CN115849354B - Graphene peeling device and graphene peeling method - Google Patents
Graphene peeling device and graphene peeling method Download PDFInfo
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- CN115849354B CN115849354B CN202211598959.0A CN202211598959A CN115849354B CN 115849354 B CN115849354 B CN 115849354B CN 202211598959 A CN202211598959 A CN 202211598959A CN 115849354 B CN115849354 B CN 115849354B
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Abstract
The invention discloses graphene stripping equipment and a graphene stripping method, wherein the graphene stripping equipment comprises a containing barrel, a stripping device and a mixer, wherein a first pipeline communicated with the mixer is arranged between the mixer and the stripping device and is used for conveying mixed materials in the mixer into the stripping device; the stripping device is arranged in the accommodating barrel; the peeling apparatus includes a first assembly having at least one first adhesive panel and a second assembly having at least one second adhesive panel. According to the invention, the first bonding plate and the second bonding plate in the first component and the second component are used for switching back and forth between the separation state and the bonding state, and when the first pipeline sends the mixed material into the stripping device, the first bonding plate and the second bonding plate which are continuously bonded and separated realize stripping of graphite materials in the mixed material, so that the stripping efficiency of graphene in the graphite materials is improved.
Description
Technical Field
The invention relates to the technical field of graphene production equipment, in particular to graphene stripping equipment and a graphene stripping method.
Background
Graphene is a two-dimensional material that was successfully prepared for the first time in the world, with only one layer of hexagonal honeycomb structure of carbon atom thickness. Since the tape method successfully peels off single-layer graphene, graphene is given the name of a universal material, and related research and application work of graphene are carried out in the scientific field and the industry.
At present, the tape method is still the optimal scheme for stripping graphene, and a high-quality single-layer graphene film can be obtained. But the number of graphene layers contained in the graphite thin layer is huge, and the single 0.05mm-0.1mm flake graphite contains 10 5 The graphene layer with the order of magnitude can only obtain partial little single-layer graphene by using a manual stripping method, and is difficult to industrially apply.
Disclosure of Invention
The invention mainly aims to provide graphene stripping equipment and a graphene stripping method, and aims to solve the technical problem of low graphene stripping efficiency in the prior art.
In order to achieve the above object, the present invention provides a graphene peeling apparatus for processing a mixed material of a graphite material and a viscous liquid, the graphene peeling apparatus comprising:
a receiving tub;
the stripping device is arranged in the accommodating barrel;
the mixer is provided with a first pipeline communicated with the stripping device, and the first pipeline is used for conveying the mixed materials in the mixer into the stripping device;
the peeling apparatus includes a first assembly having at least one first adhesive panel and a second assembly having at least one second adhesive panel;
the first bonding plate on the first component is configured to rotate around a first center, the second bonding plate on the second component is configured to rotate around a second center, and the first bonding plate and the second bonding plate are switched back and forth between separation and fitting during movement of the first component and the second component.
In some embodiments of the invention, the direction of rotation of the first adhesive plate on the first assembly is the same as the direction of rotation of the second adhesive plate on the second assembly.
In some embodiments of the present invention, the first assembly further includes a first rotating shaft, at least one first bonding plate is disposed on the first rotating shaft, and the first rotating shaft drives the first bonding plate to rotate around the first rotating shaft;
the second assembly further comprises a second rotating shaft, at least one second bonding plate is arranged on the second rotating shaft, and the second rotating shaft drives the second bonding plate to rotate around the second rotating shaft.
In some embodiments of the present invention, the first rotating shaft and the second rotating shaft are connected together or are connected with a driving component respectively;
the driving assembly comprises a rack, a piston group, a gear meshed with the rack and a turntable rotating around a central axis;
a connecting column is arranged on one side of the turntable;
the piston group comprises a piston pin and a piston, the piston is connected in the piston pin in a sliding way, one end of the piston is connected with the connecting column, and the other end of the piston is connected with the rack;
the gear is connected with the first rotating shaft/the second rotating shaft.
In some embodiments of the present invention, the first adhesive sheet and the second adhesive sheet are the same size and shape.
In some embodiments of the invention, a first temperature regulating device is provided in the mixer, the first temperature regulating device being used for regulating the temperature of the internal environment of the mixer; and/or
The accommodating barrel is internally provided with a second temperature adjusting device, and the second temperature adjusting device is used for adjusting the temperature of the internal environment of the accommodating barrel.
