CN106044764A - Apparatus and method of supercritically preparing graphene - Google Patents
Apparatus and method of supercritically preparing graphene Download PDFInfo
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- CN106044764A CN106044764A CN201610679367.XA CN201610679367A CN106044764A CN 106044764 A CN106044764 A CN 106044764A CN 201610679367 A CN201610679367 A CN 201610679367A CN 106044764 A CN106044764 A CN 106044764A
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Abstract
The invention provides an apparatus and a method of supercritically preparing graphene, wherein the apparatus includes a reaction apparatus, a supporting mechanism, a heating apparatus, a quenching apparatus and a guide rail. The reaction apparatus is connected to the supporting mechanism. The guide rail is arranged under the reaction apparatus. The heating apparatus and the quenching apparatus are both slidingly connected to the guide rail and can alternately slide to below the reaction apparatus along the guide rail. In the apparatus, a physical reaction can be fully carried out between an organic solvent and a carbon raw material so as to reduce intermolecular force of the carbon raw material and increase the layer-to-layer distance of the carbon raw material. The quenching apparatus then cools the organic solvent and the carbon raw material after the physical reaction, so that the intermolecular force of the carbon raw material is damaged as most as possible through the cold-hot alternate stimulation on the organic solvent and the carbon raw material. The apparatus and the method increase yield of graphene, ensure quality of the graphene and are low in cost.
Description
Technical field
The present invention relates to technical field of graphene preparation, prepare the device of Graphene in particular to a kind of supercritical
And method.
Background technology
Graphene is a kind of bi-dimensional cellular shape lattice structure carbonaceous material tightly packed by monolayer carbon atom.Although
Graphene only has the thickness of one layer of carbon atomic layer, but Graphene is the thinnest material being currently known, and is also the most tough material
Material, and, Graphene also has the most elastic and good electric conductivity, and therefore, Graphene is in electronics, optics, magnetics, life
The aspects such as thing medical science, sensor, energy storage are all widely used.
At present, the preparation method that Graphene is conventional includes: mechanical stripping method, oxidation-reduction method, epitaxial growth method and chemistry
Vapour deposition process.Wherein, the Graphene that mechanical stripping method is prepared generally remains complete crystal structure, but lamella is little,
Production efficiency is low.Although the yield of oxidation-reduction method Graphene is high, but quality is relatively low.Although epitaxial growth method is obtained in that height
The Graphene of quality, but the requirement to equipment is higher.Vapour deposition process has the advantages that the quality of Graphene is high, but cost
Height, process conditions also need the most perfect.Therefore, Graphene uses supercritical process to be prepared more, wherein supercritical
CO2Method application is the most extensive, but cost is high, productivity is low.
Summary of the invention
In consideration of it, the present invention proposes a kind of supercritical prepares the device of Graphene, it is intended to solve prior art uses
Supercritical CO2Method is prepared Graphene and is caused the problem that cost is high, productivity is low.The invention allows for a kind of supercritical and prepare graphite
The method of alkene.
One aspect, the present invention proposes a kind of supercritical and prepares the device of Graphene, and this device includes: reaction unit,
Supporting mechanism, heater, quenching device and guide rail；Wherein, reaction unit is connected to supporting mechanism；Guide rail is placed in reaction unit
Lower section, heater and quenching device be all slidably connected to guide rail, and, heater and quenching device are alternately
The lower section of reaction unit is slided to along guide rail.
Further, above-mentioned supercritical is prepared in the device of Graphene, and heater includes: heater body and first stretches
Bar；Wherein, one end of the first expansion link is connected with slide, and the other end of the first expansion link is connected with heater body.
Further, above-mentioned supercritical is prepared in the device of Graphene, and heater body is the heating mantle of one end open.
Further, above-mentioned supercritical is prepared in the device of Graphene, and quenching device includes: quenching body and second stretches
Bar；Wherein, the first end of the second expansion link is connected with slide, and the second end of the second expansion link is connected with quenching body；
Quenching body is used for cooling down reaction unit.
Further, above-mentioned supercritical is prepared in the device of Graphene, and quenching body includes: staving and coolant；Wherein,
Second end of staving and the second expansion link is connected, and coolant is placed in staving.
