CN112110441A - Graphene high-energy catalytic physical stripping preparation device and method - Google Patents

Graphene high-energy catalytic physical stripping preparation device and method Download PDF

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CN112110441A
CN112110441A CN202011015499.5A CN202011015499A CN112110441A CN 112110441 A CN112110441 A CN 112110441A CN 202011015499 A CN202011015499 A CN 202011015499A CN 112110441 A CN112110441 A CN 112110441A
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column
graphene
cylinder
centrifugal
aqueous solution
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CN112110441B (en
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洪进元
曹利涛
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Dongguan Julei Industry Co ltd
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Dongguan Julei Industry Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • C01B32/19Preparation by exfoliation

Abstract

The invention discloses a high-energy catalytic physical stripping preparation device and a method for graphene, wherein the preparation device comprises a fixed box, an air blowing table used for blowing hot air is arranged on the inner wall of the bottom of the fixed box, a centrifugal column which is connected with the fixed box and driven by a driver is arranged right above the air blowing table, the invention can automatically screen out aqueous solution containing large-size graphene during preparation of graphene through a centrifugal screening cylinder, a discharge printing column and an atomization column, and rapidly dry the aqueous solution to enable the graphene to be attached to the surface of a flexible pattern substrate in a powder form, in the implementation, the aqueous solution of the graphene is sucked in through the centrifugal screening cylinder, the centrifugal column is driven to drive the centrifugal screening cylinder to rotate, so that the large-size graphene is centrifugally screened out along with the aqueous solution, then the filamentous graphene aqueous solution is sprayed out towards the flexible pattern substrate through a spray printing hole, and simultaneously the sprayed filamentous graphene aqueous solution is rapidly dried through a guide sleeve, so that the graphene is directly attached to the surface of the flexible pattern substrate in powder form.

Description

Graphene high-energy catalytic physical stripping preparation device and method
Technical Field
The invention relates to the technical field of graphene preparation, in particular to a high-energy catalytic physical stripping preparation device and method for graphene.
Background
Graphene is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the futureAnd (5) feeding.
The preparation method of the graphene mainly comprises the following steps: 1) a micro-mechanical lift-off method, in which graphene flakes are directly lifted off from a larger crystal; 2) epitaxial growth, i.e., epitaxially growing graphene from the surface of silicon carbide or metal or the like in an ultrahigh vacuum and high temperature environment, 3) oxidation-reduction, the whole process involving oxidizing graphite to graphite oxide, peeling the graphite oxide to produce graphene oxide, and then chemically or thermally reducing the graphene oxide to graphene, 4) Chemical Vapor Deposition (CVD), i.e., using a carbon-containing compound such as methane as a carbon source to prepare graphene through pyrolysis growth on the surface of a substrate.
In the prior art, a chemical method is mostly adopted to prepare graphene, but the method has great influence on the performance of the graphene, and has the problems of serious environmental pollution, high raw material cost, harsh reaction conditions, low yield and the like, so a physical stripping method is also selected for preparation. The acid acts as a "molecular wedge" separating the graphene sheets from the parent graphite. By this simple process, a large amount of undispersed, high quality graphene dispersed in water is produced.
However, graphene is often used after being processed into a certain electronic pattern, but the preparation operation using the ultrasonic waves cannot be used for rapidly processing the graphene into a pattern shape, and although impact force generated by the ultrasonic waves provides driving force for interlayer peeling of graphite, the graphene is also exploded due to non-directionality of the impact force, so that the size of the prepared graphene is reduced.
Disclosure of Invention
The invention aims to provide a high-energy catalytic physical stripping preparation device and method for graphene, and aims to solve the technical problems that after large-size graphene is prepared by ultrasonic waves in the prior art, once the large-size graphene is continuously subjected to frequent ultrasonic impact, the large-size graphene in an aqueous solution is reduced, and subsequent use is easily influenced if the large-size graphene is processed into an electronic pattern shape.
