CN102730677A - Equipment and method for preparing graphene and prepared graphene - Google Patents
Equipment and method for preparing graphene and prepared graphene Download PDFInfo
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- CN102730677A CN102730677A CN2012102541934A CN201210254193A CN102730677A CN 102730677 A CN102730677 A CN 102730677A CN 2012102541934 A CN2012102541934 A CN 2012102541934A CN 201210254193 A CN201210254193 A CN 201210254193A CN 102730677 A CN102730677 A CN 102730677A
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Abstract
The invention relates to equipment for preparing graphene, comprising a reaction room (1) and a sample collecting room (5) arranged under the reaction room, wherein the walls of the reaction room (1) are provided with a first gas inlet, a second gas inlet and a first material inlet except a bottom wall, and the bottom wall of the reaction room (1) can be opened. The method for preparing the graphene comprises the following steps of: (a) putting graphite oxide into a reaction room (3) from a material inlet (8), and charging inert gas into the reaction room through a gas inlet (7), so that the inert gas is filled with the whole room; (b) charging hot inert gas into the reaction room (3) from another gas inlet (12), so that the graphite oxide is reacted; and (c) blowing the inert gas to the bottom wall (4) of the reaction room from the gas inlet (7), so that the bottom wall of the reaction room is opened, and the generated graphene is charged into the sample collecting room (5) under the blowing of the inert gas. Finally, the invention further relates to the graphene prepared by the equipment and the method.
Description
Technical field
The present invention relates to a kind of continuous preparation Graphene equipment, prepare the method for Graphene and the Graphene that makes thus by said equipment.
Background technology:Graphene has excellent physics and chemical property, is expected in fields such as high-performance nano electron device, matrix material, field emmision material, gas sensors, and particularly energy field of storage (ultracapacitor, battery etc.) obtains widespread use.
Preparation method of graphene has a lot, and wherein oxidation reduction process can be prepared a tonne grapheme material, good reproducibility, and the Graphene of preparing is quality controllable, is considered to one of important method that can realize the continuous production Graphene.The preparation principle of oxidation reduction process is generally: with strong oxidizer (like SODIUMNITRATE, the vitriol oil, potassium permanganate, ydrogen peroxide 50 etc.) graphite oxide starting material, form graphite oxide; Make original lamella graphite separately through the Van der Waals force that the reduction method deoxidation overcomes between graphite flake layer graphite oxide then, form grapheme material.Said reduction method has a lot, and wherein thermal shocking reduction method will be disperseed and reduce graphite oxide one step and accomplished, and improve production efficiency and the possibility of accomplishing scale production is arranged.The process that thermal shocking reduction graphite oxide prepares Graphene is generally: with placing the high-temperature zone of protection of inert gas rapidly after the graphite oxide grinding for preparing and keeping for some time; The graphite oxide deoxidation is reduced; Become black by pale brown look, prepare grapheme material.But this method mainly relies on manual operation, and operating process has unstable inevitably; In addition, because main dependence manual operation can't realize continuous production, limited the large-scale production of Graphene thus.
Summary of the invention:To the problems referred to above, the invention provides a kind of equipment for preparing Graphene, it comprises:
(1) reaction chamber has first gas inlet, second gas inlet and a material inlet, and said three inlets are positioned at other any walls except that diapire, and its diapire be openable and
(2) sample collection room that are positioned at the reaction chamber below.
In addition, the invention provides a kind of method for preparing Graphene, it may further comprise the steps:
(a) material inlet of graphite oxide from reaction chamber dropped into the reaction chamber; Said reaction chamber has first gas inlet, second gas inlet and a said material inlet; Said three inlets are positioned at other any walls except that diapire, and its diapire is to open; And in reaction chamber, feed rare gas element through first gas inlet of reaction chamber;
(b) close first gas inlet, in reaction chamber, feed hot inert gas through second gas inlet, make graphite oxide reaction and
(c) by the diapire blown inert gas of first gas inlet facing to reaction chamber, this diapire is opened, the Graphene of generation gets into sample collection room under the blowing of rare gas element.
The present invention also provides a kind of Graphene, and its specific surface area can reach 300-500m
2/ g, preferred 350-480m
2/ g; COR (atomic ratio) can reach 7:1 to 10:1, preferred 8:1 to 10:1.
