CN108059154A - Graphene powder preparation system - Google Patents

Graphene powder preparation system Download PDF

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Publication number
CN108059154A
CN108059154A CN201711026328.0A CN201711026328A CN108059154A CN 108059154 A CN108059154 A CN 108059154A CN 201711026328 A CN201711026328 A CN 201711026328A CN 108059154 A CN108059154 A CN 108059154A
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gas
unit
cooling device
collection
tank
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CN201711026328.0A
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CN108059154B (en
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毛鸥
钟国星
张美杰
郑涛
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Jiangsu Nanai Polytron Technologies Inc
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Jiangsu Nanai Polytron Technologies Inc
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Abstract

The invention discloses a kind of graphene powder preparation system, including:Gas cooling device, gas preheating unit, material adding set, reaction unit, material collecting device, gas concentration unit.The graphene powder preparation system of the present invention, effectively the carbon dioxide for being used as solvent can be recycled by gas concentration unit, and it is reused by being passed through gas cooling device again, so as to saving carbon dioxide, avoid the carbon dioxide (toxic gas may be carried) after reaction and be directly discharged into air air is polluted.The present invention is continuous circular response, and preparation efficiency is high, and cost is relatively low.

Description

Graphene powder preparation system
Technical field
The present invention relates to chemical technology field more particularly to a kind of graphene powder preparation systems.
Background technology
Graphene is a kind of the new of hexatomic ring periodic cellular shape lattice structure being made of carbon atom with sp2 hybridized orbits Type carbon allotrope, thickness are about 0.335nm.Graphene its because of unique two dimensional crystal structure and excellent mechanics, electricity , calorifics and optical characteristics become the research hotspot of Material Field in recent years.
At present, for the research of the preparation of grapheme material, property and application, it has also become the current whole world most popular research neck One of domain.The preparation method of graphene mainly has mechanical stripping method, chemical vapour deposition technique, epitaxial crystal growth method and oxidation to go back Former method etc..But these methods significantly limit its further application all there are some shortcomings, such as micromechanics stripping method not It is suitble to extensive property production;Though chemical vapour deposition technique can prepare the graphene film of high quality, large area, preferable base The expensive of bottom material affects the industrialized production of graphene;Oxidation-reduction method can cause graphene generation that can not repair The defects of multiple, and easily bring the reducing agents such as waste liquor contamination, hydrazine toxic during largely preparing using this method graphene, and It is inflammable and explosive, it is unfavorable for high-volume and keeps the safety in production.Realize graphene industrialization, key issue is that exploration is extensive, high-quality The graphene preparation technology of amount, low cost.
It is a kind of new technique that supercritical fluid technique, which prepares graphene, which utilizes one or more solvents (such as two Carbonoxide, ethyl alcohol, DMF, NMP equal solvent) in the supercritical state with the characteristic pair of its density, viscosity, diffusion coefficient etc. Graphite carries out intercalation, and the rapid expanding of completion graphite flake layer is removed to obtain graphene during quick pressure releasing.Chinese patent Patent No. 201110021033.0 discloses a kind of " method of preparing graphene by using supercritical fluid ", by by graphite raw material It is mixed with organic solvent, and in the range of 200 DEG C -700 DEG C and 10-100Mpa, then fast cooling and decompression is so as to preparing stone Black alkene.In that patent, have that used organic solvent toxicity is big, the graphene amount prepared in the unit interval is small, and step is numerous It is trivial, the problems such as being difficult to control, the industrialization production of graphene can not be carried out.
Therefore, it is necessary to designing a kind of can recycle that solvent, preparation efficiency are high, prepare the good graphene powder of effect Preparation system.
The content of the invention
For the above-mentioned technical problems in the prior art, the embodiment provides a kind of Graphene powder systems Standby system.
In order to solve the above technical problems, the embodiment of the present invention the technical solution adopted is that:
A kind of graphene powder preparation system, including:It is gas cooling device, gas preheating unit, material adding set, anti- Answer device, material collecting device, gas concentration unit;Wherein:
The gas cooling device is connected with source of the gas, and the gas cooling device is used for cooling gas;
The gas preheating unit is connected with the gas cooling device, and the gas preheating unit is used for will be through the gas Body cooling device gas after cooling is preheated, so that gas after cooling reaches preset temperature
The gas preheating unit and the material adding set are connected with the reaction unit, so that:Through the gas Material in the gas and the material adding set of the preheating of body preheating device enters in the reaction unit;
