CN106044765A - Apparatus and method of supercritically preparing graphene - Google Patents

Apparatus and method of supercritically preparing graphene Download PDF

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CN106044765A
CN106044765A CN201610679541.0A CN201610679541A CN106044765A CN 106044765 A CN106044765 A CN 106044765A CN 201610679541 A CN201610679541 A CN 201610679541A CN 106044765 A CN106044765 A CN 106044765A
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reaction unit
graphene
oxidant
raw material
carbon raw
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刘扬
程乐明
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ENN Science and Technology Development Co Ltd
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ENN Science and Technology Development Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

The invention provides an apparatus and a method of supercritically preparing graphene. The apparatus includes a reaction apparatus, a heating apparatus and an oxidant adding apparatus. The heating apparatus is connected to the reaction apparatus and is used for heating the reaction apparatus. The oxidant adding apparatus is connected to the reaction apparatus and is used for adding an oxidant into the reaction apparatus. By means of the apparatus, a physical reaction can be fully carried out between an organic solvent and a carbon raw material, wherein the organic solvent permeates in layers of the 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 oxidant adding apparatus feeds the oxidant to the reaction apparatus, wherein the oxidant is reacted with the organic solvent to release a large amount of heat intensively. The heat further damages the intermolecular force of the carbon raw material and further increase the layer-to-layer distance of the carbon raw material. The apparatus and the method increase yield of graphene, ensure quality of the graphene and are low in cost.

Description

Supercritical prepares the device and method of Graphene
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, Heater and oxidant adding set;Wherein, heater is connected with reaction unit, for reacting by heating device;Oxidation Agent adding set is connected with reaction unit, for adding oxidant in reaction unit.
Further, above-mentioned supercritical is prepared in the device of Graphene, and oxidant adding set includes: oxidant storage tank and Pressurizer;Wherein, the entrance of pressurizer is connected with oxidant storage tank, and the outlet of pressurizer is connected with reaction unit Logical.
Further, above-mentioned supercritical is prepared the device of Graphene and is also included: agitating device;Wherein, agitating device is with anti- Device is answered to be connected, for the material within reaction unit is stirred.
Further, above-mentioned supercritical is prepared in the device of Graphene, and agitating device includes: load carrier, rotating shaft, driving Mechanism and the stirring paddle being placed in reaction unit;Wherein, drive mechanism is connected to load carrier;Rotating shaft be arranged in reaction unit and Being partially disposed in reaction unit, and one end of rotating shaft is connected with drive mechanism, the other end of rotating shaft is connected with stirring paddle.
Further, above-mentioned supercritical is prepared the device of Graphene and is also included: blow-down tank;Wherein, reaction unit and emptying Tank is connected.
Further, above-mentioned supercritical is prepared in the device of Graphene, and reaction unit and the connecting pipe of blow-down tank set It is equipped with stop valve.
Further, above-mentioned supercritical is prepared in the device of Graphene, and reaction unit and the connecting pipe of blow-down tank set It is equipped with relief valve.
Further, above-mentioned supercritical is prepared in the device of Graphene, and reaction unit is provided with for monitoring reaction unit The Pressure gauge of internal pressure.
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, organic solvent to infiltrate into the sheet interlayer of carbon raw material so that carbonaceous The intermolecular force of raw material weakens, and increases the interfloor distance of carbon raw material, then by oxidant adding set to reaction dress Putting input oxidant, oxidant and organic solvent generation oxidation reaction, discharge violent heat, this heat can break further The intermolecular force of bad carbon raw material, increases the interfloor distance of carbon raw material again, improves the productivity of Graphene, and protects Demonstrate,prove the quality of Graphene, with low cost, solve employing supercritical CO in prior art2Method is prepared Graphene and is caused cost The problem 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 puts into organic solvent and carbon raw material in comprising the steps: the reaction unit in preparation facilities;Preparation facilities In heater reaction unit is heated, until it reaches preset reaction temperature;React with carbon raw material at organic solvent After reaching for the first response time, oxidant adding set is passed through oxidant in reaction unit, at oxidant and organic solvent and After carbon raw material reaction reached for the second response time, obtain Graphene.
Further, above-mentioned supercritical is prepared in the method for Graphene, and the water content of organic solvent is 70%~99%.