Equipment of the present invention and method can prepare Graphene continuously.In addition, equipment of the present invention is the basis of Graphene of accomplishing scale production, and helps the scale operation Graphene.The Graphene that is obtained by the present invention has good quality, for example has high specific surface area and high COR.
Description of drawings:
Fig. 1 is a synoptic diagram of present device.
Embodiment:Among the present invention, term " top ", " top ", " bottom ", " level ", " inclination " etc. all are for the level ground.
" rare gas element " is meant the material of under reaction conditions, not participating in the Graphene reaction directly, for example, and one or more rare gas.
If no special instructions, " rare gas element " is in room temperature or near room temperature (room temperature ± 5 ℃).
" hot inert gas " is meant that temperature is 500-2000 ℃ a rare gas element.
The invention provides a kind of equipment for preparing Graphene, it comprises:
(1) reaction chamber has first gas inlet, second gas inlet and a material inlet, and said three inlets are positioned at other any walls except that diapire, and its diapire be openable and
(2) sample collection room that are positioned at the reaction chamber below.
Fig. 1 is a synoptic diagram of present device, and hereinafter will combine Fig. 1 that present device is specified.But should be understood that said accompanying drawing is merely exemplary, should not be construed as to limit the scope of the invention by any way.
As shown in Figure 1, present device comprises a reaction chamber 3.Its shape is not had special qualification, can be spherical, cube shaped like (preferably cube shaped) such as the octahedral bodily form, the square bodily forms; Its wall thickness is generally 6-120mm, but is not limited thereto, and is preferably 50-100mm.
On the wall of reaction chamber 3 (except that diapire 4) material inlet 8 is arranged, be preferably placed on the roof of reaction chamber 3, can directly link to each other, preferably link to each other through one section passage with reaction chamber, as shown in Figure 1.
Preferred this material inlet links to each other with an automatic feeder system.This automatic feeder system can comprise transport unit 11 and reaction mass 10 (being graphite oxide in the present invention).
Said transport unit 11 can be travelling belt, head tank etc., but is not limited thereto.This transport unit can be level or tilt, be preferably level.Under its situation for inclination, preferred inclination angle is below 60 degree.
Also have first gas inlet 7 and second gas inlet 12 on the wall of reaction chamber 3 (except that diapire 4), they join with a compressed air source unit separately, come the pilot-gas flow velocity through the valve of controlling compressed air source unit.
The diapire of reaction chamber 3 (thickness is 6-120mm, preferred 50-100mm) is openable: can pneumaticly open that (being pneumatic diapire), electronic opening (being electronic diapire) or hydraulic pressure are moving opens (being the moving diapire of hydraulic pressure); Preferably can pneumaticly open.
In a specific embodiments, said diapire is pneumatic diapire, and this diapire is divided into two; Be connected on the sidewall of reaction chamber 3 through two rotatable shafts respectively; Be equipped with pressure pneumatic transmitter (it being had no special requirements) below the every diapire, when facing toward this diapire leading portion (being meant the seam crossing of two diapires) blown inert gas by first gas inlet 7 as long as the ability embodiment of the present invention; Produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs.
In a specific embodiments, said diapire is electronic diapire, and this diapire is divided into two; Be connected on the sidewall of reaction chamber 3 through two rotatable shafts respectively; Be equipped with pressure electrodynamictransducer (it is had no special requirements, as long as can embodiment of the present invention) below the every diapire, when facing toward the seam crossing that this diapire leading portion is meant two diapires by first gas inlet 7) during blown inert gas; Produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs.
In a specific embodiments, said diapire is the moving diapire of hydraulic pressure, and this diapire is divided into two; Be connected on the sidewall of reaction chamber 3 through two rotatable shafts respectively; Be equipped with hydrauliccapsule (it being had no special requirements) below the every diapire, when facing toward this diapire leading portion (being meant the seam crossing of two diapires) blown inert gas by first gas inlet 7 as long as the ability embodiment of the present invention; Produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs.
Preferably, the compressed air source unit that said second gas inlet 12 connects is connected with a well heater 2, is used to heat the rare gas element that is got into by gas inlet 1, and the gas through heating gets in the reaction chamber 3 via second gas inlet 12 then, makes the graphite oxide reaction.Wherein said well heater can maybe can be electrically heated, magnetic heating, electromagnetism heating, steam heating etc. through the Cowper stove heating.