In order to solve the technical problems, the invention specifically provides the following technical scheme:
a graphene high-energy catalysis physical stripping preparation device comprises a fixing box, wherein an air blowing table used for blowing hot air is installed on the inner wall of the bottom of the fixing box, a centrifugal column which is connected with the fixing box and driven by a driver is installed right above the air blowing table, and one end, close to the air blowing table, of the centrifugal column is connected with a quick stripping preparation mechanism;
the fast-disengaging preparation mechanism comprises an ultrasonic cylinder which is directly connected with an air blowing table and is used for preparing graphene suspension, a flexible pattern substrate connected with the air blowing table is sleeved on the outer side of the ultrasonic cylinder, a centrifugal screening cylinder for screening large-size graphene in the graphene suspension is connected to the inner wall of one end, close to a centrifugal column, of the ultrasonic cylinder, a discharge printing column for discharging large-size graphene solution in an atomizing mode is installed on the outer side wall of the centrifugal screening cylinder, and an atomizing column for spraying atomized liquid towards the flexible pattern substrate and drying the liquid fast is installed at one end, far away from the centrifugal screening cylinder, of the discharge printing column;
the atomizing column comprises a fog column body connected with the discharge printing column, a spray printing hole is formed in the fog column body, a flow guide sleeve used for guiding hot air towards the flexible pattern substrate is installed at one end, close to the air blowing table, of the fog column body, and a gas injection inclined cavity used for dredging the discharge printing column is formed in the other end of the fog column body;
the centrifugal screening cylinder inhales the aqueous solution of graphene prepared in the ultrasonic cylinder, and then drives the centrifugal column to drive the centrifugal screening cylinder to rotate, so that large-size graphene is screened out by the centrifugal screen along with the aqueous solution and is led into the fog column body through the discharge printing column, and then the fog column body is sprayed out towards the flexible pattern substrate through the spray printing hole to spray filamentous graphene aqueous solution, and meanwhile, the sprayed filamentous graphene aqueous solution is rapidly dried through the guide sleeve, so that the graphene is directly attached to the surface of the flexible pattern substrate in a powdery manner.
As a preferable scheme of the present invention, the centrifugal screening cylinder includes a cylinder body connected to the ultrasonic cylinder, a liquid storage baffle is installed in the cylinder body, a liquid suction column for inserting an end portion into the ultrasonic cylinder to suck liquid is installed at a central position of the liquid storage baffle, the other end of the liquid suction column penetrates through the fixed box to the outside and is connected to the centrifugal column, a liquid outlet hole is formed in the liquid storage baffle, a movable blocking block for blocking the liquid outlet hole is provided on the liquid storage baffle, a leading-in hole is formed in a side wall of one end of the liquid suction column away from the ultrasonic cylinder, a suction piston column is connected to an inner wall of one end of the liquid suction column away from the ultrasonic cylinder, and a plurality of screening holes are formed in an inner wall of the cylinder body at equal intervals.
As a preferred scheme of the present invention, the movable sealing block includes a plurality of arc-shaped hole sealing strips, an arc-shaped strip chute for accommodating the sliding of the hole sealing strips is formed on the liquid storage blocking piece, a pull-back spring connected to the hole sealing strips is installed on an inner wall of the arc-shaped strip chute, a passage hole corresponding to the liquid outlet hole is formed in the hole sealing strip, and a driving platform is installed at the other end of the hole sealing strip.
As a preferable scheme of the invention, a hole sealing sheet is connected in the filtering hole, a guide chute with a V-shaped longitudinal section is arranged on one side surface of the hole sealing sheet close to the liquid absorption column, a liquid guide column is arranged on the other side surface of the hole sealing sheet, and an atomization hole communicated with the spray printing hole is arranged in the liquid guide column.
As a preferred scheme of the present invention, the discharging printing column includes a connecting cover which is sleeved outside the liquid guiding column and connected with the cylinder, a guide column fixing sleeve is installed in the connecting cover, and a diameter adjusting column which penetrates through the liquid guiding column and is used for adjusting the aperture of the atomizing hole is connected to the guide column fixing sleeve in a threaded manner.
As a preferable scheme of the present invention, the diameter-adjusting column includes a movable column penetrating through the liquid guide column and a threaded column connected to both ends of the movable column and threadedly connected to the guide column fixing sleeve, and a plurality of diameter-adjusting holes having different diameters are formed on the surface of the movable column.
As a preferable scheme of the present invention, a longitudinal section of the gas injection inclined cavity is a parallelogram structure, a rubber piston sheet for pushing gas into the atomization hole is connected in the gas injection inclined cavity, and a connection spring connected with an inner wall of the gas injection inclined cavity is installed on a surface of the rubber piston sheet.
As a preferable scheme of the present invention, one end of the flow guide sleeve, which is far away from the mist cylinder, is connected with an air baffle, an airflow guide post connected with an air blowing table is installed on the air baffle, a predrying channel communicated with the flow guide sleeve and used for jetting hot airflow is arranged in the mist cylinder, the inner side wall of the flexible pattern substrate is connected with the surface of the mist cylinder, and the predrying channel is annularly arranged outside the jet printing hole.
As a preferable scheme of the present invention, one end of the centrifugal column, which is far away from the cylinder, is provided with a distance adjusting sleeve, one end of the suction piston column, which is far away from the cylinder, is provided with an insertion column, and the inner wall of the distance adjusting sleeve is provided with a lifting slide groove for clamping the insertion column and driving the suction piston column to move up and down.