Further, above-mentioned supercritical is prepared in the device of Graphene, and reaction unit is provided with for monitoring internal temperature
Thermometer.
Further, above-mentioned supercritical is prepared in the device of Graphene, and reaction unit is provided with for monitoring internal pressure
Pressure gauge.
In the present invention, by heater, the organic solvent in reaction unit and carbon raw material are heated so that have
Machine solvent and carbon raw material can fully occur physical reactions, and the intermolecular force of carbon raw material weakens, and increases carbonaceous former
The interfloor distance of material, then by quenching device, the organic solvent after having occurred and that physical reactions and carbon raw material are cooled down,
So cold and heat succeed each other stimulation organic solvent and carbon raw material, it is possible to farthest destroys the intermolecular force of carbon raw material,
Improve the productivity of Graphene, and ensure that the quality of Graphene, with low cost, solve employing supercritical in prior art
CO2Method is prepared Graphene and is caused the problem that cost is high, productivity is low.
On the other hand, the invention allows for a kind of utilizing above-mentioned preparation facilities to carry out supercritical to prepare the side that graphite is dilute
Method, the method comprises the steps: charging: put into organic solvent and carbon raw material in the reaction unit in preparation facilities；Add
Heat: the heater in preparation facilities is placed in the lower section of reaction unit, and reaction unit is heated by heater, until reaching
To preset temperature；Quenching: after organic solvent and carbon raw material reaction reached for the first response time, remove heater, and will
Quenching device is placed in below reaction unit and it is carried out quenching, until it reaches after the second response time, remove quenching device；Repeat
Above-mentioned heating steps and quenching step, until it is dilute to obtain graphite.
Further, above-mentioned supercritical is prepared in the method that graphite is dilute, and the water content in organic solvent is 70%～99%.
Further, above-mentioned supercritical is prepared in the method that graphite is dilute, and preset temperature is 250 DEG C～650 DEG C, the first reaction
Time is 20-50min, and the second response time was 20-50min.
In the present invention, by heating steps, the organic solvent in reaction unit and carbon raw material are heated so that have
Machine solvent and carbon raw material can fully occur physical reactions, and the intermolecular force of carbon raw material weakens, and increases carbonaceous former
Material interfloor distance, and, the water in organic solvent can preferably dissolve each other with organic solvent under preset temperature, water with
Organic solvent infiltrates into the sheet interlayer of carbon raw material, preferably destroys the molecular link of carbon raw material, further increases carbonaceous former
The interfloor distance of material；By quenching step, the organic solvent after having occurred and that physical reactions and carbon raw material are cooled down again,
So cold and heat succeed each other stimulation organic solvent and carbon raw material, it is possible to farthest destroys the intermolecular force of carbon raw material,
It is easy to the later separation of Graphene, improves the productivity of Graphene, and ensure that the quality of Graphene, with low cost.
Accompanying drawing explanation
By reading the detailed description of hereafter preferred implementation, various other advantage and benefit common for this area
Technical staff will be clear from understanding.Accompanying drawing is only used for illustrating the purpose of preferred implementation, and is not considered as the present invention
Restriction.And in whole accompanying drawing, it is denoted by the same reference numerals identical parts.In the accompanying drawings:
Fig. 1 prepares the structural representation of the device of Graphene for the supercritical that the embodiment of the present invention provides；
Fig. 2 utilizes above-mentioned preparation facilities to carry out supercritical to prepare the stream of the dilute method of graphite for what the embodiment of the present invention provided
Cheng Tu.
Detailed description of the invention
It is more fully described the exemplary embodiment of the disclosure below with reference to accompanying drawings.Although accompanying drawing shows the disclosure
Exemplary embodiment, it being understood, however, that may be realized in various forms the disclosure and should be by embodiments set forth here
Limited.On the contrary, it is provided that these embodiments are able to be best understood from the disclosure, and can be by the scope of the present disclosure
Complete conveys to those skilled in the art.It should be noted that in the case of not conflicting, embodiment in the present invention and
Feature in embodiment can be mutually combined.Describe the present invention below with reference to the accompanying drawings and in conjunction with the embodiments in detail.