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, organic solvent to infiltrate into the sheet interlayer of carbon raw material so that carbonaceous The intermolecular force of raw material weakens, and increases the interfloor distance of carbon raw material, and, the water in organic solvent is at preset temperature Under can preferably dissolve each other with organic solvent, water infiltrates into the sheet interlayer of carbon raw material with organic solvent, preferably destroys The molecular link of carbon raw material, further increases the interfloor distance of carbon raw material;Again by inputting oxidant, oxygen to reaction unit Agent and organic solvent generation oxidation reaction, discharge violent heat, and this heat can destroy dividing of carbon raw material further Sub-intermolecular forces, increases the interfloor distance of carbon raw material again, it is simple to the later separation of Graphene, improves the product of Graphene Rate, it is ensured that the quality of Graphene, and 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, heater 2 and oxidant adding set 3.Its In, heater 2 is connected with reaction unit 1, and heater 2 is for reacting by heating device 1.Oxidant adding set 3 is with anti- Answering device 1 to be connected, oxidant adding set 3 is for adding oxidant in reaction unit 1.Specifically, put in reaction unit 1 It is equipped with organic solvent and carbon raw material.Organic solvent can be ethanol, NMP, surfactant etc., and this organic solvent can be single One organic solvent, it is also possible to for the mixture of several organic solvents.Carbon raw material can be graphite, coal etc..Oxidant can be One or more in hydrogen peroxide, pure oxygen, liquid oxygen and oxygen-enriched air etc..Reaction unit 1 can include reactor 11 and can cover It is connected to the lid 12 of reactor.Heater 2 can be the heating mantle of one end open, and this heating mantle is sheathed on reaction unit 1 Outside.
During preparation, organic solvent and carbon raw material being inputted to reaction unit 1, organic solvent and carbon raw material mix Close.Reaction unit 1 is heated by heater 2 so that the temperature in reaction unit 1 reaches to preset reaction temperature, and this is preset Reaction temperature disclosure satisfy that super critical condition.Due in reaction unit 1 temperature raise, so the pressure in reaction unit 1 also with Rising.When the temperature in reaction unit 1 reaches to preset reaction temperature, organic solvent infiltrates into the sheet interlayer of carbon raw material, The intermolecular force of carbon raw material weakens so that the interfloor distance of carbon raw material increases.Anti-at organic solvent and carbon raw material After should reaching for the first response time, oxidant adding set 3 inputs oxidant, oxidant and organic solvent in reaction unit 1 Oxidation reaction occurs, and this oxidation reaction can discharge violent heat, and this heat can destroy the molecule of carbon raw material further Intermolecular forces, increases the interfloor distance of carbon raw material again.Oxidant and organic solvent react and reached for the second response time, oxidation Agent adding set 3 stops adding oxidant, and heater 2 stops heating, and reaction unit 1 naturally cools to room temperature, obtains graphite Alkene.
During it should be noted that be embodied as, default reaction temperature can be 250 DEG C~650 DEG C, it is also possible to according to reality Situation determines, this is not done any restriction by the present embodiment.Pressure in reaction unit 1 can be 21MPa~30MPa, it is possible to According to circumstances to determine according to reality, this is not done any restriction by the present embodiment.First response time can be 20~ 50min, the second response time can be 10~30min.When being embodied as, the first response time, the second response time can root Determining according to practical situation, this is not limited in any way 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 2 Row heating so that organic solvent and carbon raw material can fully occur physical reactions, organic solvent to infiltrate into the sheet of carbon raw material Interlayer so that the intermolecular force of carbon raw material weakens, is increased the interfloor distance of carbon raw material, then is added by oxidant Device 3 inputs oxidant, oxidant and organic solvent generation oxidation reaction to reaction unit 1, discharges violent heat, this heat Amount can destroy the intermolecular force of carbon raw material further, again increases the interfloor distance of carbon raw material, it is simple to Graphene Later separation, improve the productivity of Graphene, and ensure that the quality of Graphene, with low cost, solve prior art Middle employing 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, oxidant adding set 3 may include that oxidant storage tank 31 and supercharging dress Put 32.Wherein, the entrance of pressurizer 32 is connected with oxidant storage tank 31, the outlet of pressurizer 32 and reaction unit 1 phase Connection.Specifically, if oxidant is gas, such as oxygen etc., pressurizer 32 can be supercharger.If oxidant is liquid, as Liquid oxygen, hydrogen peroxide etc., pressurizer 32 can be force (forcing) pump.