In order to solve the above technical problems, the present invention further provides the following technical solutions:
a preparation method of a graphene high-energy catalytic physical stripping preparation device comprises the following steps:
s100, performing ultrasonic treatment on a mixture of dilute organic acid, alcohol and water in which graphite is soaked in an ultrasonic cylinder by using ultrasonic waves to obtain a graphene dispersion aqueous solution;
s200, driving a centrifugal screening cylinder to rotate at a high speed through a centrifugal column, and simultaneously sucking a graphene dispersed aqueous solution into the centrifugal screening cylinder so as to screen the graphene dispersed aqueous solution in the centrifugal screening cylinder, and simultaneously rotating a diameter-adjusting column up and down to adjust the aperture of an atomization hole so as to discharge the large-size graphene aqueous solution in a filament shape through the atomization hole in a liquid guide column;
s300, driving an air blowing table to blow hot air into the guide sleeve and the pre-drying cavity channel so that the discharged large-size graphene aqueous solution is quickly dried, and driving an atomizing column to slide along the surface of the flexible pattern substrate through a rotating centrifugal screening cylinder so that graphene is attached to the surface of the flexible pattern substrate in a powder shape.
Compared with the prior art, the invention has the following beneficial effects:
the invention can automatically screen out the aqueous solution containing large-size graphene during the preparation of the graphene through the centrifugal screening cylinder, the discharge printing column and the atomization column, and rapidly dry the aqueous solution to enable the graphene to be in a powder shape to be attached to the surface of the flexible pattern substrate, when the method is implemented, the aqueous solution containing the large-size graphene is firstly sucked into the ultrasonic cylinder through the centrifugal screening cylinder, then the centrifugal column is driven to drive the centrifugal screening cylinder to rotate, so that the large-size graphene is centrifugally screened out along with the aqueous solution and is guided into the fog column body through the discharge printing column, then the filamentous graphene aqueous solution is sprayed out towards the flexible pattern substrate through the spray printing hole, and meanwhile, the sprayed filamentous graphene aqueous solution is rapidly dried through the guide sleeve to enable the graphene to be directly in a powder shape to be attached to the surface of the flexible pattern substrate, so that the prepared large-size graphene solution can be prevented from being impacted to reduce the size of the graphene, leading to situations where subsequent use is affected.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
FIG. 1 is a schematic overall structure diagram of an embodiment of the present invention;
FIG. 2 is a top view of a liquid storage baffle according to an embodiment of the invention;
fig. 3 is a schematic structural view of an atomizing column according to an embodiment of the present invention.
The reference numerals in the drawings denote the following, respectively:
1-a stationary box; 2-blowing table; 3-centrifugal column; 4-a quick-release preparation mechanism; 5-centrifugal screening cylinder; 6-discharging the printing column; 7-an atomizing column; 8-an ultrasonic cylinder; 9-a flexible pattern substrate;
301-distance adjusting sleeve; 302-insert column; 303-lifting slide card slot;
501-cylinder body; 502-reservoir flap; 503-liquid absorption column; 504-liquid outlet holes; 505-a movable seal stop; 506-an introduction hole; 507-a suction piston column; 508-screen holes; 509-arc chute; 510-hole sealing sheet; 511-a guide chute; 512-liquid guiding column; 513-atomization holes;
5051-sealing the hole; 5052-pulling back the spring; 5053-a passage hole; 5054-driving the platform;
601-a connection cover; 602-guide post fixing sleeves; 603-diameter adjusting column;
6031-moving column; 6032-threaded post; 6033-diameter adjusting holes;
701-fog column; 702-jet printing holes; 703-a flow guide sleeve; 704-gas injection inclined cavity; 705-rubber piston disc; 706-connecting spring; 707-air blocking sheet; 708-airflow guide columns; 709-pre-trunk cavity channel.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in FIG. 1, the invention provides a graphene high-energy catalytic physical stripping preparation device, which comprises a fixed box 1, wherein an air blowing table 2 for blowing hot air is installed on the inner wall of the bottom of the fixed box 1, a centrifugal column 3 which is connected with the fixed box 1 and driven by a driver is installed right above the air blowing table 2, and one end of the centrifugal column 3, which is close to the air blowing table 2, is connected with a quick stripping preparation mechanism 4.
When the device is used, the mode of accessible centrifugal screening fully guarantees that the graphite alkene that makes is all great size, and in the centrifugal screening process, still can spout the seal operation, spouts the seal operation promptly when screening to avoid the graphite alkene size that makes at last to be lower, and influence the condition of follow-up use and take place.