The direction of the rare gas element that in reaction chamber, is blown into by second gas inlet 12 should be parallel or away from the reaction chamber diapire, in order to avoid diapire imperfect tense is opened in reaction, preferred parallel is in diapire.
The below of diapire is a sample collection room 5.The Graphene that generates gets into this collecting chamber through the diapire of opening, and in the entering process, cools off with inert gas flow.
Preferably, sample collection room 5 links to each other with a final sampling hut 6 with a sample channel 13 successively.The Graphene that generates gets into sample channel 13 under air-flow and action of gravity, in passing the process of this passage, further cool off, and the type of cooling is naturally cooling or cools off by heat-eliminating medium.End (lower end) at sample channel 13 is connected with a final sampling hut 6, and sample finally is cooled to the temperature that can take out therein.
The waste gas that generates in the reaction process is preferably discharged through an outlet port.Discharge realizes by the inert gas flow that is fed by at least one first gas inlet 7.Said outlet port can be the relief outlet 9 (as shown in fig. 1) that is separately located in reaction chamber top.In addition, under the situation more than one first gas inlet 7, said outlet port also can be one first gas inlet 7.
Preferably, outlet port links to each other with a waste gas recovering device (preferred carbon trap setting), to reclaim waste gas and to be used.
The present device concrete structure is not limited to a kind of ad hoc structure by design feature decision itself.
Each parts of present device are preferably by identical or different high temperature alloy; For example high temperature steel or blast furnace hood steel constitute, and the temperature of fusion that wherein constitutes the material of reaction chamber 3 should be higher than the top temperature (temperature of reaction among the present invention is 500-2000 ℃) in the reaction process.
In addition, the invention provides a kind of method for preparing Graphene, it may further comprise the steps:
(a) material inlet of graphite oxide from reaction chamber dropped into the reaction chamber; Said reaction chamber has first gas inlet, second gas inlet and a said material inlet; Said three inlets are positioned at other any walls except that diapire, and its diapire is to open; And in reaction chamber, feed rare gas element through first gas inlet of reaction chamber;
(b) close first gas inlet, in reaction chamber, feed hot inert gas through second gas inlet, make graphite oxide reaction and
(c) by the diapire blown inert gas of first gas inlet facing to reaction chamber, this diapire is opened, the Graphene of generation gets into sample collection room under the blowing of rare gas element.
Below in conjunction with Fig. 1 a specific embodiments of the inventive method is described.
Step (a): graphite oxide is dropped in the reaction chamber of present device via material inlet 8 through a transport unit 11, and in reaction chamber 3, feed rare gas element, make the indoor rare gas element that is full of of entire reaction through first gas inlet 7.
Graphite oxide any method known in the art capable of using, preferred conventional H ummers method (Ha Mosi method) or improved Hummers method (improved Ha Mosi method), graphite oxide starting material and making, or be commercially available.The purity of used graphite raw material is＞99%, granularity＜45 micron, preferred size＜25 micron.Graphite oxide should have high degree of oxidation, so that prepare high-quality Graphene product, said degree of oxidation is C/O (atomic ratio)＜5:1, is preferably C/O=2:1.
The process that conventional H ummers method prepares graphite oxide is: with powdered graphite and strong oxidizer; For example SODIUMNITRATE, the vitriol oil (for example 98 quality %), potassium permanganate, ydrogen peroxide 50 etc. mix stirring; The reaction some hrs obtains pale brown colored stone China ink oxide powder after cleaning, dewater, drying.
An operational instances of above-mentioned conventional H ummers method is: (consumption is with three kinds of compound forms with powdered graphite, the vitriol oil (for example 98 weight % concentration) and SODIUMNITRATE; By the pure substance part by weight; Graphite: sulfuric acid: SODIUMNITRATE=5-10:150-450:2-8) mix stirring remains on mixing solutions in the ice bath simultaneously; (consumption is by the pure substance part by weight, graphite: potassium permanganate=5-10:10-35), stir slowly to add potassium permanganate; Slowly add deionized water; This moment, solution temperature rose sharply (temperature is 80-100 ℃), kept this temperature, and (consumption is by the pure substance part by weight slowly to add deionized water and ydrogen peroxide 50; Graphite: water: ydrogen peroxide 50=5-10:200-500:6-16), solution colour becomes golden yellow.Solution is carried out centrifugal treating, clean with deionized water, hydrochloric acid and absolute ethyl alcohol again, in case of necessity the repeated washing process.With the centrifugal pale brown look solid oven dry that obtains, finally obtain the graphite oxide powder.