Supercritical prepares the device embodiment of Graphene:
See the structural representation that Fig. 1, Fig. 1 prepare the device of Graphene for the supercritical that the embodiment of the present invention provides.As
Shown in figure, this supercritical is prepared the device of Graphene and is included: reaction unit 1, supporting mechanism 2, heater 3, quenching device 4 and
Guide rail 5.Wherein, reaction unit 1 is connected to supporting mechanism 2, and guide rail 5 is arranged at the lower section of reaction unit 1, heater 3 and quenching
Device for cooling 4 is all slidably connected to guide rail 5, and, heater 3 and quenching device 4 alternately slide into instead along guide rail 5
Answer the lower section of device 1.Specifically, having preset height between reaction unit 1 and guide rail 5, this preset height can be according to circumstances
Determining, this is not done any restriction by the present embodiment.Reaction unit 1 can include that reactor 11 and conjunction of can uncapping are connected to reaction
The lid 12 of device.Organic solvent can be ethanol, NMP, surfactant etc., and this organic solvent can be single organic solvent,
It can also be the mixture of several organic solvent.Carbon raw material can be graphite, coal etc..
Supporting mechanism 2 may include that gripper shoe 21 and at least two support bar 22.Wherein, each support bar 22 all with support
Plate 21 is connected so that have preset height between gripper shoe 21 and guide rail 5.Gripper shoe 21 is provided with opening, and reaction unit 1 is worn
It is located at opening and is connected with gripper shoe 21.Specifically, reaction unit 1 and gripper shoe 21 are for removably connecting, say, that anti-
Answer device 1 can be taken off by gripper shoe 21.When being embodied as, the outer wall of reaction unit 1 is provided with a block piece 13, reaction unit 1
Being set up in gripper shoe 21 by a block piece 13, such reaction unit 1 and gripper shoe 21 are by 13 shelves of block piece, it is simple to reaction dress
Put 1 to take off and install.
During preparation, organic solvent and carbon raw material being put in reaction unit 1, organic solvent and carbon raw material mix
Close.Heater 3 slides into the lower section of reaction unit 1, and heats reaction unit 1 so that the temperature in reaction unit 1
Reaching preset temperature, this preset temperature disclosure satisfy that super critical condition.Owing in reaction unit 1, temperature raises, so reaction dress
The pressure put in 1 also increases.When the temperature in reaction unit 1 reaches preset temperature, it is former that organic solvent infiltrates into carbonaceous
The sheet interlayer of material, the intermolecular force of carbon raw material weakens so that the interfloor distance of carbon raw material increases.At organic solvent and
After carbon raw material reaction reached for the first response time, heater 3 is slid into side by guide rail 5, quenching device 4 is slided
To the lower section of reaction unit 1, reaction unit 1 is cooled down by quenching device 4, owing to the temperature in reaction unit 1 is the highest, so
When reaction unit 1 is cooled down by quenching device 4, the temperature of reaction unit 1 reduces, and colding and heat succeed each other, it is former to destroy carbonaceous further
The intermolecular force of material.It was cooled to for the second response time, then quenching device 4 is slid into side, heater 3 is slid into
The lower section of reaction unit 1, continues to heat reaction unit 1, repeats the step of above-mentioned heating and quenching, finally give graphite
Alkene.
During it should be noted that be embodied as, preset temperature can be 250 DEG C～650 DEG C, it is also possible to according to practical situation
Determining, this is not done any restriction by the present embodiment.Pressure in reaction unit 1 can be 21MPa～30MPa, it is also possible to real
Border according to circumstances determines, this is not done any restriction by the present embodiment.First response time can be 20-50min, the second reaction
Time can be 20-50min.When being embodied as, the first response time and the second response time can also come according to practical situation
Determining, this is not done any restriction by the present embodiment.
It should be appreciated by those skilled in the art that the Graphene that above-mentioned reaction unit 1 obtains is crude product Graphene, crude product graphite
Alkene proceeds to separate and just can obtain Graphene.