The reaction unit is used to that gas to be made to be mixed to form gas-solid mixture with raw material;
The material collecting device is connected with the reaction unit and is used to receive the gas-solid mixture, and gas-solid is mixed The reaction product closed in object is separated with gas, and the reaction product enters collecting bag;
The gas concentration unit is connected with the material collecting device, and is divided for receiving the material collecting device From gas;
The gas concentration unit is connected with the gas cooling device, and the gas cooling device is used to receive the gas Gas in body retracting device.
Preferably, the gas cooling device includes the drier and condenser that are connected, to pass the gas through drier It is cooled down afterwards into the condenser.
Preferably, the gas preheating unit includes the first circulation being connected pump and preheater;The first circulation pump So that the gas through gas cooling device cooling enters the preheater with certain pressure, the preheater is used for gas It is preheated to preset temperature.
Preferably, the reaction unit includes retort, is provided with blender in the retort, the blender is used for It will be sufficiently mixed to form the solids and gas mixture with gas into the material in the retort.
Preferably, the material collecting device includes collection of products tank and the vacuum connected with the collection of products tank Pump, the vacuum pump are used to that the collection of products tank to be made to make the product before the solids and gas mixture of the reaction unit is received Pressure in collecting tank reduces;The lower end of the collection of products tank is provided with collecting bag, and the collecting bag produces for collecting reaction Object simultaneously separates gas;Gas enters the gas concentration unit after the collecting bag.
Preferably, the gas concentration unit includes the gas collection tank being connected and powder filter;The powder mistake Filter is used to filter the reaction product of the powder shaped in gas;The gas collection tank is for collection through the powder filter mistake The gas of filter.
Preferably, it is provided with second circulation pump between the gas concentration unit and the gas cooling device, described the Two circulating pumps are used to the gas in the gas concentration unit being pumped into the gas cooling device.
Preferably, switch valve is provided at least between reaction unit and material collecting device, when being arranged at the reaction After switch valve between device and material collecting device is opened, the solids and gas mixture in the reaction unit sprays into the product and receives Collect in tank.
Compared with prior art, the advantageous effect for the graphene powder preparation system that the embodiment of the present invention is provided is: The graphene powder preparation system of the present invention can effectively be returned the carbon dioxide for being used as solvent by gas concentration unit It receives, and is reused by being passed through gas cooling device again, so as to save carbon dioxide, avoid reaction Carbon dioxide (may carry toxic gas) afterwards is directly discharged into air and air is polluted.The present invention is continuous Xun Huan Reaction, preparation efficiency is high, and cost is relatively low.
Description of the drawings
Fig. 1 is the structure diagram for the graphene powder preparation system that one embodiment of the present of invention provides.
Fig. 2 be gas tank in the graphene powder preparation system that provides of one embodiment of the present of invention, the 3rd switch valve with And the connection relation between control valve.
Fig. 3 is the enlarged view of the local A of Fig. 2.
Fig. 4 is the enlarged view of the local B of Fig. 2.
In figure:
10- gas cooling devices;11- driers;12- condensers;13- first switch valves;20- gas preheating units;21- First circulation pumps;22- preheaters;23- second switch valves;30- material adding sets;31- measuring tanks;40- reaction units;41- Retort;42- blenders;50- material collecting devices;51- collection of products tanks;52- vacuum pumps;The 3rd switch valves of 54-;541- is forever Magnet;542- electromagnets;543- passages;544- pilot holes;60- gas concentration units;61- powder filters;62- gas collections Tank;63- second circulations pump;The 5th switch valves of 64-;The 4th switch valves of 70-;80- gas tanks;81- conduits;90- control valves;91- valves Body;92- spools;93- air guide channels;94- air inlets;95- gas outlets;96- functional holes.
Specific embodiment
For those skilled in the art is made to be better understood from technical scheme, below in conjunction with the accompanying drawings and specific embodiment party Formula elaborates to the present invention.
