A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
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- C01B32/19—Preparation by exfoliation
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Abstract
The invention discloses a kind of graphene production method and devices, wherein, the graphene process units includes the first blender being sequentially communicated by pipeline, high speed disperser, the second blender, reaction kettle, cooling holding vessel, decanter centrifuge, homogenizer and desiccant, described device is of simple structure and low cost, and can realize low energy consumption, pollution-free, high efficiency large-scale industrial production high purity graphite alkene.
Description
Technical field
The present invention relates to field of preparation of graphene more particularly to a kind of graphene production method and devices.
Background technique
Graphene (Graphene) is a kind of two dimension for forming hexangle type in honeycomb lattice with sp2 hybridized orbit by carbon atom
Carbon nanomaterial.Graphene has excellent optics, electricity, mechanical characteristic, in materialogy, micro-nano technology, the energy, biomedicine
It is with important application prospects with drug delivery etc., it is considered to be a kind of future revolutionary material.Manchester, England
College Physics scholar An Deliegaimu and Constantine's Nuo Woxiao love are separated from graphite with micromechanics stripping method success
Graphene out, therefore Nobel Prize in physics in 2010 is obtained jointly.
The method of the common power production of graphene includes mechanical stripping method, oxidation-reduction method and SiC epitaxial growth etc.
Method, however these methods can typically be only used to laboratory small lot manufacture, can not extensive, industrialized production, immediately
It produces, also contains a large amount of impurity, it is difficult to use.That there is also energy losses is big for the above method, and easily causes environment dirty
The problems such as dye.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of graphene production method and device,
Aim at low energy consumption, pollution-free, high efficiency large-scale industrial production high purity graphite alkene purpose.
Technical scheme is as follows：
A kind of graphene process units, wherein including for crystalline flake graphite and intercalator to be stirred generation graphite mixture
The first blender, the high speed disperser for dispersing the graphite mixture is cold for carrying out graphite mixture
But cooling holding vessel, the second blender for the graphite mixture and reaction solution to be stirred, for keeping graphite mixed
It closes object and reaction solution carries out the reaction kettle that reaction generates graphene magma, the sleeping spiral shell for being cleaned to the graphene magma
Centrifuge, homogenizer for being dispersed to the graphene magma and for the graphene magma to be dried
To the drying machine of graphene pulvis, first blender, high speed disperser, cooling holding vessel, the second blender, reaction kettle,
Decanter centrifuge, homogenizer and drying machine pass sequentially through pipeline connection.
The graphene process units, wherein further include the heating furnace for carrying out expanding treatment to crystalline flake graphite, institute
Heating furnace is stated to be connected to by pipeline with first blender.
The graphene process units, wherein further include the cleaning machine for being started the cleaning processing to crystalline flake graphite, institute
Cleaning machine is stated to be connected to by pipeline with the heating furnace.
The graphene process units, wherein first blender is de-airing mixer.
A kind of graphene production method, wherein including step：
Crystalline flake graphite after cleaning is put into heating furnace and carries out expansion process, obtains the crystalline flake graphite of extruding；
The crystalline flake graphite of the extruding and intercalator are put into the first blender and are stirred under vacuum, intercalator uniformly penetrating is made
Graphite mixture is obtained into the crystalline flake graphite of the extruding；
The graphite mixture is put into high speed disperser and carries out decentralized processing；
Graphite mixture after the progress decentralized processing is put into cooling storage tank and carries out cooling treatment；
Graphite mixture after cooling treatment is put into the second blender with reaction solution and is stirred；
Graphite mixture after stir process is put into reaction kettle with reaction solution and is sufficiently reacted, graphene magma is generated；
The graphene magma is put into progress eccentric cleaning processing in no screw centrifuge；
Graphene magma after centrifugal treating is put into homogenizer and carries out decentralized processing；
Graphene magma after decentralized processing is put into drying machine and is dried, graphene pulvis is obtained.
The graphene production method, wherein the step crystalline flake graphite after cleaning is put into heating furnace carry out it is swollen
Swollen processing obtains the crystalline flake graphite of extruding, specifically includes：
The crystalline flake graphite alkene cleaned up is put into heating furnace, 1000-1200 DEG C of high temperature shelves and 100-150 DEG C of low temperature are set
Shelves switch a temperature gear every 30-60min, and high/low temperature handles 2-3 times and obtains the crystalline flake graphite of extruding repeatedly.