In some embodiments of the present invention, a second pipeline is disposed at the bottom of the accommodating barrel and is communicated with the accommodating barrel, the other end of the second pipeline is connected with the stripping device, and the second pipeline is used for conveying the material in the accommodating barrel to the stripping device.
In some embodiments of the present invention, a third pipeline communicated with the accommodating barrel is arranged at the bottom of the accommodating barrel, and the third pipeline is further connected with a reduced pressure evaporation device, and the reduced pressure evaporation device is used for removing viscous liquid and flushing solvent in the stripped material in the accommodating barrel.
In some embodiments of the present invention, the decompression evaporation device includes a material container, a circulation cooler, and a vacuum pump connected in sequence;
the circulating cooler is also connected with a viscous liquid collector, and a liquid bath heater is arranged outside the material container and is used for heating the material container;
when the decompression evaporation device works, the vacuum pump and the liquid bath heater enable viscous liquid and the flushing solvent in the material containing container to be vaporized under preset working conditions, and the vaporized viscous liquid and the vaporized flushing solvent are cooled through the circulating cooler and are liquefied and collected in the collector, so that the stripped graphene material is obtained in the material containing container.
The embodiment of the invention also provides a graphene stripping method, which comprises the steps of:
mixing the graphite material and the viscous liquid in the mixer according to a preset proportion to form the mixed material, and conveying the mixed material to the stripping device for treatment through the first pipeline;
delivering the materials treated by the stripping device into the stripping device again for reprocessing, and if the reprocessed materials do not reach the preset stripping standard, continuing delivering the stripped materials into the stripping device again for stripping;
repeating the steps until the stripping effect of the material processed by the stripping device reaches the preset stripping standard;
and separating the stripping materials reaching the preset stripping standard to obtain the graphene material.
According to the invention, the stripping device is arranged in the accommodating barrel, and the first bonding plate and the second bonding plate in the first component and the second component are used for switching back and forth between the separating state and the attaching state, so that when the first pipeline conveys the mixed material into the stripping device, the first bonding plate and the second bonding plate are continuously attached and separated, and the mechanical structure is used for applying an acting force to graphene in the graphite material instead of the traditional tape method, so that the graphite material in the mixed material is stripped, and the stripping efficiency of the graphene in the graphite material is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of a graphene peeling apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the kinematic fit of a first component (single bond plate) and a second component (single bond plate) according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of the kinematic fit of a first component (double bond plate) and a second component (double bond plate) according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of a first component (second component) according to an embodiment of the present invention;
FIG. 5 is a schematic view of a first component (second component) according to another embodiment of the present invention;
FIG. 6 is a schematic diagram of a driving assembly according to an embodiment of the invention;
FIG. 7 is a schematic view of a mixer according to an embodiment of the invention;
FIG. 8 is a schematic view of a mixer according to yet another embodiment of the invention;
FIG. 9 is a schematic view of a feeder according to an embodiment of the present invention;
FIG. 10 is a schematic view showing the positional relationship between the feeder and the first component (second component) according to an embodiment of the present invention;
FIG. 11 is a schematic view showing the positional relationship between the feeder and the first member (second member) according to still another embodiment of the present invention.
Reference numerals: 100. a receiving tub; 101. a second temperature regulating device; 200. a mixer; 301. a first pipeline; 302. a second pipeline; 303. a third pipeline; 400. a decompression evaporation device; 401. a material container; 402. a vacuum pump; 403. a circulation cooler; 404. a liquid bath heater; 405. a viscous liquid collector; 500. a first component; 501. a first adhesive sheet; 502. a first rotation shaft; 600. a second component; 601. a second adhesive sheet; 602. a second rotation shaft; 701. a turntable; 702. a connecting column; 703. a piston pin; 704. a piston; 705. a rack; 706. a gear; 800. and a feeder.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that all directional indicators (such as up, down, left, right, front, and rear … …) in the embodiments of the present invention are merely used to explain the relative positional relationship, movement, etc. between the components in a particular posture (as shown in the drawings), and if the particular posture is changed, the directional indicator is changed accordingly.