As shown in fig. 1 and fig. 3, the fast-releasing preparation mechanism 4 includes an ultrasonic cylinder 8 directly connected to the air blowing table 2 and used for preparing graphene suspension, a flexible pattern substrate 9 connected to the air blowing table 2 is sleeved outside the ultrasonic cylinder 8, a centrifugal screening cylinder 5 for screening large-size graphene in the graphene suspension is connected to an inner wall of one end of the ultrasonic cylinder 8 close to the centrifugal column 3, a discharge print column 6 for discharging large-size graphene solution by atomization is installed on an outer side wall of the centrifugal screening cylinder 5, and an atomization column 7 for spraying atomized liquid toward the flexible pattern substrate 9 and drying the liquid quickly is installed at one end of the discharge print column 6 far from the centrifugal screening cylinder 5;
the atomizing column 7 comprises a fog column body 701 connected with the discharge printing column 6, a spray printing hole 702 is formed in the fog column body 701, a flow guide sleeve 703 for guiding hot air towards the flexible pattern substrate 9 is installed at one end, close to the air blowing table 2, of the fog column body 701, and a gas injection inclined cavity 704 for dredging the discharge printing column 6 is formed at the other end of the fog column body 701;
the centrifugal screening cylinder 5 sucks the aqueous solution of the prepared graphene in the ultrasonic cylinder 8, then drives the centrifugal column 3 to drive the centrifugal screening cylinder 5 to rotate, so that large-size graphene is centrifugally screened out along with the aqueous solution and is guided into the fog column body 701 through the discharge printing column 6, then the filamentous graphene aqueous solution is sprayed out towards the flexible pattern substrate 9 through the spray printing holes 702, and meanwhile, the sprayed filamentous graphene aqueous solution is rapidly dried through the guide sleeve 703, so that the graphene is directly attached to the surface of the flexible pattern substrate 9 in a powder shape.
In order to prepare graphene with high yield in the prior art, the patent application number is 201910431302.7, the patent name is a graphene high-energy catalytic physical stripping preparation method, graphene is stripped layer by layer through infiltration, ultrasound, SiC ball milling, a surfactant and secondary high-energy ultrasound, the process is mild, and the phenomena of crushing and abrasion are basically avoided.
When the device is used, mixed liquid of graphite, dilute organic acid and the like can be simultaneously poured into the ultrasonic cylinder 8, then an ultrasonic generator in the ultrasonic cylinder 8 is started, the graphite is subjected to ultrasonic radiation treatment, after graphene is prepared, the centrifugal column 3 can be started to drive the centrifugal screening cylinder 5 to rotate, meanwhile, the centrifugal screening cylinder 5 can suck aqueous solution of the prepared graphene in the ultrasonic cylinder 8, so that large-size graphene is centrifugally screened out along with the aqueous solution and is guided into the fog column body 701 through the discharge printing column 6, the filamentous graphene aqueous solution is sprayed out towards the flexible pattern substrate 9 through the spray printing holes 702, and meanwhile, the sprayed filamentous graphene aqueous solution is rapidly dried through the guide sleeve 703, so that the graphene is directly attached to the surface of the flexible pattern substrate 9 in a powder shape.
As shown in fig. 1, the centrifugal sieving cylinder 5 includes a cylinder 501 connected to the ultrasonic cylinder 8, a liquid storage baffle 502 is installed in the cylinder 501, a liquid absorption column 503 for inserting the end portion into the ultrasonic cylinder 8 to absorb liquid is installed at the center position of the liquid storage baffle 502, the other end of the liquid absorption column 503 penetrates through the fixing box 1 to the outside and is connected to the centrifugal column 3, a liquid outlet 504 is formed in the liquid storage baffle 502, a movable blocking block 505 for blocking the liquid outlet 504 is arranged on the liquid storage baffle 502, a leading-in hole 506 is formed in the side wall of one end of the liquid absorption column 503 far away from the ultrasonic cylinder 8, a sucking piston 507 is connected to the inner wall of one end of the liquid absorption column 503 far away from the ultrasonic cylinder 8, and a plurality of sieving holes 508 are formed in the inner wall of the cylinder 501 at equal.
Further, in order to realize the operation of sucking the graphene aqueous solution into the centrifugal screening cylinder 5 while performing centrifugal screening on the centrifugal screening cylinder 5, i.e. injecting the graphene aqueous solution while performing screening, when the operation is performed, the centrifugal column 3 directly drives the liquid sucking column 503, then the movable liquid sucking column 503 drives the cylinder 501 to rotate, when the cylinder 501 moves, the sucking piston column 507 automatically moves up and down, at the moment, the vertically movable sucking piston column 507 moves along the inner wall of the liquid sucking column 503 (the principle at this moment can refer to an injector), when the sucking piston column 507 moves, the air pressure in the liquid sucking column 503 is repeatedly reduced or increased, so that the graphene aqueous solution in the ultrasonic cylinder 8 continuously enters the liquid sucking column 503 and then enters the cylinder 501 from the liquid outlet 504, at the moment, the rotating cylinder 501 can drive the graphene aqueous solution to perform centrifugal operation, so that the large-size graphene solution is screened out through the screening hole 508, namely, large-size graphene is automatically screened out, so that the graphene aqueous solution generated in the ultrasonic cylinder 8 can continuously enter the cylinder 501, and then the screening operation is performed through the cylinder 501.