As shown in Figure 1, embodiment of the invention discloses that a kind of graphene powder preparation system, including gas cooling device 10th, gas preheating unit 20, material adding set, reaction unit, material collecting device 50, gas concentration unit 60;Gas is cold But device 10 is connected with source of the gas, and for source of the gas for providing carbon dioxide, gas cooling device 10 is used for cooled carbon dioxide gas Body;Gas preheating unit 20 is connected with gas cooling device 10, and gas preheating unit 20 is used for will be cold through gas cooling device 10 But the carbon dioxide after is preheated, so that gas after cooling reaches preset temperature, (preset temperature is required by participating in reacting Rated temperature);Gas preheating unit 20 and material adding set are connected with reaction unit, and object adding set is used for anti- It answers and graphite is added in device, gas preheating unit 20 is used to be passed through carbon dioxide, carbon dioxide into reaction unit It is sufficiently mixed with graphite in reaction unit, to form solids and gas mixture;Material collecting device 50 is connected with reaction unit And for receiving gas-solid mixture, after solids and gas mixture sprays into material collecting device 50 with certain flow rate, filled in material collection Just graphene is generated in putting 50, which is also divided generated graphene and carbon dioxide From the graphene as reaction product enters collecting bag;Gas concentration unit 60 is connected with material collecting device 50, and for connecing Receive the separated carbon dioxide of material collecting device 50;Gas concentration unit 60 is connected with gas cooling device 10, gas Cooling device 10 is used to receive the carbon dioxide in gas concentration unit 60.
As described above, the present invention graphene powder preparation system, by gas concentration unit 60 can effectively by Carbon dioxide as solvent recycles, and is reused by being passed through gas cooling device 10 again, so as to save Carbon dioxide has been saved, the carbon dioxide (toxic gas may be carried) after reaction has been avoided and is directly discharged into air to big Gas pollutes.The present invention is continuous circular response, and preparation efficiency is high, and cost is relatively low.
It should be noted that:Carbon dioxide is mixed with out graphene as physical reactions with graphite, well known, carbon dioxide Being sprayed into graphite mixture with certain speed in collection device just makes graphite be converted into graphene.That is, for the present invention, graphene For material collecting device 50, (mixture of carbon dioxide and graphite is sprayed into certain flow rate in material collecting device 50 generation position Just graphene is generated, and the chemical form of carbon dioxide does not change).
Gas cooling device 10, gas preheating unit 20, material adding set, reaction unit, material collecting device 50 with And the combination of 60 each device of gas concentration unit can there are many, in a preferred embodiment of the invention, gas cooling dress Putting 10 includes the drier 11 that is connected and condenser 12, with pass the gas through after drier 11 carried out into condenser 12 it is cold But.Gas preheating unit 20 includes the first circulation being connected pump 21 and preheater 22;First circulation pump 21 is so that cold through gas But the gas that device 10 cools down enters preheater 22 with certain pressure, and preheater 22 is used to gas being preheated to preset temperature.Instead Device is answered to include retort, is provided with blender in retort, blender for will enter the material in retort and gas into Row is sufficiently mixed to form solids and gas mixture.Material collecting device 50 includes collection of products tank 51 and connects with collection of products tank 51 Logical vacuum pump 52, vacuum pump 52 are used to that collection of products tank 51 to be made to receive product before the solids and gas mixture of reaction unit is received The pressure collected in tank 51 reduces;The lower end of collection of products tank 51 is provided with collecting bag, and collecting bag is for collecting reaction product and divides From gas;Gas enters gas concentration unit 60 after collecting bag.Gas concentration unit 60 includes the gas collection being connected Tank 62 and powder filter 61;Powder filter 61 is used to filter the reaction product of the powder shaped in gas;Gas collection tank 62 For collecting the gas filtered through powder filter 61.Second is provided between gas concentration unit 60 and gas cooling device 10 Circulating pump 63, second circulation pump 63 are used to the gas in gas concentration unit 60 being pumped into gas cooling device 10.
As described above, the gas in gas collection tank 62 enters by second circulation pump 63 in gas cooling device 10 Drier 11 be dried first, it is dry after into being cooled down in condenser 12, then in the effect of first circulation pump 21 Under, into preheater 22, the carbon dioxide of cooling is heated up, gas temperature is made to meet reaction requirement, then, then is passed through anti- It answers in tank, and the measuring tank in material adding set imports graphite in retort after measuring the amount of graphite, in retort Blender mixes carbon dioxide with graphite, however mixture is made to be sprayed into larger speed in collection of products tank 51, so as to Graphene is obtained in collection of products tank 51, the lower end collecting bag which is installed in collection of products tank 51 is collected, and dioxy Change carbon gas and enter powder filter 61 by collecting bag, the powder filter 61 is powdered by what is be mixed in carbon dioxide Graphene filter out, carbon dioxide after filtering enter gas collection tank 62 and again pass by second circulation pump 63 pump Enter drier 11 to recycle again.
Preferably, first switch valve 13 is provided between condenser 12 and first circulation pump 21, in preheater 22 and instead It answers and is provided with second switch valve 23 between tank, the 3rd switch valve 54 is provided between retort and collection of products tank 51;In powder The 4th switch valve 70 is provided between body filter 61 and collection of products tank 51, is set between second circulation pump 63 and drier 11 It is equipped with the 5th switch valve 64.Each switch valve plays an important role of identical:Control reaction process or end-around carry.