An operational instances of improved Hummers method is:
The first step according to conventional H ummers method, adds graphite in the vitriol oil, SPA, Potcrate (consumption is by the pure substance part by weight, graphite: sulfuric acid: phosphoric acid: Potcrate=(5-10): (100-400): (20-33): (10-35)); Or after graphite is immersed in the vitriol oil (for example 98 weight % concentration), add potassium permanganate (consumption is by the pure substance part by weight, graphite: sulfuric acid: potassium permanganate=(5-10): (150-450): (10-35)),
Second step, at room temperature stir, add water and ydrogen peroxide 50 (consumption is by the pure substance part by weight, graphite: water: ydrogen peroxide 50=(5-10): (200-500): (6-16)); Or at room temperature stir, heating (temperature is 80-100 ℃) adds water and ydrogen peroxide 50 (consumption is by the pure substance part by weight, graphite: water: ydrogen peroxide 50=(5-10): (200-500): (6-16)).
In addition, also can use other improved Hummers methods to prepare graphite oxide.
Said transport unit can be travelling belt or head tank etc., but is not limited thereto.The transfer rate of transport unit is 0.5-3 m/s, preferred 1-2 m/s.
The preferred argon gas of said rare gas element.The time that feeds rare gas element is generally 10-30 minute; Flow velocity is a 1-5 L/min/L chamber volume.In this step, the pressure of rare gas element is generally 0.5-2 normal atmosphere in the reaction chamber, is preferably 1-1.5 normal atmosphere.
Step (b): be passed in reaction chamber 3 and the reaction times of lasting 5-60s through second gas inlet 12 hot inert gas, make the graphite oxide reaction.
The preferred argon gas of rare gas element described herein is heated to 500-2000 ℃ via well heater 2, and preferred 800-1800 ℃, further preferred 1000-1800 ℃; Feed in the reaction chamber 3 through second gas inlet 12 then, make the graphite oxide reaction.Said well heater can maybe can be electrically heated, magnetic heating, electromagnetism heating, steam heating etc. through the heating of internal combustion type hot blast reaction chamber, preferred electrically heated.The flow velocity that hot inert gas feeds in the reaction chamber 3 is a 0.1-10 L/min/L chamber volume, preferred 1-5 L/min/L chamber volume.In addition, the direction of the rare gas element that is fed by second gas inlet 12 should face toward diapire, and should be parallel or away from diapire, in order to avoid diapire imperfect tense is opened reacting, preferred parallel is in diapire.
Graphite oxide reacts on the diapire that is positioned at reaction chamber 34, the reaction times look adding graphite oxide amount and decide, be generally 5-60s, preferred 10-40 s.Reaction pressure is generally 0.5-2 normal atmosphere, is preferably 1-1.5 normal atmosphere.
Step (c): by diapire 4 blown inert gas of first gas inlet 7 facing to reaction chamber 3, this diapire is opened, the Graphene of generation gets into sample collection room 5 under the blowing of rare gas element.
Said diapire is preferably pneumatic diapire; Be divided into two; Be connected on the sidewall of reaction chamber 3 through two rotatable shafts respectively, be equipped with the pressure pneumatic transmitter below the every diapire, when by first gas inlet 7 facing to this diapire leading portion (being meant the seam crossing of two diapires) when being blown into rare gas element; Produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs.The temperature of the rare gas element that is blown into should be lower than the indoor temperature of reaction afterreaction at least, is preferably room temperature or subambient gas.Gas flow rate is so that diapire 4 braking is opened exceeds, and its flow velocity is a 0.1-10 L/min/L chamber volume usually, preferred 1-5 L/min/L chamber volume.