When being embodied as, the connecting pipe between pressurizer 32 and reaction unit 1 can be provided with check valve, this is single It is prevented from the carbon raw material in reaction unit 1, organic solvent or oxidant adverse current to pressurizer 32 to valve.Pressurizer 32 And being also provided with stop valve on the connecting pipe between reaction unit 1, this stop valve can control to add to reaction unit 1 The flow of interior oxidant.
It can be seen that in the present embodiment, the oxidant of oxidant storage tank 31 output carries out supercharging by pressurizer 32, makes The pressure of oxidant improves, it is simple to oxidant adds in reaction unit 1, it is to avoid hypertonia in reaction unit 1 and aoxidize The relatively low oxidant caused of agent pressure cannot add to reaction unit 1.
With continued reference to Fig. 1, in the various embodiments described above, this supercritical is prepared the device of Graphene and can also be included: stirring dress Put 4.Wherein, agitating device 4 is connected with reaction unit 1, and this agitating device 4 is for carrying out the material within reaction unit 1 Stirring.
It can be seen that in the present embodiment, by arranging agitating device 4, it is possible to preferably make oxidant, organic solvent and carbon Raw material is sufficiently mixed, and when oxidant and organic solvent generation oxidation reaction, oxidation reaction discharges violent heat, The stirring of agitating device 4 can also make even heat be distributed, it is to avoid the local temperature of reaction unit 1 is too high causes reaction unit 1 damages.
With continued reference to Fig. 1, in the various embodiments described above, this agitating device 4 may include that load carrier 41, rotating shaft 42, drives Mechanism 43 and stirring paddle 44.Wherein, drive mechanism 43 is connected to load carrier 41, and rotating shaft 42 is arranged in reaction unit 1 and part It is placed in reaction unit 1.One end of rotating shaft 42 is connected with drive mechanism 43, and the other end of rotating shaft 42 is connected with stirring paddle 44 Connecing, stirring paddle 44 is placed in reaction unit 1.Specifically, load carrier 41 can be to be placed in fixing above reaction unit 1 to put down Platform, drive mechanism 43 is arranged at fixed platform, and drive mechanism 43 drive shaft 42 rotates, and the rotation of rotating shaft 42 drives stirring paddle 44 Rotate, and then make stirring paddle 44 that the organic solvent in reaction unit 1, carbon raw material and oxidant are played the effect of stirring. Drive mechanism 43 can be to drive motor.
It can be seen that in the present embodiment, agitating device 4 simple in construction, it is easy to operation.
With continued reference to Fig. 1, in the various embodiments described above, this supercritical is prepared the device of Graphene and can also be included: blow-down tank 5.Wherein, reaction unit 1 is connected with blow-down tank 5.Oxidant and organic solvent generation oxidation reaction can generate CO, O2And CO2, Whether this blow-down tank 5, for detecting the gas of reaction unit 1 output, is CO, O according to the gas of reaction unit 1 output2And CO2, The organic matter that can determine whether in reaction unit 1 in organic solvent whether exhaustive oxidation.When the gas of reaction unit 1 output is mainly O2 And CO2, it is determined that the exhaustive oxidation of the organic matter in organic solvent in reaction unit 1, oxidant adding set 3 stops to reaction Input oxidant in device 1, heater 2 stops heating, and reaction unit 1 naturally cools to room temperature, obtains Graphene.
It can be seen that in the present embodiment, by arranging blow-down tank 5, it is possible to according to the kind of the gas of reaction unit 1 output Judge the whether exhaustive oxidation of the organic matter in organic solvent, better control over the total amount of the oxidant added to reaction unit 1, Avoid adding too much oxidant, it is ensured that the safe operation of reaction unit 1.
With continued reference to Fig. 1, in the various embodiments described above, the connecting pipe of reaction unit 1 and blow-down tank 5 can be provided with and cut Only valve 6.When being in an emergency, open stop valve 6, it is possible to quickly reaction unit 1 is carried out pressure release.Preferably, stop valve 6 For at least two.