In the present invention, unless specifically stated and limited otherwise, the terms "connected," "affixed," and the like are to be construed broadly, and for example, "affixed" may be a fixed connection, a removable connection, or an integral body; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In addition, if there is a description of "first", "second", etc. in the embodiments of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In addition, the meaning of "and/or" as it appears throughout includes three parallel schemes, for example "A and/or B", including the A scheme, or the B scheme, or the scheme where A and B are satisfied simultaneously. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
As shown in fig. 1 to 5, the present invention provides a graphene peeling apparatus for treating a mixture of a graphite material and a viscous liquid, the graphene peeling apparatus including a receiving tub, a peeling device, a mixer, and a first pipe communicating the mixer and the peeling device.
The peeling apparatus includes a first assembly having at least one first adhesive panel and a second assembly having at least one second adhesive panel.
One possible embodiment of the peeling apparatus is that the first adhesive plate on the first assembly is configured to rotate about a first center, the second adhesive plate on the second assembly is configured to rotate about a second center, and the first and second assemblies are switched back and forth between separation and attachment during movement of the first and second adhesive plates.
In this embodiment, the first assembly includes a first rotating shaft and a first bonding plate connected to the first rotating shaft along a length direction of the first rotating shaft, and the first bonding plate may be directly connected to the first rotating shaft or may be connected to the first rotating shaft through a connecting piece, and the first bonding plate connected to the first rotating shaft rotates around the first rotating shaft under the driving of the first rotating shaft.
The second assembly comprises a second rotating shaft and a second bonding plate connected with the second rotating shaft along the length direction of the second rotating shaft, the second bonding plate can be directly connected with the second rotating shaft, the second bonding plate can also be connected with the second rotating shaft through a connecting piece, and the second bonding plate rotates around the second rotating shaft under the driving of the second rotating shaft.
In the arrangement of the first and second assemblies, in order to enable the first and second adhesive plates to be attached to each other, detached after attachment, and attached after detachment along with respective rotations, the rotation centers of the first and second rotation shafts may be arranged on the same line, and a distance between the first and second rotation shafts may be smaller than or equal to a maximum width in the first and second adhesive plates, so that the first and second adhesive plates may have portions that are in contact with each other during rotation.
In the arrangement of the first and second modules, the first and second adhesive plates may have the same shape and size so as to increase the bonding degree and the overlapping area of each bonding as much as possible during the respective rotations of the first and second adhesive plates. In addition, the distance between the first rotation axis and the second rotation axis is configured such that the first bonding plate and the second bonding plate are completely bonded when the first bonding plate and the second bonding plate are bonded. For example, when the first adhesive plate is directly connected and fixed to the first rotation shaft and the second adhesive plate is directly connected and fixed to the second rotation shaft, the interval between the first rotation shaft and the second rotation shaft is the width of the first adhesive plate.
In the arrangement of the first and second modules, the first adhesive plate of the first module may be rotated in the same direction as the second adhesive plate of the second module so that the first adhesive plate and the second adhesive plate are bonded to each other in each rotation. And in order to further ensure that the first bonding plate of the first assembly and the second bonding plate of the second assembly can be bonded at least once in each rotation, the rotation speed of the first rotation shaft is the same as the rotation speed of the second rotation shaft.
Based on the above description, one skilled in the art may further adopt an embodiment in which the peeling apparatus includes a first assembly having a first rotation shaft and a first adhesive sheet attached to the first rotation shaft; the second component is provided with a second rotating shaft and a second bonding plate connected to the second rotating shaft, and the first bonding plate and the second bonding plate are the same in size and shape; the first rotating shaft and the second rotating shaft are arranged at intervals, and the rotating direction of the first rotating shaft is the same as the rotating direction of the second rotating shaft and the rotating speed is the same; the first rotating shaft and the second rotating shaft are parallel to each other and have a distance equal to the width of the first bonding plate.
Also, the person skilled in the art can further adopt an embodiment based on the above description, wherein the first rotating shaft is provided with two first bonding plates oppositely connected to the first rotating shaft, and an included angle between the two first bonding plates is 180 degrees; two second bonding plates which are oppositely connected to the first rotating shaft are arranged on the second rotating shaft, and an included angle between the two second bonding plates is 180 degrees; the first bonding plate and the second bonding plate are identical in size and shape in bending, and the distance between the first rotating shaft and the second rotating shaft is equal to the width of the first bonding plate.
Based on the above technical solution, one embodiment that can be adopted by a person skilled in the art is that for the first rotation axis and the second rotation axis, two different motors can be directly used for driving respectively.