The one end that centrifugal column 3 kept away from barrel 501 is installed roll adjustment cover 301, and the one end that suction piston post 507 kept away from barrel 501 is installed and is inserted post 302, has seted up the lift draw-off groove 303 that blocks and insert post 302 and be used for driving suction piston post 507 activity from top to bottom at roll adjustment cover 301's inner wall.
Further, in order to realize the operation that the pumping piston column 507 moves up and down along the liquid absorption column 503 in the rotary screening process of the cylinder 501, when the operation is performed, once the centrifugal column 3 drives the liquid absorption column 503 to rotate, the distance adjusting sleeve 301 moves together, then the movable distance adjusting sleeve 301 drives the insertion column 302 to move through the lifting slide groove 303, and the pumping piston column 507 moves up and down in the moving process of the insertion column 302 to pump the graphene aqueous solution.
In this embodiment, the number of the pumping piston 507 is large, and an electric push rod or other lifting devices may be selected, which is a solution for reducing the number of components.
As shown in fig. 1 and fig. 2, the movable seal stopper 505 includes a plurality of arc-shaped seal strips 5051, an arc-shaped strip chute 509 for accommodating the seal strips 5051 to slide is formed in the liquid storage baffle 502, a pull-back spring 5052 connected to the seal strips 5051 is installed on an inner wall of the arc-shaped strip chute 509, a channel hole 5053 corresponding to the liquid outlet 504 is formed in the seal strip 5051, and a driving table 5054 is installed at the other end of the seal strip 5051.
Further, in order to prevent the aqueous solution entering the cylinder 501 from directly leaking out during the centrifugation process, during the implementation, once the cylinder 501 rotates, the driving table 5054 can have a lateral force and slide along the arc-shaped sliding groove 509, at this time, the movable driving table 5054 can drive the sealing strip 5051 to move together, and at the same time, the pull-back spring 5052 is stretched, so that the sealing strip 5051 has a resetting capability, and at this time, the sealing strip 5051 seals the liquid outlet 504, and then once the cylinder 501 stops rotating, the pull-back spring 5052 can reset and pull the sealing strip 5051, so that the channel 5053 corresponds to the liquid outlet 504, and the aqueous solution can normally flow.
As shown in fig. 1 and 3, a hole sealing sheet 510 is connected in the screening hole 508, a guide chute 511 with a V-shaped longitudinal section is formed on one side surface of the hole sealing sheet 510 close to the liquid absorption column 503, a liquid guide column 512 is installed on the other side surface of the hole sealing sheet 510, and an atomization hole 513 communicated with the spray printing hole 702 is formed in the liquid guide column 512.
Further, in order to enable the screened graphene aqueous solution to smoothly flow out, when the graphene aqueous solution screening device is implemented, the cylinder 501 drives the aqueous solution to perform centrifugal operation, and then the graphene with larger size in the graphene aqueous solution enters the liquid guiding column 512 along the guiding chute 511 along with the aqueous solution contacting the hole sealing sheet 510 and flows out in a filament shape along the atomizing hole 513.
In this embodiment, the diameter of the atomization holes 513 should satisfy the purpose of passing through only large-sized graphene, and if the diameter is too small, the graphene cannot pass through normally, and if the diameter is too large, the size of the screened graphene is not uniform.
As shown in fig. 1 and 3, the discharging print column 6 includes a connection cover 601 sleeved outside the liquid guiding column 512 and connected to the cylinder 501, a guide column fixing sleeve 602 is installed in the connection cover 601, and a diameter adjusting column 603 penetrating the liquid guiding column 512 and used for adjusting the aperture of the atomizing hole 513 is connected to the guide column fixing sleeve 602 by screw.
The diameter-adjusting column 603 is composed of a movable column 6031 penetrating the liquid guide column 512 and a threaded column 6032 connected to both ends of the movable column 6031 and in threaded connection with the guide column fixing sleeve 602, the connection mode at the position can be selected from a T-shaped clamping groove for connection, and a plurality of diameter-adjusting holes 6033 with different apertures are formed in the surface of the movable column 6031.