In above-mentioned each switch valve, there are one special roles compared to other switch valves tool for the 3rd switch valve 54:Make retort In carbon dioxide and the mixture of graphite collection of products tank 51 is entered with certain flow rate, the mixture of carbon dioxide and graphite Flow velocity is bigger, and the quality of prepared graphene is better.For this purpose, the 3rd switch valve 54 is through swtich valve, so that The 3rd switch valve 54 of process of the mixture of carbon dioxide and graphite smoothly.
The reason for mixture of carbon dioxide and graphite can enter collection of products tank 51 using certain flow rate as:Collection of products Tank 51 is by 52 vacuum state of vacuum pump, so that generating certain pressure difference between retort and collection of products tank 51.It is actual Upper this pressure difference is more big more the flow velocity of mixture can be made bigger, so as to more prepare the preferable graphene of mass.
However, under the premise of it can not reduce the pressure in collection of products tank 51 (its close to vacuum state, pressure can not be again Reduce), it is necessary to improve the pressure in retort, however, make retort keep for a long time high pressure conditions to parts thereon with And its security is a stern challenge.
To solve the problems, such as mixture velocity, in a preferred embodiment of the invention, as shown in Figures 2 to 4, make Three switch valves 54 are arranged to:For controlling the spool of 54 break-make of the 3rd switch valve, there are two magnet control action, one of magnetic Body is permanent magnet 541, another magnet is electromagnet 542;By being that 542 on/off of electromagnet is electric and the 3rd switch valve 54 of closure In passage 543, so as to control the break-make between collection of products tank 51 and retort, i.e. control the ejection of mixture;And Pilot hole 544 is offered in the passage 543 of three switch valves 54;Graphene powder preparation system also adds gas tank 80, the gas tank 80 High-pressure carbon dioxide gas is inside contained with, which is connected by a control valve 90 with retort, which is used for Gas tank 80 is controlled to lead to gases at high pressure into retort.The control valve 90 includes the valve body 91 with air inlet 94 and gas outlet 95, The spool 92 being arranged in valve body 91, air guide channel 93 is offered in the spool 92, and spool 92 makes air inlet 94 by mobile It is connected by air guide channel 93 with gas outlet 95, so as to lead to gases at high pressure or by mobile for retort for blocking Air inlet 94 and gas outlet 95 are ventilated so as to block gas tank 80 for retort, and under the action of 91 spring of valve body, spool 92 is usual It is held in the position blocked.A functional hole 96 is opened up on valve body 91, after the functional hole 96 is connected with certain pressure gas, Pushing and pressing spool 92 moves and air inlet 94 is made to be connected with gas outlet 95.The pilot hole 544 of 3rd switch valve 54 by conduit 81 with The functional hole 96 of valve body 91 connects.
As described above, it is in the 3rd switch valve 54 after mixing to work as carbon dioxide and graphite in retort Electromagnet 542 be powered after, in spool action and open the passage 543 in it, mixture in retort was by should Passage 543 sprays, meanwhile, the gas in mixture enters functional hole 96 by pilot hole 544, conduit 81, pushes against control valve 90 In spool 92 act, and connect the air admission hole of control valve 90 and venthole, at this point, gas tank 80 is quickly by the titanium dioxide of high pressure Carbon gas is passed through retort and the pressure in retort is made to raise rapidly by control valve 90, then makes retort and collection of products Pressure difference between tank 51 increases rapidly, so that the outflow that mixture sprays into collection of products tank 51 increases rapidly, so as to make Standby mass more graphene.It is the electromagnet 542 in the 3rd switch valve 54 after the mixture in retort will spray Power-off, the spool of the 3rd switch valve 54 act and block passage 543, and pilot hole 544 passes through without gas, and control valve 90 is in spring Under the action of power, spool 92, which is returned to, blocks position, and the pressure in retort declines.
The present invention associates the action of control valve 90 of the action of the 3rd switch valve 54 with controlling gas tank 80 so that retort While being sprayed to collection of products tank 51, control valve 90 is made to open and reaction pressure inside the tank is made to increase rapidly, consequently facilitating carrying The flow velocity of high mixture, and when that need not spray, closing control valve 90.
The said structure of the present invention is in the moment of retort injection retort to be caused to be in high pressure conditions, thus will not The all parts of damage thereon, Keep Clear-High Voltage, and coefficient greatly reduces.
It should be noted that:By set at pilot hole 544 filter device can favorable filtration fall powder in mixture, And gas is only allowed to pass through conduit 81.
Above example is only exemplary embodiment of the present invention, is not used in the limitation present invention, protection scope of the present invention It is defined by the claims.Those skilled in the art can make the present invention respectively in the essence and protection domain of the present invention Kind modification or equivalent substitution, this modification or equivalent substitution also should be regarded as being within the scope of the present invention.