With continued reference to Fig. 1, in the various embodiments described above, reaction unit 1 is also provided with on the connecting pipe of blow-down tank 5 Relief valve 7.When the pressure in reaction unit 1 exceedes preset pressure higher limit, relief valve 7 is opened, the pressure in reaction unit 1 Reduce, it is ensured that the safe operation of reaction unit 1.When being embodied as, preset pressure higher limit can determine according to practical situation, This is not intended to be limited in any by the present embodiment.
With continued reference to Fig. 1, in the various embodiments described above, reaction unit 1 can be provided with for monitoring the internal pressure of reaction unit 1 The Pressure gauge 8 of power, it is simple to monitoring pressure change within reaction unit 1, it is ensured that organic solvent and carbon raw material in reaction unit 1 Normal reaction, improve the safety of reaction unit 1.
With continued reference to Fig. 1, in the various embodiments described above, reaction unit 1 can be provided with thermometer 9, and this thermometer 9 is used for supervising Temperature within measured reaction device 1, in such manner, it is possible to the speed raising temperature in reaction unit 1 is controlled, it is achieved that reaction The scalable of temperature in device 1.
In sum, by heater 2, the organic solvent in reaction unit 1 and carbon raw material are heated so that Organic solvent and carbon raw material can fully occur physical reactions, and the intermolecular force of carbon raw material weakens, and increases carbonaceous The interfloor distance of raw material, then input oxidant by oxidant adding set 3 to reaction unit 1, oxidant is sent out with organic solvent Raw oxidation reaction, discharges violent heat, and this heat can destroy the intermolecular force of carbon raw material further, again increases The interfloor distance of big carbon raw material, improves the productivity of Graphene, and ensure that the quality of Graphene, with low cost.
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:
Step S1, puts into organic solvent and carbon raw material in the reaction unit 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%, and 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..
Step S2, reaction unit is heated by the heater in preparation facilities, until it reaches preset reaction temperature.
Specifically, default reaction temperature disclosure satisfy that super critical condition.By heater 2, reaction unit 1 is added Heat, along with the rising of temperature in reaction unit 1, the pressure in reaction unit 1 also can raise.In the present embodiment, reaction unit 1 Interior default reaction temperature can be 250 DEG C~650 DEG C, and pressure can be 21MPa~30MPa.When being embodied as, preset reaction Temperature can also determine according to practical situation, and this is not intended to be limited in any by the present embodiment.Pressure can also be according to practical situation Determining, this is not intended to be limited in any by the present embodiment.
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.
Step S3, after organic solvent and carbon raw material react and reached for the first response time, oxidant adding set is to instead It is passed through oxidant in answering device, after oxidant and organic solvent and carbon raw material react and reached for the second response time, obtains stone Ink alkene.
Specifically, after organic solvent and carbon raw material reaction reached for the first response time, oxidant adding set 3 is to instead Answering input oxidant in device 1, oxidant and organic solvent generation oxidation reaction, this oxidation reaction discharges violent heat, This heat can destroy the intermolecular force of carbon raw material further, again increases the interfloor distance of carbon raw material.In oxidation Agent and organic solvent react after reaching for the second response time, and oxidant adding set 3 stops adding oxidant, and heater 2 stops Only heating, reaction unit 1 naturally cools to room temperature, obtains Graphene.
Oxidant can be one or more in hydrogen peroxide, pure oxygen, liquid oxygen and oxygen-enriched air etc..First response time can Thinking 20~50min, the second response time can be 10~30min.During it should be noted that be embodied as, during the first reaction Between and the second response time can determine according to practical situation, 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 and carbon raw material are carried out by heating steps Heating so that organic solvent and carbon raw material can fully occur physical reactions, organic solvent to infiltrate into the lamella of carbon raw material Between so that the intermolecular force of carbon raw material weakens, and increases the interfloor distance of carbon raw material, and, in organic solvent Water can preferably dissolve each other with organic solvent under preset temperature, and water infiltrates into the lamella of carbon raw material with organic solvent Between, preferably destroy the molecular link of carbon raw material, further increase the interfloor distance of carbon raw material;Again by reaction unit 1 input oxidant, oxidant and organic solvent generation oxidation reaction, discharge violent heat, this heat can break further The intermolecular force of bad carbon raw material, increases the interfloor distance of carbon raw material again, it is simple to the later separation of Graphene, improves The productivity of Graphene, it is ensured that the quality of Graphene, and with low cost.