For electronic diapire; Opening procedure is following: diapire is divided into two; Be connected on the sidewall of reaction chamber 3 through two rotatable shafts respectively, be equipped with the pressure electrodynamictransducer below the every diapire, when by first gas inlet 7 during facing to this diapire leading portion (being meant the seam crossing of two diapires) blown inert gas; Produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs.
For the moving diapire of hydraulic pressure; Opening procedure is following: diapire is divided into two; Be connected on the sidewall of reaction chamber 3 through two rotatable shafts respectively, be equipped with hydrauliccapsule below the every diapire, when by first gas inlet 7 during facing to this diapire leading portion (being meant the seam crossing of two diapires) blown inert gas; Produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs.
The temperature of rare gas element should be lower than the temperature in reaction chamber this moment at least, is preferably room temperature or subambient gas.
The Graphene that the reaction back is generated flows in the sample collection room 5 with rare gas element via the diapire of opening 4, and in the entering process, cools off with inert gas flow.
Preferably, the Graphene in the sample collection room 5 gets in the final sampling hut 6 through a coupled sample channel 13.Purpose is to make Graphene through further cooling in the process of sample channel 13, and the type of cooling is naturally cooling or cools off by heat-eliminating medium.
In addition, under the blowing of rare gas element, the waste gas that produces in the reaction is discharged via an outlet port.Said outlet port can be the relief outlet 9 (as shown in Figure 1) that is separately located in reaction chamber top.In addition, under the situation more than one first gas inlet 7, said outlet port also can be one first gas inlet 7.Preferably, outlet port links to each other with a waste gas recovering device, to reclaim waste gas and to be used.Said waste gas recovering device is preferably a carbon trap setting.
Implement above-mentioned steps (a) to (c) through circulation, can realize the continuous production of Graphene.
Can prepare Graphene continuously through present device and method, help the large-scale production of Graphene.In addition, obviously, the automated operation process is more stable than manual operation.Its specific surface area of Graphene that is made by said equipment and method can reach 300-500m
2/ g, preferred 350-480m
2/ g; COR (atomic ratio) can reach 7:1 to 10:1, preferred 8:1 to 10:1.
Embodiment
Hereinafter will more be described in detail the present invention with reference to specific embodiment and comparative example, but the invention is not restricted to these embodiment.
Used graphite oxide all utilizes following conventional H ummers method to make among the embodiment:
Powdered graphite (5 g, granularity is 44 microns), the vitriol oil (concentration is 98 quality %, 115 ml) and SODIUMNITRATE (2.5 g) are packed in the container of one 1 L, simultaneously this container is remained in 0 ℃ the ice bath, mix and stir; Under condition of stirring, slowly add potassium permanganate (15 g) then, continue to stir 30 minutes; Slowly add deionized water (230 ml) afterwards, this moment, solution temperature rose sharply 98 ℃.After 15 minutes, slowly add deionized water (230 ml) and ydrogen peroxide 50 (5 ml), solution colour becomes golden yellow.Solution is carried out 5 minutes centrifugal treating in whizzer (3200 rev/mins), with the product of centrifugation with deionized water (500ml), hydrochloric acid (concentration is 20 volume %, 500ml) and absolute ethyl alcohol (500ml) clean successively.Repeated washing 3 times obtains pale brown look solid graphite oxide compound, with its oven dry (40 ℃, 12 hours), grinds, and is for use.
Embodiment1; Adopt device shown in Figure 1 (two first gas inletes 7; One second gas inlet 12, entire equipment is processed by high temperature steel (GB4238-2007), wall thickness is 50mm) and carry out: the gained graphite oxide is dropped in the reaction chamber via material inlet through the flow velocity of travelling belt with 1m/s; And in reaction chamber 3, fed the room temperature argon gas 10 minutes with the flow velocity of 1L/min/L chamber volume through first gas inlet 7, make in the entire reaction chamber to be full of argon gas; In well heater 2, import argon gas through gas inlet 1 afterwards, heater 2, its argon gas is heated to 1000 ℃ with flowing through; Make argon gas be parallel to diapire via second gas inlet 12 and feed in the reaction chamber 3 then, and continue to feed 30 seconds, make graphite oxide fully reaction in reaction chamber through heating; Open two first gas inletes 7 afterwards; Flow velocity with the 10L/min/L chamber volume is blown into the room temperature argon gas facing to diapire direction in the reaction chamber: diapire is divided into two; Be equipped with pressure pneumatic transmitter (KAL08-U01 KAL08-U01 for example below the every diapire; Available from industrial automation equipment ltd of Dongguan star section); When facing toward this diapire leading portion (being meant the seam crossing of two diapires) blown inert gas by first gas inlet 7, produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs.The Graphene that generates gets under air-flow and action of gravity in the sample collection room 5 below the diapire, gets into final sampling hut 6 via a coupled sample channel 13 then.Open in the process of diapire being blown into argon gas, the reaction chamber waste gas is discharged in the carbon trap setting by outlet port 9.