Claims (8)

1. a kind of graphene powder preparation system, which is characterized in that including:Gas cooling device, gas preheating unit, material add Feeder apparatus, reaction unit, material collecting device, gas concentration unit;Wherein:
The gas cooling device is connected with source of the gas, and the gas cooling device is used for cooling gas;
The gas preheating unit is connected with the gas cooling device, and the gas preheating unit is used for will be cold through the gas But device gas after cooling is preheated, so that gas after cooling reaches preset temperature;
The gas preheating unit and the material adding set are connected with the reaction unit, so that:It is pre- through the gas Material in the gas and the material adding set of thermal preheating enters in the reaction unit;
The reaction unit is used to that gas to be made to be mixed to form gas-solid mixture with raw material;
The material collecting device is connected with the reaction unit and is used to receive the gas-solid mixture, and by gas-solid mixture In reaction product separated with gas, the reaction product enters collecting bag;
The gas concentration unit is connected with the material collecting device, and separated for receiving the material collecting device Gas;
The gas concentration unit is connected with the gas cooling device, and the gas cooling device is returned for receiving the gas Gas in receiving apparatus.
2. graphene powder preparation system according to claim 1, which is characterized in that the gas cooling device includes phase The drier and condenser of connection, to be cooled down into the condenser after passing the gas through drier.
3. graphene powder preparation system according to claim 1, which is characterized in that the gas preheating unit includes phase The first circulation pump and preheater of connection;The first circulation pumps so that the gas through gas cooling device cooling is with certain Pressure enters the preheater, and the preheater is used to gas being preheated to preset temperature.
4. graphene powder preparation system according to claim 1, which is characterized in that the reaction unit includes reaction Tank, blender is provided in the retort, and the blender carries out for that will enter the material in the retort with gas It is sufficiently mixed to form the solids and gas mixture.
5. graphene powder preparation system according to claim 1, which is characterized in that the material collecting device includes production Object collecting tank and the vacuum pump connected with the collection of products tank, the vacuum pump are used to receiving the collection of products tank Before the solids and gas mixture of the reaction unit, reduce the pressure in the collection of products tank;The lower end of the collection of products tank Collecting bag is provided with, the collecting bag is for collecting reaction product and separates gas;Gas enters institute after the collecting bag State gas concentration unit.
6. graphene powder preparation system according to claim 1, which is characterized in that the gas concentration unit includes phase The gas collection tank of connection and powder filter;The powder filter is used to filter the reaction product of the powder shaped in gas; The gas that the gas collection tank filters for collection through the powder filter.
7. graphene powder preparation system according to claim 1, which is characterized in that the gas concentration unit with it is described It is provided with second circulation pump between gas cooling device, second circulation pump is for by the gas in the gas concentration unit It is pumped into the gas cooling device.
8. graphene powder preparation system according to claim 5, which is characterized in that at least received in reaction unit and material Switch valve is provided between acquisition means, after the switch valve being arranged between the reaction unit and material collecting device is opened, Solids and gas mixture in the reaction unit is sprayed into the collection of products tank.
CN201711026328.0A 2017-10-27 Graphene powder preparation system Active CN108059154B (en)