It can be seen that in the present embodiment, the organic solvent in reaction unit 1 and carbon raw material are entered by heater 3
Row heating so that organic solvent and carbon raw material can fully occur physical reactions, and the intermolecular force of carbon raw material weakens,
Increase the interfloor distance of carbon raw material, then by quenching device 4 to having occurred and that the organic solvent after physical reactions and carbonaceous
Raw material cools down, and so cold and heat succeed each other stimulation organic solvent and carbon raw material, it is possible to farthest destroy carbon raw material
Intermolecular force, improves the productivity of Graphene, and ensure that the quality of Graphene, with low cost, solves existing skill
Art uses supercritical CO2Method is prepared Graphene and is caused the problem that cost is high, productivity is low.
With continued reference to Fig. 1, in above-described embodiment, heater 3 may include that heater body 31 and the first expansion link 32.
Wherein, one end of the first expansion link 32 is slidably connected with guide rail 5, and the other end of the first expansion link 32 is connected with heater body 31
Connect.Preferably, heater body 31 is the heating mantle of one end open, and heating mantle is sheathed on the outside of reaction unit 1.First expansion link
One end of 32 is connected with guide rail 5 and can slide along guide rail 5, and the other end of the first expansion link 32 is connected with heating mantle.Specifically
During enforcement, heating mantle can be electric heating cover.First expansion link 32 can be electric expansion bar, hydraulically extensible bar etc., it is also possible to
For being capable of lifting other structures of heater body 31, this is not done any restriction by the present embodiment.
First expansion link 32 is used for lifting heating mantle, when the first expansion link 32 is raised above so that heating mantle is sheathed on reaction
During device 1 outside, reaction unit 1 is heated by heating mantle.When heating reaches preset temperature and reaches the first reaction
After between, the first expansion link 32 falls downward makes heating mantle depart from the outside of reaction unit 1, and heating mantle stops reaction unit 1
Heating, the first expansion link 32 drives heating mantle to remove the lower section of reaction unit 1 together, and quenching device 4 is slid into reaction
Below device 1, reaction unit 1 is cooled down by quenching device 4.
It can be seen that in the present embodiment, lift heater body 31 by the first expansion link 32 so that heater body 31 is permissible
According to actual needs reaction unit 1 is heated, and the first expansion link 32 is slidably connected to guide rail 5 so that first
Expansion link 32 can be in the slid underneath of reaction unit 1, and heater body 31 is sliding in the lower section of reaction unit 1 with the first expansion link 32
Dynamic, it is simple to heater body 31 removes the lower section of reaction unit 1, and then be easy to quenching device 4 and slide into the lower section of reaction unit 1 also
Reaction unit 1 is cooled down, simple in construction, it is easy to implement.
With continued reference to Fig. 1, in the various embodiments described above, quenching device 4 may include that quenching body 41 and the second expansion link
42.Wherein, the first end of the second expansion link 42 is slidably connected with guide rail 5, the second end of the second expansion link 42 and quenching body 41
Being connected, quenching body 41 is used for cooling down reaction unit 1.Specifically, the first end of the second expansion link 42 be connected with guide rail 5 and
Can slide along guide rail 5.When being embodied as, the second expansion link 42 can be electric expansion bar, hydraulically extensible bar etc., it is also possible to for energy
Enough other structures realizing lifting quenching body 41, this is not done any restriction by the present embodiment.
Second expansion link 42 is used for lifting quenching body 41, when heater 3 removes the lower section of reaction unit 1, and second
Expansion link 42 drives quenching body 41 to slide into the lower section of reaction unit 1, and reaction unit 1 is cooled down by quenching body 41.When
After cooling reached for the second response time, the second expansion link 42 falls downward makes quenching body 41 depart from reaction unit 1, and,
Second expansion link 42 drives quenching body 41 to remove the lower section of reaction unit 1, and the first expansion link 32 drives heater body 31 to slide
To the lower section of reaction unit 1, reaction unit 1 is heated by heater body 31, repeats aforesaid operations.
It can be seen that in the present embodiment, lift quenching body 41 by the second expansion link 42 so that quenching body 41 is controlled
Reaction unit 1 is cooled down by system ground, and the second expansion link 42 is slidably connected to guide rail 5 so that the second expansion link 42
Can be in the slid underneath of reaction unit 1, it is simple to quenching body 41 removes the lower section of reaction unit 1 with the second expansion link 42, and then
It is easy to heater 3 slide into the lower section of reaction unit 1 and reaction unit 1 heated, simple in construction, it is easy to implement.