Embodiment2, by carrying out with embodiment 1 identical process, difference is, the argon gas gas of the well heater 2 of flowing through is heated to 500 ℃, and it is continued to feed 60 seconds in reaction chamber 3.
Embodiment3
,By carrying out with embodiment 1 identical process, difference is, the argon gas gas of the well heater 2 of flowing through is heated to 2000 ℃, and it is continued to feed 5 seconds in reaction chamber 3.
Embodiment4
,By carrying out with embodiment 1 identical process, difference is that diapire is electronic diapire; Open through electric device: diapire is divided into two; Be equipped with pressure electrodynamictransducer (for example KAL08-U01 KAL08-U01, available from industrial automation equipment ltd of Dongguan star section) below the every diapire, when by first gas inlet 7 during facing to this diapire leading portion (being meant the seam crossing of two diapires) blown inert gas; Produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs.
Embodiment5, by carrying out with embodiment 1 identical process, difference is; Diapire is the moving diapire of hydraulic pressure, and open through hydraulicefficiency plant: diapire is divided into two, is equipped with hydrauliccapsule (KAL08-U01 KAL08-U01 for example below the every diapire; Available from industrial automation equipment ltd of Dongguan star section); When facing toward this diapire leading portion (being meant the seam crossing of two diapires) blown inert gas by first gas inlet 7, produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs.
Sample analysis to embodiment 1-5 is following: from final sampling hut, respectively get 1 g sample, it in 150 ℃ of vacuum-dryings 12 hours, is analyzed then: adopt its specific surface area of Quantachrome AUTOSORB-1 test system and test; Adopt PHI 5000 Versa Probe. x-ray photoelectrons ability spectrum testing system and MultiPak V 9.0 digital simulation softwares to measure its carbon/Sauerstoffatom ratio.The result sees the following form:
| Numbering | Specific surface area (m 2/g） | The C/O ratio |
| 500 | 10:1 | |
| |
507 | 9.8:1 |
| |
495 | 9.5:1 |
| |
498 | 9.9:1 |
| |
489 | 10:1 |
Though describe the present invention with reference to particular; But what those skilled in the art will recognize that is; Under the situation that does not depart from purport of the present invention and scope, can change or improve said embodiment, the scope of the invention limits through appended claims.
Claims (10)
1. equipment for preparing Graphene, it comprises:
A reaction chamber has first gas inlet (7), second gas inlet (12) and a material inlet (8), and said three inlets are positioned at other any walls except that diapire (4), and its diapire (4) be openable and
A sample collection room (5) that is positioned at the reaction chamber below.
2. the equipment of claim 1, wherein said diapire is that said diapire is pneumatic diapire, this diapire is divided into two, is connected on the sidewall of reaction chamber (3) through two rotatable shafts respectively, is equipped with the pressure pneumatic transmitter below the every diapire; Be electronic diapire, this diapire is divided into two, is connected on the sidewall of reaction chamber (3) through two rotatable shafts respectively, is equipped with the pressure electrodynamictransducer below the every diapire; Or being the moving diapire of hydraulic pressure, this diapire is divided into two, is connected on the sidewall of reaction chamber (3) through two rotatable shafts respectively, is equipped with hydrauliccapsule below the every diapire; Be preferably pneumatic diapire.
3. the equipment of claim 1, it also has an outlet port, for the relief outlet (9) that is separately located in reaction chamber top or be a gas inlet (7); Said outlet port links to each other with a waste gas recovering device, and said waste gas recovering device is preferably the carbon trap setting.