The graphene production method, wherein the intercalator includes the hydrogen peroxide of 60-80% and the peroxide of 20-40%
Change the mixture that carbonate and nonionic couplant are formed.
The graphene production method, wherein the revolving speed of the vacuum stirring is 1000-1500r/min, when vacuum stirring
Between be 15-30min.
The graphene production method, wherein the temperature of the cooling treatment is lower than 15 DEG C.
The graphene production method, wherein the reaction solution includes the ethylenediamine tetraacetic of 25-45% by weight percentage
Acetic acid ammonia, the trimethylen-edinitrilo-tetraacetic acid potassium of 25-45% and the water of 20-40%.
Beneficial effect：Graphene process units provided by the invention include the first blender being sequentially communicated by pipeline,
High speed disperser, cooling holding vessel, the second blender, reaction kettle, decanter centrifuge, homogenizer and desiccant, described device
It is of simple structure and low cost, and can realize low energy consumption, pollution-free, high efficiency large-scale industrial production high purity graphite alkene.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of graphene process units preferred embodiment of the present invention.
Fig. 2 is a kind of flow chart of graphene production method preferred embodiment of the present invention.
Specific embodiment
The present invention provides a kind of graphene production method and devices, to make the purpose of the present invention, technical solution and effect
Clearer, clear, the present invention is described in more detail below.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
Referring to Fig. 1, Fig. 1 is a kind of structural schematic diagram of graphene process units preferred embodiment of the present invention, as schemed institute
Show, wherein the graphene process units includes generating graphite mixture for crystalline flake graphite and intercalator to be stirred
First blender 10, the high speed disperser 20 for dispersing the graphite mixture are used for the graphite mixture
The second blender 30 being stirred with reaction solution generates graphene magma for making graphite mixture and reaction solution carry out reaction
Reaction kettle 40, for the graphene magma to be carried out to cooling cooling holding vessel 50, after to the cooling treatment
The decanter centrifuge 60 that graphene magma is cleaned, homogenizer 70 and use for being dispersed to the graphene magma
In the graphene magma is dried to obtain the drying machine 80 of graphene pulvis, first blender 10, high speed dispersion
Machine 20, the second blender 30, reaction kettle 40, cooling holding vessel 50, decanter centrifuge 60, homogenizer 70 and drying machine 80 are successively
It is connected to by pipeline.
Graphene process units in the present embodiment is of simple structure and low cost；Graphene in through this embodiment is raw
Low energy consumption, pollution-free, high efficiency large-scale industrial production high purity graphite alkene can be realized by producing device.
Preferably, a water pump is provided on each root canal road.
In a preferred embodiment, described device further includes the heating for carrying out expanding treatment to crystalline flake graphite
Furnace 11, the heating furnace are connected to by pipeline with first blender.Extruding is carried out to crystalline flake graphite by the heating furnace
Processing, so that the crystalline flake graphite after extruding is easier to permeate intercalator.
In a kind of preferred real-time mode, described device further includes the cleaning for starting the cleaning processing to crystalline flake graphite
Machine 12, the cleaning machine are connected to by pipeline with the heating furnace.Crystalline flake graphite is cleaned by the cleaning machine, is removed
The various impurity of the inside guarantee the purity of crystalline flake graphite, and the crystalline flake graphite is the mined graphite of graphite ore, by a scale
Very little to smash the graphite products screened, various sizes of crystalline flake graphite can produce corresponding graphene product.
In a preferred embodiment, first blender is de-airing mixer, by stirring under vacuum conditions
The crystalline flake graphite and intercalator for mixing the extruding are more advantageous to the crystalline flake graphite that the intercalator equably penetrates into the extruding
In, it is convenient for subsequent reactions.