Referring to fig. 6, in other possible embodiments, the first rotational axis (and/or the second rotational axis) is driven by a drive assembly. The driving assembly comprises a rack, a piston group, a gear meshed with the rack and a rotary table driven by a motor, the rotary table rotates around the central axis of the rotary table under the driving of the motor, and a connecting column is arranged on one side of the rotary table.
The piston group comprises a piston pin and a piston, the piston is connected in the piston pin in a sliding way, one end of the piston is connected with the connecting column, and the other end of the piston is connected with the rack; when the connecting column rotates along with the turntable, one end of the piston moves back and forth in the piston pin as the piston is connected with the connecting column; that is, the piston moves back and forth on its straight line, the other end of the piston is connected with a rack, the rack follows the piston to move back and forth, and a gear connected with the first rotating shaft (or the second rotating shaft) is meshed with the rack, when the rack follows the piston to move back and forth along the straight line, the gear rotates back and forth on the rack, thereby driving the first rotating shaft (or the second rotating shaft) to rotate back and forth.
Other driving methods may be used by those skilled in the art to drive the first rotation shaft and the second rotation shaft, and will not be described in detail herein.
The first bonding plate (and the second bonding plate) may be made of metal stainless steel, aluminum alloy, titanium alloy, magnesium alloy, zinc alloy, polymer polytetrafluoroethylene, polyurethane, polyvinyl chloride, at least one of natural wood board and natural rubber, or related composite materials.
In some embodiments, the roughness profile arithmetic mean deviation Ra of the first bonding plate (second bonding plate) is 0.2 μm to 25 μm, which can prevent the bonding plate surface from being excessively rough, the large particle material from being stuck in the surface gap, and thus cannot be bonded to reduce the peeling efficiency.
In some possible embodiments, the cross section of the first bonding plate and/or the second bonding plate may be rectangular or trapezoid, in the case of only one bonding plate or less bonding plates, the bonding plates with rectangular cross sections are tightly attached between the fan blades after rotating and bonding, but in the state of multiple bonding plates, if the cross section is still rectangular, the problem of loose attachment exists between the bonding plates, and the trapezoidal design of the cross section can greatly improve the attachment degree of the bonding plates, so the cross section of the bonding plates is the cross section of the bonding plates along the length direction of the first rotation axis or the second rotation axis.
In view of the foregoing, it will be appreciated by those skilled in the art that in the case of any one of the above embodiments, the present invention improves the efficiency of peeling graphene from a graphite material by providing a peeling apparatus in a receiving tub, and using the first and second bonding plates in the first and second assemblies to switch back and forth between separated and bonded states, wherein when a first pipeline feeds a mixture into the peeling apparatus, the bonded and separated first and second bonding plates effect peeling of the graphite material from the mixture.
The accommodating barrel is used for accommodating the mixed materials and the stripped materials, and the stripping device is arranged in the accommodating barrel. The stripping device can be adapted to the size of the receiving tub, leaving at least one fifth of the space at the bottom of the receiving tub for carrying stripped material.
Referring to fig. 7-8, in some possible embodiments, a mixer for mixing the graphite material and the viscous liquid is provided in an open configuration, and the shape may be rectangular, square, funnel, bucket, cylinder, inverted cone, or the like.
In order to increase the volume of the mixer, the bottom of the mixer is arranged to be straight. Wherein, the discharge gate has been seted up to the bottom of blender, and its discharge gate is connected with first pipeline, and the mixed material is carried towards stripping off the device through first pipeline.
On the other hand, a flushing solvent may also be stored in the mixer for flushing the containment drum and the stripping device. Wherein the flushing solvent can be water or at least one of ethanol, xylene, glycerol and glycol. The mixer contains washing solvent for washing the stripping device of the stripping assembly, when the viscosity of the viscous liquid is too high, the mixture flows slowly and is agglomerated on the bonding plate, or graphite materials are bonded and agglomerated on the bonding plate without flowing along with the mixture, the washing solvent is used for washing the bonding plate, and the viscosity of the mixture is properly regulated, so that the mixture flows and the graphite materials are stripped further.
In some possible embodiments, at least one stirring device is provided in the mixer, which comprises an electric motor and stirring blades connected to the electric motor. In order to ensure that the stirring blade does not damage the graphite material during stirring, the rotation speed of the stirring blade is controlled to be less than or equal to 10 revolutions per second.