4. the equipment of claim 1, wherein said material inlet (8) links to each other with an automatic feeder system, and said sample collection room (5) links to each other with a final sampling hut (6) with a sample channel (13) successively.
5. method for preparing Graphene, it may further comprise the steps:
(a) material inlet (8) of graphite oxide from reaction chamber (3) dropped into the reaction chamber (3); Said reaction chamber has first gas inlet (7), second gas inlet (12) and a said material inlet (8); Said three inlets are positioned at other any walls except that diapire (4), and its diapire (4) is to open; And in reaction chamber, feed rare gas element through first gas inlet (7) of reaction chamber (3);
(b) close first gas inlet (7), in reaction chamber (3), feed hot inert gas through second gas inlet (12), make graphite oxide reaction and
(c) by first gas inlet (7) the diapire blown inert gas facing to reaction chamber (3), this diapire is opened, the Graphene of generation gets into sample collection room (5) under the blowing of rare gas element.
6. the method for claim 5, wherein graphite oxide described in the step (a) is by the Ha Mosi method or the preparation of improved Ha Mosi method of routine.
7. the method for claim 5, wherein rare gas element is one or more rare gas described in the step (a) to (c), preferred argon gas.
8. the method for claim 5, wherein the temperature of hot inert gas is 500-2000 ℃ described in the step (b), pressure is 0.5-2 normal atmosphere; Be preferably 1-1.5 normal atmosphere, the feeding time is 5-60s, preferred 10-40 s; Flow velocity is a 0.1-10 L/min/L chamber volume; Preferred 1-5 L/min/L chamber volume, its direction that is passed in the reaction chamber is parallel or away from diapire, preferred parallel is in diapire.
9. the method for claim 5; Wherein diapire is pneumatic diapire described in the step (c), and this diapire is divided into two, is connected on the sidewall of reaction chamber (3) through two rotatable shafts respectively; Be equipped with the pressure pneumatic transmitter below the every diapire; When facing toward this diapire leading portion blown inert gas by first gas inlet (7), produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs; Or be electronic diapire; This diapire is divided into two; Be connected on the sidewall of reaction chamber (3) through two rotatable shafts respectively, be equipped with the pressure electrodynamictransducer below the every diapire, when by first gas inlet (7) during facing to this diapire leading portion blown inert gas; Produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs; Or be that hydraulic pressure moves diapire; This diapire is divided into two; Be connected on the sidewall of reaction chamber (3) through two rotatable shafts respectively, be equipped with the pressure electrodynamictransducer below the every diapire, when by first gas inlet (7) during facing to this diapire leading portion blown inert gas; Produce pressure, diapire is outwarded winding to both sides from the centre around two axle along continuous straight runs.
10. Graphene is obtained by the method for claim 5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106829935A (en) * | 2017-03-27 | 2017-06-13 | 重庆墨希科技有限公司 | The continuous growth apparatus of multi-chamber Graphene of lateral arrangement |
| CN112661141A (en) * | 2021-01-08 | 2021-04-16 | 常州机电职业技术学院 | Equipment for preparing graphene |
| CN112875690A (en) * | 2021-04-29 | 2021-06-01 | 中国恩菲工程技术有限公司 | Graphene synthesis device and graphene synthesis method using same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106829935A (en) * | 2017-03-27 | 2017-06-13 | 重庆墨希科技有限公司 | The continuous growth apparatus of multi-chamber Graphene of lateral arrangement |
| CN106829935B (en) * | 2017-03-27 | 2023-03-24 | 重庆墨希科技有限公司 | Multi-cavity graphene continuous growth equipment arranged transversely |
| CN112661141A (en) * | 2021-01-08 | 2021-04-16 | 常州机电职业技术学院 | Equipment for preparing graphene |
| CN112661141B (en) * | 2021-01-08 | 2023-05-05 | 常州机电职业技术学院 | Equipment for preparing graphene |
| CN112875690A (en) * | 2021-04-29 | 2021-06-01 | 中国恩菲工程技术有限公司 | Graphene synthesis device and graphene synthesis method using same |
| CN112875690B (en) * | 2021-04-29 | 2021-08-31 | 中国恩菲工程技术有限公司 | Graphene synthesis device and graphene synthesis method using same |
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