Based on above-mentioned apparatus, the present invention also provides a kind of graphene production methods, wherein as shown in Fig. 2, including step：
S10, it the crystalline flake graphite after cleaning is put into heating furnace carries out expansion process, obtain the crystalline flake graphite of extruding；
S20, it the crystalline flake graphite of the extruding and intercalator is put into the first blender is stirred under vacuum, keep intercalator uniform
It penetrates into the crystalline flake graphite of the extruding and obtains graphite mixture；
S30, it the graphite mixture is put into high speed disperser carries out decentralized processing；
S40, by it is described progress decentralized processing after graphite mixture and reaction solution be put into the second blender and be stirred；
S50, the graphite mixture after stir process is put into reaction kettle with reaction solution and is sufficiently reacted, it is former to generate graphene
Slurry；
S50, it the graphene magma is put into cooling storage tank carries out cooling treatment；
S70, the graphene magma after the cooling treatment is put into progress eccentric cleaning processing in no screw centrifuge；
S80, it the graphene magma after centrifugal treating is put into homogenizer carries out decentralized processing；
S90, it the graphene magma after decentralized processing is put into drying machine is dried, obtain graphene pulvis.
In a preferred embodiment, the crystalline flake graphite alkene cleaned up is put into heating furnace, sets 1000-
1200 DEG C of high temperature shelves and 100-150 DEG C of low temperature shelves switch a temperature gear every 30-60min, and high/low temperature handles 2- repeatedly
Obtain the crystalline flake graphite of extruding 3 times.The present embodiment carries out at high/low temperature repeatedly crystalline flake graphite using the principle expanded with heat and contract with cold
Reason makes the crystalline flake graphite that extruding occur, facilitates the infiltration of subsequent intercalator.
Preferably, the switching time of the temperature gear can be adjusted according to the size of crystalline flake graphite, if crystalline flake graphite
Size is larger, interval time can will be appropriately extended 20%.
In a preferred embodiment, by the crystalline flake graphite of the extruding and intercalator be put into the first blender into
Row is stirred under vacuum, and the revolving speed of the vacuum stirring is 1000-1500r/min, and the vacuum stirring time is 15-30min, in the stirring
Under the conditions of so that intercalator uniformly penetrating is obtained graphite mixture into the crystalline flake graphite of the extruding.
Preferably, the intercalator includes the hydrogen peroxide of 60-80% and the peroxycarbonate of 20-40% and nonionic coupling
The mixture that mixture is formed.The reaction solution includes the ethylenediamine tetra-acetic acid ammonia of 25-45% by weight percentage, 25-45%'s
The water of trimethylen-edinitrilo-tetraacetic acid potassium and 20-40%.
Specifically, the crystalline flake graphite, which can be regarded as, passes through Van der Waals force heap between layers by single-layer graphene
What product was formed together, the intercalator can be equably inserted into the gap of crystalline flake graphite between layers as small organic agents
Face, after reaction solution to be added, the reaction solution can also be punctured into described as another lesser chemical reagent of molecular structure
In the gap of crystalline flake graphite between layers, chemical reaction can occur when the reaction solution and the intercalator contact so that
Single-layer graphene in crystalline flake graphite overcomes Van der Waals force between layers, to detach to form stone from crystalline flake graphite
Black alkene piece.
In a preferred embodiment, the crystalline flake graphite mixture for being mixed with intercalator is extracted and is placed on high speed point
It dissipates in machine and carries out dispersion intercalation.
In a preferred embodiment, the crystalline flake graphite mixture for being mixed with intercalator will be extracted in cooling holding vessel
It into second blender, and is added after reaction solution carries out stirring in 5 minutes or so, is put into reaction kettle.To reaction solution and stone
After black mixture sufficiently reacts, the graphene magma of generation then swims in the surface of reaction kettle, and impurity then incorporates in water or heavy
Enter the bottom, bleed off the impure reaction solution in reaction kettle lower part, then remaining is exactly graphene magma.
Further, the crystalline flake graphite mixture that dispersion is completed is extracted into cooling holding vessel and carries out cooling storage, preferably
, the temperature of the cooling treatment is lower than 15 DEG C.Because intercalator and reaction solution chemically react, while producing power,
Also heat can be generated, reaction system bulk temperature can increase.Since single-layer graphene film is very small, can acutely be transported when temperature is high
It is dynamic, in some cases, and it may be bonded together with other graphene films.For this purpose, the present invention has to reduce after the reaction
Temperature, to reduce the probability that graphene film regroups together.
In a preferred embodiment, graphene magma will be extracted out from reaction kettle, carried out clearly with decanter centrifuge
It washes, further removes the impurity inside graphene magma, further increase the purity of graphene.It is used later with homogenizer pair
The graphene magma cleaned is dispersed, finally with heat drying machine or spray dryer to the graphene magma after dispersion
It is dried, obtains most graphene pulvis.