In some possible embodiments, the mixer is provided with a first temperature regulating device, the first temperature regulating device comprises a heating wire and a cooling circulating pipe, the mixer can be provided with a double-layer hollow structure, the heating wire or the cooling circulating pipe is arranged in the hollow structure, and the temperature inside the mixer is regulated through the heating wire or the cooling circulating pipe. Specifically, the temperature adjustment range is 5-200 ℃.
Referring to fig. 1, in other possible embodiments, a second temperature adjusting device is provided in the accommodating tub, the second temperature adjusting device including a heating wire and a cooling circulation pipe, the accommodating tub may be provided in a double-layered hollow structure in which the heating wire or the cooling circulation pipe is provided, and the temperature inside the accommodating tub is adjusted by the heating wire or the cooling circulation pipe. Specifically, the temperature adjustment range is 5-200 ℃.
The temperature of the mixed material and thus the limit between the viscous liquid and the graphite material in the holding tank or the mixer are adjusted by adjusting the temperature of the mixed material.
Based on the above description, one skilled in the art may further adopt an embodiment that a second pipeline communicated with the accommodating barrel is disposed at the bottom of the accommodating barrel body, and the other end of the second pipeline is connected with the stripping device, where the second pipeline is used for conveying the material in the accommodating barrel to the stripping device.
Referring to fig. 9 to 11, based on the above description, one skilled in the art may further adopt an embodiment in which a feeder is provided at an end of the first pipe connected to the peeling apparatus, and the mixed material fed from the mixer is dispersed onto the first bonding plate and/or the second bonding plate through the feeder. The feeder can be hollow cylinder, and first pipeline is connected to the upper end, and the lower extreme then is provided with slit opening, towards first bonding board or second bonding board, slit opening is not less than 1mm to guarantee that the mixed material flows normally.
In some possible embodiments, the feeder is secured to the first adhesive plate or the second adhesive plate diagonally above either side by a mount.
One end of the first pipeline connected with the stripping device can be provided with a plurality of shunt tubes, and each shunt tube is connected with a feeder.
The connection mode of the second pipeline and the stripping device can also adopt the technical scheme.
In other embodiments, the section of the second conduit at the end connected to the stripping means is provided with a plurality of injection openings so as to inject the material in the second conduit onto the first and second bonding plates.
In other embodiments, the pipe section of the end of the second pipeline connected with the stripping device is annular, and a plurality of jet openings distributed at intervals are arranged on the annular part, and each jet opening is arranged corresponding to one of the first bonding plate or the second bonding plate. It can be understood that the stripped material in the accommodating barrel is stripped again by adopting the second pipeline, so that the stripping success rate can be improved.
The material in the holding tank is transferred to the stripping assembly by using the pump pressure as a driving force in the second pipeline.
In some embodiments, the pump pressure supply device is a compound pump or a diaphragm pump, the pump does not have fan blades or gears and cannot damage the particle size of the graphite material, and particularly, the reciprocating pump or the diaphragm pump is preferably used for stripping graphene with the size of more than 100 μm, the pump circulation pressure is 0.101MPa-10 MPa, and the pipeline diameter is 2mm-50mm.
In some embodiments, the pipeline material of the first pipeline and the second pipeline is at least one of polytetrafluoroethylene, polyethylene, stainless steel and polymer-aluminum film composite, and the material can meet pipeline pressure requirements and ensure long-time normal operation of the device.
The person skilled in the art can see the above solutions for the same arrangement of the first pipelines.
Based on the above description, one skilled in the art may further adopt an embodiment that the bottom of the accommodating barrel is provided with a third pipeline communicated with the accommodating barrel, and the third pipeline is further connected with a reduced pressure evaporation device, where the reduced pressure evaporation device is used for removing the viscous liquid and the flushing solvent in the stripped material in the accommodating barrel.
The viscous liquid is a substance having a boiling point lower than 400 ℃ or removable by distillation under reduced pressure; the catalyst may be stearic acid, paraffin wax, vaseline, etc. and may be glycerin, polyvinylpyrrolidone, polyethylene glycol, etc. The graphite material is stripped by using the viscous liquid, if the viscous liquid is not easy to remove after stripping, graphene is stored in mucus to lose further utilization value, or the mucus is removed by means of high-temperature burning and the like, so that the surface of the graphene is extremely easy to damage, and the quality and the yield of the graphene are reduced, and therefore, the viscous liquid is removed by using a substance with the boiling point lower than 400 ℃ or removable under reduced pressure through a reduced pressure distillation device under relatively mild conditions after stripping is finished, and the graphite material is obtained.