With continued reference to Fig. 1, in above-described embodiment, quenching body 41 may include that staving and coolant.Wherein, staving with
Second end of the second expansion link 42 is connected, and staving is sheathed on the outside of reaction unit 1.Coolant it is provided with in staving.
Specifically, coolant can be mixture of ice and water.
It can be seen that in the present embodiment, quenching device 4 is the staving equipped with coolant, simple in construction, it is simple to operation.
With continued reference to Fig. 1, in the various embodiments described above, reaction unit 1 is provided with thermometer 6, and this thermometer 6 is used for monitoring instead
Answer the temperature within device 1, so, it is simple to the speed raising temperature in reaction unit 1 is controlled, it is achieved that reaction unit
The scalable of temperature in 1.
With continued reference to Fig. 1, in the various embodiments described above, reaction unit 1 is additionally provided with for monitoring reaction unit 1 internal pressure
Pressure gauge 7.Specifically, this supercritical is prepared the device of Graphene and can also be included connecting pipeline, connects pipeline and is arranged in instead
Answering device 1, the first end connecting pipeline is placed in reaction unit 1, and the second end connecting pipeline is placed in the outside of reaction unit 1,
Pressure gauge 7 is connected to connect pipeline.When being embodied as, when reaction unit 1 includes reactor 11 and lid 12, lid 12 is offered
Having perforating, connect pipeline and be arranged in this perforating, the first end connecting pipeline is placed in reactor 11, connects the second of pipeline
End is placed in the outside of reaction 11 devices.
It can be seen that in the present embodiment, by arranging Pressure gauge 7, it is simple to monitoring pressure change within reaction unit 1,
Ensure that organic solvent and the normal reaction of carbon raw material in reaction unit 1, improve the safety of reaction unit 1.
With continued reference to Fig. 1, in the various embodiments described above, connect pipeline and be also provided with relief valve 8, when in reaction unit 1
When pressure exceedes default reaction pressure, relief valve 8 is opened, and the pressure in reaction unit 1 reduces, it is ensured that the safety of reaction unit 1
Run.When being embodied as, default reaction pressure can determine according to practical situation, and this is not done any restriction by the present embodiment.
Connecting pipeline and be also provided with stop valve 9, in there is reaction unit 1, pressure overpressure higher limit etc. is tight
During anxious situation, open stop valve 9, it is possible to quickly reaction unit 1 is carried out pressure release.Preferably, stop valve 9 is at least two.Tool
When body is implemented, upper pressure limit value can determine according to practical situation, and this is not done any restriction by the present embodiment.
In sum, in the present embodiment, by heater, the organic solvent in reaction unit and carbon raw material are carried out
Heating so that organic solvent and carbon raw material can fully occur physical reactions, and the intermolecular force of carbon raw material weakens, increases
The big interfloor distance of carbon raw material, then by quenching device to having occurred and that the organic solvent after physical reactions and carbon raw material
Cooling down, so cold and heat succeed each other stimulation organic solvent and carbon raw material, it is possible to farthest destroys the molecule of carbon raw material
Intermolecular forces, it is simple to the later separation of Graphene, improves the productivity of Graphene, and ensure that the quality of Graphene, cost
Cheap.
Supercritical prepares the embodiment of the method for Graphene:
The invention allows for a kind of utilizing above-mentioned preparation facilities to carry out supercritical to prepare the method that graphite is dilute.See Fig. 2,
Fig. 2 utilizes above-mentioned preparation facilities to carry out supercritical to prepare the flow chart of the dilute method of graphite for what the embodiment of the present invention provided.As
Figure is described, and the method comprises the steps:
Addition step S1, puts into organic solvent and carbon raw material in the reaction unit 1 in above-mentioned preparation facilities.
Specifically, organic solvent and carbon raw material are sufficiently mixed in reaction unit 1.Wherein, the containing of organic solvent
The water yield is 70%～99%.Organic solvent can be ethanol, NMP, surfactant etc., and this organic solvent can be single organic
Solvent, it is also possible to for the mixture of several organic solvents.Carbon raw material can be graphite, coal etc..