In conclusion graphene process units provided by the invention include the first blender being sequentially communicated by pipeline,
High speed disperser, the second blender, reaction kettle, cooling holding vessel, decanter centrifuge, homogenizer and desiccant, described device
It is of simple structure and low cost, and can realize low energy consumption, pollution-free, high efficiency large-scale industrial production high purity graphite alkene.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of graphene process units, which is characterized in that including for crystalline flake graphite and intercalator to be stirred generation stone
First blender of black mixture, the high speed disperser for dispersing the graphite mixture are used for the graphite
The second blender that mixture and reaction solution are stirred generates graphene for making graphite mixture and reaction solution carry out reaction
The reaction kettle of magma, for the graphene magma to be carried out to cooling cooling holding vessel, after to the cooling treatment
The decanter centrifuge that graphene magma is cleaned, homogenizer for being dispersed to the graphene magma and for pair
The graphene magma is dried to obtain the drying machine of graphene pulvis, and first blender, high speed disperser, second stir
It mixes machine, reaction kettle, cooling holding vessel, decanter centrifuge, homogenizer and drying machine and passes sequentially through pipeline connection.
2. graphene process units according to claim 1, which is characterized in that further include swollen for being carried out to crystalline flake graphite
Change the heating furnace of processing, the heating furnace is connected to by pipeline with first blender.
3. graphene process units according to claim 2, which is characterized in that further include clear for being carried out to crystalline flake graphite
The cleaning machine of processing is washed, the cleaning machine is connected to by pipeline with the heating furnace.
4. according to right to go 1 described in graphene process units, which is characterized in that first blender be stirred under vacuum
Machine.
5. a kind of graphene production method, which is characterized in that including step：
Crystalline flake graphite after cleaning is put into heating furnace and carries out expansion process, obtains the crystalline flake graphite of extruding；
The crystalline flake graphite of the extruding and intercalator are put into the first blender and are stirred under vacuum, intercalator uniformly penetrating is made
Graphite mixture is obtained into the crystalline flake graphite of the extruding；
The graphite mixture is put into high speed disperser and carries out decentralized processing；
Graphite mixture after the progress decentralized processing is put into the second blender with reaction solution and is stirred；
Graphite mixture after stir process is put into reaction kettle with reaction solution and is sufficiently reacted, graphene magma is generated；
The graphene magma is put into cooling storage tank and carries out cooling treatment；
Graphene magma after the cooling treatment is put into progress eccentric cleaning processing in no screw centrifuge；
Graphene magma after centrifugal treating is put into homogenizer and carries out decentralized processing；
Graphene magma after decentralized processing is put into drying machine and is dried, graphene pulvis is obtained.
6. graphene production method according to claim 5, which is characterized in that the step puts the crystalline flake graphite after cleaning
Enter and carry out expansion process in heating furnace, obtains the crystalline flake graphite of extruding, specifically include：
The crystalline flake graphite alkene cleaned up is put into heating furnace, 1000-1200 DEG C of high temperature shelves and 100-150 DEG C of low temperature are set
Shelves switch a temperature gear every 30-60min, and high/low temperature handles 2-3 times and obtains the crystalline flake graphite of extruding repeatedly.
7. graphene production method according to claim 5, which is characterized in that the intercalator includes the hydrogen peroxide of 60-80%
And the mixture that the peroxycarbonate and nonionic couplant of 20-40% is formed.
8. graphene production method according to claim 5, which is characterized in that the revolving speed of the vacuum stirring is 1000-
1500r/min, vacuum stirring time are 15-30min.
9. graphene production method according to claim 5, which is characterized in that the temperature of the cooling treatment is lower than 15 DEG C.
10. graphene production method according to claim 5, which is characterized in that the reaction solution wraps by weight percentage
Include the ethylenediamine tetra-acetic acid ammonia of 25-45%, the trimethylen-edinitrilo-tetraacetic acid potassium of 25-45% and the water of 20-40%.
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Cited By (2)
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| CN110127677A (en) * | 2019-05-05 | 2019-08-16 | 陈让珠 | Water body graphene slurry production method |
| 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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