The decompression evaporation device is used for receiving materials discharged from the third pipeline by the accommodating barrel in the graphene stripping equipment and processing the received materials.
It is understood that the processing of the effluent in the graphene stripping system by the reduced pressure evaporation apparatus includes removing viscous liquid and/or rinse solvent from the effluent to obtain a pure graphene material.
Referring to fig. 1, based on the above technical solution, one skilled in the art may further adopt an embodiment, where the reduced pressure evaporation device includes a material container, a circulation cooler, and a vacuum pump connected in sequence. The circulating cooler is also connected with a viscous liquid collector; the liquid bath heater is arranged outside the material container and is used for heating the material container. When the decompression evaporation device works, the vacuum pump and the liquid bath heater enable viscous liquid and flushing solvent in the material containing container to be vaporized under preset working conditions, and the vaporized viscous liquid and flushing solvent are cooled through the circulating cooler and are liquefied and collected in the collector, so that stripped graphene materials are obtained in the material containing container.
Specifically, the accommodating barrel is connected with the material accommodating device through a third pipeline, so that discharged materials in the accommodating barrel are collected into the material accommodating device.
After the discharged materials enter the decompression evaporation device through the third pipeline, the discharged materials are contained in the mixed material container, the vacuum circulating pump provides negative pressure, the liquid bath heating device provides a heat source, the boiling point of viscous liquid in the mixed materials is greatly reduced, the viscous liquid in the mixed materials is vaporized and overflows from the mixed material container, the circulating cooler cools the viscous liquid after being boiled and vaporized, and the viscous liquid enters the collector.
The normal temperature and normal pressure boiling point of the viscous liquid is usually above 150 ℃, the liquid has viscosity, the ultimate negative pressure of a vacuum pump of the device is less than or equal to 0.001MPa, and the liquid is heated relatively uniformly, so that the liquid is heated by adopting a liquid bath, the heating temperature is between room temperature and 300 ℃, and the temperature provided by a circulating cooler is between minus 50 ℃ and room temperature.
The room temperature is in the range of 5℃to 30 ℃.
Based on the above technical solution, the implementation manner that the skilled person can further take in the field is that the graphene production stripping apparatus includes a plurality of accommodating barrels connected in sequence, when the plurality of accommodating barrels are connected in sequence, the stripping devices in the plurality of accommodating barrels are connected in sequence, the stripping device in one accommodating barrel is used for carrying out the stripping treatment again on the material processed by the stripping device in the accommodating barrel connected with the stripping device, and after the stripping treatment is completed, the material is conveyed to the stripping device connected with the next accommodating barrel or the decompression evaporation device connected with the next accommodating barrel.
The invention further provides a graphene stripping method based on the graphene stripping equipment, which comprises the following steps:
s100, mixing graphite materials and viscous liquid in a mixer according to a preset proportion to form a mixed material, and conveying the mixed material to a stripping device for treatment through a first pipeline.
S200, conveying the materials processed by the stripping device to the stripping device again for reprocessing, and if the reprocessed materials do not reach the preset stripping standard, continuously conveying the stripped materials to the stripping device again for stripping.
S300, repeating the step S200 until the stripping effect of the materials processed by the stripping device reaches the preset stripping standard.
S400, separating the stripping materials reaching the preset stripping standard to obtain the graphene material.
The graphite material and the viscous liquid are mixed in a predetermined ratio, where the predetermined ratio is the volume of the viscous liquid (V Mucus Per unit L) and graphite material mass (W Graphite Per unit g).
In some embodiments, the viscous liquid volume (V Mucus Per unit L) and graphite material mass (W Graphite The ratio of/g) is V Mucus :W Graphite ≥0.047。
When the viscous liquid volume (V Mucus Per unit L) and graphite material mass (W Graphite When the total amount ratio per unit g) does not reach the preset ratio, the adjustment can be carried out by adding a flushing solvent.