Furthermore, in order to make the screened graphene aqueous solution pass through the discharging printing column 6, the hole for discharging the graphene aqueous solution is not too large, so the atomizing hole 513 in the liquid guiding column 512 needs to be controlled, when the method is implemented, only the threaded column 6032 needs to be rotated, as shown in fig. 3, if the threaded column 6032 is rotated from bottom to top, the lower threaded column 6032 pushes the movable column 6031 to move along the liquid guiding column 512, and meanwhile, the diameter adjusting hole 6033 with a smaller diameter directly moves into the atomizing hole 513 until the aperture center of the atomizing hole 513 is aligned with the aperture center of the diameter adjusting hole 6033 (when the diameter adjusting hole 6032 is aligned, the threaded column 6032 cannot continuously rotate, that is, the purpose of limiting is achieved through the threaded column 6032).
As shown in fig. 3, the longitudinal section of the gas injection inclined cavity 704 is a parallelogram structure, a rubber piston sheet 705 for pushing gas into the atomization hole 513 is connected in the gas injection inclined cavity 704, and a connecting spring 706 connected with the inner wall of the gas injection inclined cavity 704 is mounted on the surface of the rubber piston sheet 705.
Furthermore, in order to prevent the atomization holes 513 from being blocked when the screened graphene aqueous solution is discharged, once the cylinder 501 rotates, the cylinder 501 and the rubber piston plate 705 have a centrifugal force, at this time, the rubber piston plate 705 moves along the inclined plane of the gas injection inclined cavity 704 under the action of the centrifugal force, and the longitudinal section of the gas injection inclined cavity 704 is of a parallelogram structure, so that the rubber piston plate 705 moves, when the rubber piston plate moves, the connecting spring 706 is stretched, and at the same time, the pressure in the gas injection inclined cavity 704 is reduced to suck gas, and then, once the cylinder 501 stops rotating, the connecting spring 706 resets to pull the rubber piston plate 705 to reset, so that the gas in the gas injection inclined cavity 704 enters the atomization holes 513, and the gas in the atomization holes 513 moves along the atomization holes 513, thereby blowing away the impurities blocked in the cylinder.
As shown in fig. 1 and 3, an air baffle 707 is connected to one end of the flow guide sleeve 703 away from the mist column 701, an airflow guide post 708 connected to the blowing table 2 is installed on the air baffle 707, a predrying cavity 709 communicated with the flow guide sleeve 703 and used for jetting hot airflow is formed in the mist column 701, the inner side wall of the flexible pattern substrate 9 is connected to the surface of the mist column 701, and the predrying cavity 709 is annularly arranged outside the jet printing hole 702.
In this embodiment, the guiding sleeve 703 is annularly installed on the mist cylinder 701, and when the mist cylinder 701 moves, the guiding sleeve 703 also moves, and the air blocking sheet 707 plays a role of sealing.
Further, in order to solve the problem that the graphene aqueous solution is difficult to rapidly adhere to the flexible pattern substrate 9 when being sprayed out, during implementation, hot air flow is directly injected into the air flow guide column 708 through the air blowing table 2, so that the guide sleeve 703 is filled with the hot air flow, then the air flow can directly enter the pre-drying cavity channel 709, when the pre-drying cavity channel 709 is filled with the hot air flow, the spray printing hole 702 can be directly heated, when the fine-line graphene aqueous solution is sprayed out through the spray printing hole 702, the fine-line graphene aqueous solution can be directly and rapidly heated and evaporated, and then the dried graphene can be driven by the hot air flow to be directly spray printed on the surface of the flexible pattern substrate 9.
A preparation method of a graphene high-energy catalytic physical stripping preparation device comprises the following steps:
s100, performing ultrasonic treatment on a mixture of dilute organic acid, alcohol and water in which graphite is soaked in an ultrasonic cylinder by using ultrasonic waves to obtain a graphene dispersion aqueous solution;
s200, driving a centrifugal screening cylinder to rotate at a high speed through a centrifugal column, and simultaneously sucking a graphene dispersed aqueous solution into the centrifugal screening cylinder so as to screen the graphene dispersed aqueous solution in the centrifugal screening cylinder, and simultaneously rotating a diameter-adjusting column up and down to adjust the aperture of an atomization hole so as to discharge the large-size graphene aqueous solution in a filament shape through the atomization hole in a liquid guide column;
s300, driving an air blowing table to blow hot air into the guide sleeve and the pre-drying cavity channel so that the discharged large-size graphene aqueous solution is quickly dried, and driving an atomizing column to slide along the surface of the flexible pattern substrate through a rotating centrifugal screening cylinder so that graphene is attached to the surface of the flexible pattern substrate in a powder shape.
The above embodiments are only exemplary embodiments of the present application, and are not intended to limit the present application, and the protection scope of the present application is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present application and such modifications and equivalents should also be considered to be within the scope of the present application.