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Application Number Priority Date Filing Date Title
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CN108059154A true CN108059154A (en) 2018-05-22
CN108059154B CN108059154B (en) 2024-07-05

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112429727A (en) * 2020-11-23 2021-03-02 谢首情 Stripping device and stripping method for graphene
CN114293814A (en) * 2022-01-10 2022-04-08 湖南大学 Stable dry grinding self-adaptive heavy concrete wall dismantling device

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Publication number Priority date Publication date Assignee Title
KR20020027749A (en) * 2000-10-05 2002-04-15 김현효 Recycling System and Method of Supercritical Carbon Dioxide
CN102828161A (en) * 2012-08-21 2012-12-19 许子寒 Graphene production method and continuous production device of graphene
KR20130137839A (en) * 2012-06-08 2013-12-18 (주) 시온텍 Manufacturing method of graphene
CN105473499A (en) * 2013-08-21 2016-04-06 韩化石油化学株式会社 Graphene, method for preparing graphene, and apparatus for preparing graphene
CN207511834U (en) * 2017-10-27 2018-06-19 江苏天奈科技股份有限公司 Graphene powder preparation system

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20020027749A (en) * 2000-10-05 2002-04-15 김현효 Recycling System and Method of Supercritical Carbon Dioxide
KR20130137839A (en) * 2012-06-08 2013-12-18 (주) 시온텍 Manufacturing method of graphene
CN102828161A (en) * 2012-08-21 2012-12-19 许子寒 Graphene production method and continuous production device of graphene
CN105473499A (en) * 2013-08-21 2016-04-06 韩化石油化学株式会社 Graphene, method for preparing graphene, and apparatus for preparing graphene
CN207511834U (en) * 2017-10-27 2018-06-19 江苏天奈科技股份有限公司 Graphene powder preparation system

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112429727A (en) * 2020-11-23 2021-03-02 谢首情 Stripping device and stripping method for graphene
CN114293814A (en) * 2022-01-10 2022-04-08 湖南大学 Stable dry grinding self-adaptive heavy concrete wall dismantling device

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