It will be appreciated that: after the graphite material is peeled into single-layer or multi-layer graphene, the graphene is used for reducing the surface energySpontaneous arrangement or morphology conversion can be performed in the modes of layer surface fluctuation, bending, wrinkling and the like, so that the interlayer spacing of the graphene is increased, and the volume of a corresponding stripping product is increased; the true density of graphite is 2.09-2.33g/cm 3 The volume of 1g of crystalline flake graphite is about 2.09mL-2.33mL, the interlayer spacing of the graphite monolayer is expanded to 3.3nm from initial 0.33nm and expanded by about 10 times, the volume of 1g of crystalline flake graphite is expanded to 20.9mL-23.3mL after the crystalline flake graphite is completely peeled off, the interlayer spacing of the graphite monolayer is expanded to 33nm from initial 0.33nm and expanded by about 100 times, the volume of 1g of crystalline flake graphite is expanded to 209mL-233mL after the crystalline flake graphite is completely peeled off, and in fact, due to the existence of the length Cheng Xizhou, the distance between two layers of graphene at a macroscopic angle is far more than 3.3nm (expanded by 10 times), for example, the expandable graphite becomes expanded graphite after being heated, and the volume can be basically more than 100 times before; therefore, the volume of the graphene material after the graphite material is peeled and expanded is smaller than that of the viscous liquid, the volume advantage of the viscous liquid is ensured, excessive graphene is prevented from being attached to the surface of mucus in a large amount after peeling, the viscous liquid is shielded and prevented from further peeling, and the transmissibility of the viscous liquid is required to be maintained, so that the volume of the mucus is more than 2 times of the volume of the graphite after the graphite material is peeled and expanded.
In the process of mixing graphite material and viscous liquid in a mixer according to a preset proportion to form a mixed material and conveying the mixed material to a stripping device for treatment through a first pipeline in step S100, the method can further comprise the following steps:
s101 adding a graphite material and a viscous liquid to the mixer.
S102, adjusting the temperature inside the mixer through a first temperature adjusting device, so that the viscosity of the viscous liquid can be changed.
S103 starts the stirring device in the mixer and mixes the graphite material and the viscous liquid.
The steps S101, S102, and S103 may be performed simultaneously.
In some embodiments, the viscosity of the viscous liquid is adjusted to 0.5 Pa-s to 30 Pa-s.
And in other embodiments, step S102 may be replaced by adding a regulating solvent to regulate the viscosity of the viscous liquid, where the regulating solvent may be water or at least one of xylene, glycerin, and ethylene glycol.
In other embodiments, the total amount ratio of the graphite material to the viscous liquid is dynamically adjusted, and in such embodiments, the graphene stripping method based on the graphene stripping device comprises the following steps:
s100, adding graphite material and viscous liquid according to a first preset proportion to form a mixed material, and conveying the mixed material to a stripping device for treatment through a first pipeline.
S200, conveying the materials processed by the stripping device to the stripping device again for reprocessing, and if the reprocessed materials do not reach the preset stripping standard, continuously conveying the stripped materials to the stripping device again for stripping.
S300, repeating the step S200 until the stripping effect of the material processed by the stripping device reaches a preset stripping standard; and in the process of repeating the step S200, a flushing solvent or a regulating solvent is added to the mixer to enable the viscous liquid and the graphite material to reach a second preset proportion.
S400, separating the stripping materials reaching the preset stripping standard to obtain the graphene material.
The first preset ratio and the second preset ratio are both viscous liquid volumes (V Mucus Per unit L) and graphite material mass (W Graphite Per unit g). Because the whole stripping process of the graphite material is progressive stripping, the volume of graphene is not expanded in the initial stripping stage, the volume of mucus in the initial stripping stage can be correspondingly smaller, and a flushing solvent or a regulating solvent is additionally added through a later-stage circulating system to regulate V Mucus :W Graphite Proportion, thus adjusting V Mucus :W Graphite The ratio may be adjusted in step S100, or may be adjusted in step S300 by adding a rinse solvent or a conditioning solvent.
It should be noted that, in the first preset proportion and the second preset proportion, V Mucus :W Graphite ≥0.047。
In other embodiments, S200 conveys the material processed by the stripping device to the stripping device again for further processing, and if the material processed again does not reach the preset stripping standard, the material processed by the stripping device is conveyed to the stripping device through the second pipeline in the process of conveying the stripped material to the stripping device again for stripping.
In other embodiments, S400 separates the peeled material that meets the preset peeling standard to obtain a graphene material, which includes separating graphene from the viscous liquid and the rinse solvent by using the reduced pressure evaporation apparatus described above.
The foregoing description is only of the optional embodiments of the present invention, and is not intended to limit the scope of the invention, and all the equivalent structural changes made by the description of the present invention and the accompanying drawings or the direct/indirect application in other related technical fields are included in the scope of the invention.