Claims (10)

1. The utility model provides a preparation facilities is peeled off to graphite alkene high energy catalysis physics which characterized in that: the device comprises a fixed box (1), wherein an air blowing table (2) used for blowing hot air is installed on the inner wall of the bottom of the fixed box (1), a centrifugal column (3) which is connected with the fixed box (1) and driven by a driver is installed right above the air blowing table (2), and one end, close to the air blowing table (2), of the centrifugal column (3) is connected with a quick release preparation mechanism (4);
the fast-release preparation mechanism (4) comprises an ultrasonic cylinder (8) which is directly connected with an air blowing table (2) and used for preparing graphene suspension, a flexible pattern substrate (9) connected with the air blowing table (2) is sleeved on the outer side of the ultrasonic cylinder (8), a centrifugal screening cylinder (5) used for screening large-size graphene in the graphene suspension is connected to the inner wall of one end, close to a centrifugal column (3), of the ultrasonic cylinder (8), a discharge printing column (6) used for discharging filament-shaped large-size graphene solution is installed on the outer side wall of the centrifugal screening cylinder (5), and an atomization column (7) used for spraying the filament-shaped large-size graphene solution towards the flexible pattern substrate (9) and rapidly drying the liquid is installed at one end, far away from the centrifugal screening cylinder (5), of the discharge printing column (6);
the atomizing column (7) comprises a mist cylinder (701) connected with the discharging printing column (6), a spray printing hole (702) is formed in the mist cylinder (701), a flow guide sleeve (703) used for guiding hot air towards the flexible pattern substrate (9) is installed at one end, close to the air blowing table (2), of the mist cylinder (701), and an air injection inclined cavity (704) used for dredging the discharging printing column (6) is formed in the other end of the mist cylinder (701);
the centrifugal screening cylinder (5) sucks the aqueous solution of prepared graphene in the ultrasonic cylinder (8), then the centrifugal column (3) is driven to drive the centrifugal screening cylinder (5) to rotate, so that large-size graphene is centrifugally screened out along with the aqueous solution and is guided into the fog column body (701) through the discharge printing column (6), then the fine-wire-shaped graphene aqueous solution is sprayed out towards the flexible pattern substrate (9) through the spray printing holes (702), and meanwhile, the sprayed fine-wire-shaped graphene aqueous solution is rapidly dried through the guide sleeve (703), so that the graphene is directly attached to the surface of the flexible pattern substrate (9) in a powder shape.
2. The graphene high-energy catalytic physical stripping preparation device according to claim 1, characterized in that: the centrifugal screening cylinder (5) comprises a cylinder body (501) connected with the ultrasonic cylinder (8), a liquid storage separation blade (502) is arranged in the cylinder body (501), a liquid absorption column (503) with an end part inserted into the ultrasonic cylinder (8) for absorbing liquid is arranged at the central position of the liquid storage separation blade (502), the other end of the liquid absorption column (503) penetrates through the fixed box (1) to the outer side and is connected with the centrifugal column (3), a liquid outlet (504) is arranged on the liquid storage baffle (502), a movable sealing block (505) for sealing the liquid outlet (504) is arranged on the liquid storage baffle (502), a leading-in hole (506) is arranged on the side wall of one end of the liquid absorption column (503) far away from the ultrasonic cylinder (8), and the inner wall of one end of the liquid absorption column (503) far away from the ultrasonic cylinder (8) is connected with a suction piston column (507), a plurality of screening holes (508) are arranged on the inner wall of the cylinder body (501) at equal intervals.
3. The graphene high-energy catalytic physical stripping preparation device according to claim 2, characterized in that: the movable seal stop block (505) comprises a plurality of arc-shaped seal strips (5051), an arc strip sliding groove (509) used for accommodating the seal strips (5051) in a sliding mode is formed in the liquid storage baffle plate (502), a pull-back spring (5052) connected with the seal strips (5051) is installed on the inner wall of the arc strip sliding groove (509), a channel hole (5053) corresponding to the liquid outlet hole (504) is formed in the seal strips (5051), and a driving platform (5054) is installed at the other end of the seal strips (5051).
4. The graphene high-energy catalytic physical stripping preparation device according to claim 2, characterized in that: the inside of the screening hole (508) is connected with a hole sealing sheet (510), one side surface of the hole sealing sheet (510) close to the liquid absorption column (503) is provided with a guide chute (511) with a V-shaped longitudinal section, the other side surface of the hole sealing sheet (510) is provided with a liquid guide column (512), and an atomization hole (513) communicated with the spray printing hole (702) is formed in the liquid guide column (512).