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), heater (2) and oxygen Agent adding set (3);Wherein,
Described heater (2) is connected with described reaction unit (1), is used for heating described reaction unit (1);
Described oxidant adding set (3) is connected with described reaction unit (1), for adding in described reaction unit (1) Oxidant.
Supercritical the most according to claim 1 prepares the device of Graphene, it is characterised in that described oxidant adding set (3) including: oxidant storage tank (31) and pressurizer (32);Wherein,
The entrance of described pressurizer (32) is connected with described oxidant storage tank (31), the outlet of described pressurizer (32) with Described reaction unit (1) is connected.
Supercritical the most according to claim 1 prepares the device of Graphene, it is characterised in that also include: agitating device (4);Wherein,
Described agitating device (4) is connected with described reaction unit (1), for entering the material that described reaction unit (1) is internal Row stirring.
Supercritical the most according to claim 3 prepares the device of Graphene, it is characterised in that described agitating device (4) wraps Include: load carrier (41), rotating shaft (42), drive mechanism (43) and the stirring paddle (44) being placed in described reaction unit (1);Its In,
Described drive mechanism (43) is connected to described load carrier (41);
In described rotating shaft (42) is arranged in described reaction unit (1) and is partially disposed in described reaction unit (1), and described rotating shaft (42) one end is connected with described drive mechanism (43), and the other end of described rotating shaft (42) is connected with described stirring paddle (44) Connect.
Supercritical the most according to any one of claim 1 to 4 prepares the device of Graphene, it is characterised in that also include: Blow-down tank (5);Wherein, described reaction unit (1) is connected with described blow-down tank (5).
Supercritical the most according to claim 5 prepares the device of Graphene, it is characterised in that described reaction unit (1) with Stop valve (6) it is provided with on the connecting pipe of described blow-down tank (5).
Supercritical the most according to claim 5 prepares the device of Graphene, it is characterised in that described reaction unit (1) with Relief valve (7) it is provided with on the connecting pipe of described blow-down tank (5).
Supercritical the most according to claim 1 prepares the device of Graphene, it is characterised in that described reaction unit (1) sets It is equipped with the Pressure gauge (8) for monitoring reaction unit internal pressure.
9. 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:
Organic solvent and carbon raw material is put in reaction unit in described preparation facilities;
Described reaction unit is heated by the heater in described preparation facilities, until it reaches preset reaction temperature;
After described organic solvent and described carbon raw material react and reached for the first response time, oxidant adding set to described instead It is passed through oxidant in answering device, reacts when reaching the second reaction with described organic solvent and described carbon raw material at described oxidant After between, obtain Graphene.
The most according to claim 9 utilizing above-mentioned preparation facilities to carry out supercritical to prepare the method that graphite is dilute, its feature exists In, the water content of described organic solvent is 70%~99%.
CN201610679541.0A 2016-08-17 2016-08-17 Apparatus and method of supercritically preparing graphene Pending CN106044765A (en)

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CN106744893A (en) * 2016-12-19 2017-05-31 厦门大学 The controllable adding set of oxidant that batch prepares Graphene quality can be improved
CN106829938A (en) * 2017-03-09 2017-06-13 辽宁兰晶科技有限公司 The method that overcritical sulfur hexafluoride stripping prepares Graphene or graphene nanometer sheet
CN108609613A (en) * 2018-07-27 2018-10-02 郑州大学 A kind of preparation method of zero defect graphene

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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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CN203428916U (en) * 2013-05-02 2014-02-12 黑龙江科技学院 Supercritical reaction kettle for nanometer graphene preparation
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
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CN106744893A (en) * 2016-12-19 2017-05-31 厦门大学 The controllable adding set of oxidant that batch prepares Graphene quality can be improved
CN106829938A (en) * 2017-03-09 2017-06-13 辽宁兰晶科技有限公司 The method that overcritical sulfur hexafluoride stripping prepares Graphene or graphene nanometer sheet
CN108609613A (en) * 2018-07-27 2018-10-02 郑州大学 A kind of preparation method of zero defect graphene
CN108609613B (en) * 2018-07-27 2021-09-17 郑州大学 Preparation method of defect-free graphene

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