Claims (9)
1. A graphene peeling apparatus for processing a mixture of a graphite material and a viscous liquid, comprising:
a receiving tub;
the stripping device is arranged in the accommodating barrel;
the mixer is provided with a first pipeline communicated with the stripping device, and the first pipeline is used for conveying the mixed materials in the mixer into the stripping device;
the peeling apparatus includes a first assembly having at least one first adhesive panel and a second assembly having at least one second adhesive panel;
the first bonding plate on the first component is configured to rotate around a first center, the second bonding plate on the second component is configured to rotate around a second center, the first bonding plate and the second bonding plate are switched back and forth between separation and fitting in the process of movement, and the sizes and the shapes of the first bonding plate and the second bonding plate are the same; the interval between the first rotating shaft and the second rotating shaft is configured to ensure that the first bonding plate and the second bonding plate are completely bonded when the first bonding plate and the second bonding plate are bonded;
the viscous liquid includes at least one of: glycerol, polyvinylpyrrolidone, polyethylene glycol;
the volume of the viscous liquid is more than 2 times of the volume of the graphite material expanded by 10 times.
2. The graphene peeling apparatus according to claim 1, wherein a rotation direction of the first bonding plate on the first component is the same as a rotation direction of the second bonding plate on the second component.
3. The graphene peeling apparatus according to claim 1, wherein the first assembly further comprises a first rotation shaft on which at least one of the first bonding plates is disposed, the first rotation shaft driving the first bonding plate to rotate about the first rotation shaft;
the second assembly further comprises a second rotating shaft, at least one second bonding plate is arranged on the second rotating shaft, and the second rotating shaft drives the second bonding plate to rotate around the second rotating shaft.
4. A graphene peeling apparatus according to claim 3, wherein the first and second rotation shafts are connected together or respectively with one driving assembly;
the driving assembly comprises a rack, a piston group, a gear meshed with the rack and a turntable rotating around a central axis;
a connecting column is arranged on one side of the turntable;
the piston group comprises a piston pin and a piston, the piston is connected in the piston pin in a sliding way, one end of the piston is connected with the connecting column, and the other end of the piston is connected with the rack;
the gear is connected with the first rotating shaft/the second rotating shaft.
5. The graphene peeling apparatus according to claim 1, wherein a first temperature adjusting device is provided in the mixer, the first temperature adjusting device being for adjusting a temperature of an internal environment of the mixer; and/or
The accommodating barrel is internally provided with a second temperature adjusting device, and the second temperature adjusting device is used for adjusting the temperature of the internal environment of the accommodating barrel.
6. The graphene peeling apparatus according to claim 1, wherein a second pipeline communicating with the accommodating tub is provided at a bottom of the accommodating tub, and the other end of the second pipeline is connected with the peeling device, and the second pipeline is used for conveying the material in the accommodating tub into the peeling device.
7. The graphene peeling apparatus according to claim 1, wherein a third pipeline which is communicated with the accommodating bucket is provided at the bottom of the accommodating bucket, and the third pipeline is further connected with a reduced pressure evaporation device for removing viscous liquid and a flushing solvent in the peeled material in the accommodating bucket.
8. The graphene peeling apparatus according to claim 7, wherein the reduced pressure evaporation device comprises a material container, a circulation cooler, and a vacuum pump, which are sequentially connected;
the circulating cooler is also connected with a viscous liquid collector, and a liquid bath heater is arranged outside the material container and is used for heating the material container;
when the decompression evaporation device works, the vacuum pump and the liquid bath heater enable viscous liquid and the flushing solvent in the material containing container to be vaporized under preset working conditions, and the vaporized viscous liquid and the vaporized flushing solvent are cooled through the circulating cooler and are liquefied and collected in the collector, so that the stripped graphene material is obtained in the material containing container.
9. A graphene peeling-off method comprising using the graphene peeling-off apparatus according to any one of claims 1 to 8, the graphene peeling-off method comprising the steps of:
mixing the graphite material and the viscous liquid in the mixer according to a preset proportion to form the mixed material, and conveying the mixed material to the stripping device for treatment through the first pipeline;
delivering the materials treated by the stripping device into the stripping device again for reprocessing, and if the reprocessed materials do not reach the preset stripping standard, continuing delivering the stripped materials into the stripping device again for stripping;
repeating the steps until the stripping effect of the material processed by the stripping device reaches the preset stripping standard;
and separating the stripping materials reaching the preset stripping standard to obtain the graphene material.
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