5. The graphene high-energy catalytic physical stripping preparation device according to claim 4, characterized in that: the discharging printing column (6) comprises a connecting cover (601) which is sleeved on the outer side of the liquid guide column (512) and connected with the cylinder body (501), a guide column fixing sleeve (602) is installed in the connecting cover (601), and a diameter adjusting column (603) which penetrates through the liquid guide column (512) and is used for adjusting the aperture of the atomizing hole (513) is in threaded connection with the guide column fixing sleeve (602).
6. The graphene high-energy catalytic physical stripping preparation device according to claim 5, characterized in that: the diameter adjusting column (603) is composed of a movable column (6031) which is connected to the liquid guide column (512) in a penetrating way and a threaded column (6032) which is connected to two ends of the movable column (6031) and is in threaded connection with the guide column fixing sleeve (602), and a plurality of diameter adjusting holes (6033) with different apertures are formed in the surface of the movable column (6031).
7. The graphene high-energy catalytic physical stripping preparation apparatus according to claim 4, wherein a longitudinal section of the gas injection inclined cavity (704) is a parallelogram structure, a rubber piston sheet (705) for pushing gas into the atomization holes (513) is connected in the gas injection inclined cavity (704), and a connection spring (706) connected with an inner wall of the gas injection inclined cavity (704) is mounted on a surface of the rubber piston sheet (705).
8. The graphene high-energy catalytic physical stripping preparation device according to claim 1, wherein one end of the flow guide sleeve (703) far away from the mist cylinder (701) is connected with an air baffle (707), the air baffle (707) is provided with an air flow guide post (708) connected with the air blowing table (2), a predrying cavity channel (709) which is communicated with the flow guide sleeve (703) and is used for spraying hot air is arranged in the mist cylinder (701), the inner side wall of the flexible pattern substrate (9) is connected with the surface of the mist cylinder (701), and the predrying cavity channel (709) is annularly arranged outside the spray printing hole (702).
9. The graphene high-energy catalytic physical stripping preparation device according to claim 1, wherein one end of the centrifugal column (3) far away from the cylinder body (501) is provided with a distance adjusting sleeve (301), one end of the suction piston column (507) far away from the cylinder body (501) is provided with an insertion column (302), and the inner wall of the distance adjusting sleeve (301) is provided with a lifting slide groove (303) which blocks the insertion column (302) and is used for driving the suction piston column (507) to move up and down.
10. The preparation method of the graphene high-energy catalytic physical stripping preparation device according to any one of claims 1 to 9 is characterized by comprising the following steps:
s100, performing ultrasonic treatment on a mixture of dilute organic acid, alcohol and water in which graphite is soaked in an ultrasonic cylinder by using ultrasonic waves to obtain a graphene dispersion aqueous solution;
s200, driving a centrifugal screening cylinder to rotate at a high speed through a centrifugal column, and simultaneously sucking a graphene dispersed aqueous solution into the centrifugal screening cylinder so as to screen the graphene dispersed aqueous solution in the centrifugal screening cylinder, and simultaneously rotating a diameter-adjusting column up and down to adjust the aperture of an atomization hole so as to discharge the large-size graphene aqueous solution in a filament shape through the atomization hole in a liquid guide column;
s300, driving an air blowing table to blow hot air into the guide sleeve and the pre-drying cavity channel so that the discharged large-size graphene aqueous solution is quickly dried, and driving an atomizing column to slide along the surface of the flexible pattern substrate through a rotating centrifugal screening cylinder so that graphene is attached to the surface of the flexible pattern substrate in a powder shape.
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CN102020270A (en) * 2009-09-09 2011-04-20 中国科学院金属研究所 Macro-preparation for big size graphene
US20150071844A1 (en) * 2013-09-12 2015-03-12 The Hong Kong University Of Science And Technology Synthesis of Ultra-Large Graphene Oxide Sheets
CN104817071A (en) * 2015-03-17 2015-08-05 清华大学 Size grading method for graphene material
CN108862257A (en) * 2018-08-02 2018-11-23 无锡泰科纳米新材料有限公司 A kind of preparation method and device of graphene
US20180339906A1 (en) * 2015-11-16 2018-11-29 Fudan University Preparation method for large-size graphene oxide or graphene

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102020270A (en) * 2009-09-09 2011-04-20 中国科学院金属研究所 Macro-preparation for big size graphene
US20150071844A1 (en) * 2013-09-12 2015-03-12 The Hong Kong University Of Science And Technology Synthesis of Ultra-Large Graphene Oxide Sheets
CN104817071A (en) * 2015-03-17 2015-08-05 清华大学 Size grading method for graphene material
US20180339906A1 (en) * 2015-11-16 2018-11-29 Fudan University Preparation method for large-size graphene oxide or graphene
CN108862257A (en) * 2018-08-02 2018-11-23 无锡泰科纳米新材料有限公司 A kind of preparation method and device of graphene

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