Heating steps S2, is placed in the lower section of reaction unit 1 by the heater 3 in preparation facilities, and heater 3 is to reaction
Device 1 heats, until it reaches preset temperature.
Specifically, this preset temperature disclosure satisfy that super critical condition.By heater 3, reaction unit 1 is heated,
Along with the rising of temperature in reaction unit 1, the pressure in reaction unit 1 also can raise.In the present embodiment, in reaction unit 1
Preset temperature can be 250 DEG C～650 DEG C, pressure can be 21MPa～30MPa.When being embodied as, preset temperature can also
Determining according to practical situation, this is not intended to be limited in any by the present embodiment.Pressure can also determine according to practical situation, this reality
Execute example and this is not done any restriction.
When the temperature in reaction unit 1 reaches preset temperature, the organic solvent in reaction unit 1 infiltrates into carbon raw material
Sheet interlayer, the intermolecular force of carbon raw material weakens so that the interfloor distance of carbon raw material increases.Due in organic solvent
Water content many, and the temperature and pressure in this reaction unit 1 met super critical condition, so the water in organic solvent
Can preferably dissolve each other with the organic matter in organic solvent, then water infiltrates into the sheet interlayer of carbon raw material with organic solvent,
Preferably destroy the molecular link of carbon raw material, increase the interfloor distance of carbon raw material.
Quenching step S3, after organic solvent and carbon raw material reaction reached for the first response time, removes heater, and
Quenching device 4 is placed in the lower section of reaction unit 1, and quenching device 4 carries out quenching to reaction unit 1, until it reaches the second reaction
After time, remove quenching device 4.
Specifically, after organic solvent and carbon raw material reaction reached for the first response time, heater 3 stops heating,
Product is cooled down by quenching device 4, owing to the temperature in reaction unit 1 is the highest, so when quenching device 4 is to reaction dress
Putting 1 when cooling down, the temperature of reaction unit 1 reduces, and colds and heat succeed each other and can destroy the intermolecular interaction of carbon raw material further
Power.Being cooled to for the second response time, quenching device 4 stops cooling down reaction unit 1.
Repeat above-mentioned heating and quenching step, obtain Graphene.
First response time can be 20-50min, and the second response time can be 20-50min.It should be noted that tool
When body is implemented, the first response time and the second response time can also determine according to practical situation, and this is not done by the present embodiment
Any restriction.
It should be appreciated by those skilled in the art that the Graphene that above-mentioned reaction unit 1 obtains is crude product Graphene, crude product graphite
Alkene proceeds to separate and just can obtain Graphene.
It can be seen that in the present embodiment, the organic solvent in reaction unit and carbon raw material are carried out by heating steps
Heating so that organic solvent and carbon raw material can fully occur physical reactions, and the intermolecular force of carbon raw material weakens, increases
The big interfloor distance of carbon raw material, and, the water in organic solvent can preferably enter with organic solvent under preset temperature
Row dissolves each other, and water infiltrates into the sheet interlayer of carbon raw material with organic solvent, preferably destroys the molecular link of carbon raw material, increases further
The big interfloor distance of carbon raw material；Again by quenching step to having occurred and that the organic solvent after physical reactions and carbon raw material
Cooling down, so cold and heat succeed each other stimulation organic solvent and carbon raw material, it is possible to farthest destroys the molecule of carbon raw material
Intermolecular forces, it is simple to the later separation of Graphene, improves the productivity of Graphene, and ensure that the quality of Graphene, cost
Cheap.
Obviously, those skilled in the art can carry out various change and the modification essence without deviating from the present invention to the present invention
God and scope.So, if these amendments of the present invention and modification belong to the scope of the claims in the present invention and equivalent technologies thereof
Within, then the present invention is also intended to comprise these change and modification.
Claims (10)
1. a supercritical prepares the device of Graphene, it is characterised in that including: reaction unit (1), supporting mechanism (2), heating
Device (3), quenching device (4) and guide rail (5)；Wherein,
Described reaction unit (1) is connected to described supporting mechanism (2)；
Described guide rail (5) is placed in the lower section of described reaction unit (1), described heater (3) and described quenching device (4)
It is slidably connected to described guide rail (5), and, described heater (3) and described quenching device (4) are led described in alternately edge
Rail (5) slides to the lower section of described reaction unit (1).
Supercritical the most according to claim 1 prepares the device of Graphene, it is characterised in that described heater (3) wraps
Include: heater body (31) and the first expansion link (32)；Wherein,
One end of described first expansion link (32) is slidably connected with described guide rail (5), the other end of described first expansion link (32)
It is connected with described heater body (31).
Supercritical the most according to claim 1 prepares the device of Graphene, it is characterised in that described heater body (31) is
The heating mantle of one end open.
Supercritical the most according to claim 1 prepares the device of Graphene, it is characterised in that described quenching device (4) wraps
Include: quenching body (41) and the second expansion link (42)；Wherein,
First end of described second expansion link (42) is slidably connected with described guide rail (5), the second of described second expansion link (42)
End is connected with described quenching body (41)；Described quenching body (41) is used for cooling down described reaction unit (1).
Supercritical the most according to claim 4 prepares the device of Graphene, it is characterised in that described quenching body (41) is wrapped
Include: staving and coolant；Wherein,
Described staving is connected with the second end of described second expansion link (42), and described coolant is placed in described staving.
Supercritical the most according to any one of claim 1 to 5 prepares the device of Graphene, it is characterised in that described instead
Device (1) is answered to be provided with the thermometer (6) for monitoring internal temperature.
Supercritical the most according to any one of claim 1 to 5 prepares the device of Graphene, it is characterised in that described instead
Device (1) is answered to be provided with the Pressure gauge (7) for monitoring internal pressure.
8. one kind utilizes above-mentioned preparation facilities to carry out supercritical to prepare the method that graphite is dilute, it is characterised in that comprise the steps:
Charging: put into organic solvent and carbon raw material in the reaction unit in described preparation facilities；
Heating: the heater in described preparation facilities is placed in the lower section of described reaction unit, and described heater is to described
Reaction unit heats, until it reaches preset temperature；
Quenching: after described organic solvent and carbon raw material reaction reached for the first response time, remove described heater, and will
Quenching device is placed in below described reaction unit and it is carried out quenching, until it reaches after the second response time, remove described quenching
Device；
Repeat above-mentioned heating steps and quenching step, until it is dilute to obtain graphite.
The most according to claim 8 utilizing above-mentioned preparation facilities to carry out supercritical to prepare the method that graphite is dilute, its feature exists
In, the water content in described organic solvent is 70%～99%.
The most according to claim 8 utilizing above-mentioned preparation facilities to carry out supercritical to prepare the method that graphite is dilute, its feature exists
In, described preset temperature is 250 DEG C～650 DEG C, and described first response time is 20-50min, and described second response time is
20-50min。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500281A (en) * | 2017-09-15 | 2017-12-22 | 北京师范大学 | A kind of stripping means of two-dimensional material |
| CN110653021A (en) * | 2019-11-06 | 2020-01-07 | 核工业理化工程研究院 | Lifting and heating integrated device suitable for cylindrical container |
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| CN102115078A (en) * | 2011-01-19 | 2011-07-06 | 上海交通大学 | Method for preparing graphene by using supercritical fluid |
| CN103771401A (en) * | 2013-12-26 | 2014-05-07 | 中国石油大学(北京) | Preparation method for single-layered graphene |
| CN105129790A (en) * | 2015-10-10 | 2015-12-09 | 杭州海虹精细化工有限公司 | Novel method for preparing graphene oxide under supercritical water condition |
| CN105366668A (en) * | 2015-11-04 | 2016-03-02 | 福建翔丰华新能源材料有限公司 | Method for preparing graphene through supercritical fluid |
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| CN107500281A (en) * | 2017-09-15 | 2017-12-22 | 北京师范大学 | A kind of stripping means of two-dimensional material |
| CN110653021A (en) * | 2019-11-06 | 2020-01-07 | 核工业理化工程研究院 | Lifting and heating integrated device suitable for cylindrical container |
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