CN115849354A - Graphene stripping equipment and graphene stripping method - Google Patents
Graphene stripping equipment and graphene stripping method Download PDFInfo
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- CN115849354A CN115849354A CN202211598959.0A CN202211598959A CN115849354A CN 115849354 A CN115849354 A CN 115849354A CN 202211598959 A CN202211598959 A CN 202211598959A CN 115849354 A CN115849354 A CN 115849354A
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Abstract
The invention discloses graphene stripping equipment and a graphene stripping method, wherein the graphene stripping equipment comprises an accommodating barrel, a stripping device and a mixer, a communicated first pipeline is arranged between the mixer and the stripping device, and the first pipeline is used for conveying a mixed material in the mixer into the stripping device; the stripping device is arranged in the accommodating barrel; the peeling apparatus includes a first member having at least one first adhesive sheet and a second member having at least one second adhesive sheet. According to the stripping device, the first bonding plate and the second bonding plate in the first assembly and the second assembly are switched back and forth between the separation state and the attachment state, when a mixed material is fed into the stripping device through the first pipeline, the first bonding plate and the second bonding plate which are continuously attached and separated realize stripping of the graphite material in the mixed material, and therefore the stripping efficiency of graphene in the graphite material 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 which is successfully prepared for the first time in the world and has a hexagonal honeycomb structure with the thickness of only one layer of carbon atoms. Since the adhesive tape method successfully peels off the single-layer graphene, the graphene is given the name of a universal material, and then researches and application work related to the graphene are carried out in the scientific and industrial fields.
At present, the adhesive tape method stillThe method is an optimal scheme for stripping graphene, and a high-quality single-layer graphene film can be obtained. However, the number of graphene layers contained in the graphite thin layer is huge, and single 0.05mm-0.1mm flake graphite contains 10 5 The graphene layer with the order of magnitude can only obtain partial single-layer graphene with extremely small quantity by a manual stripping method, and industrial application is difficult.
Disclosure of Invention
The invention mainly aims to provide graphene stripping equipment and a graphene stripping method, and aims to solve the technical problem that graphene stripping efficiency is low in the prior art.
In order to achieve the above object, the present invention provides a graphene stripping apparatus for processing a mixed material of a graphite material and a viscous liquid, the graphene stripping apparatus including:
an accommodating barrel;
the stripping device is arranged in the accommodating barrel;
a first pipeline communicated with the mixer is arranged between the mixer and the stripping device, and the first pipeline is used for feeding the mixed material in the mixer into the stripping device;
the peeling apparatus includes a first member having at least one first adhesive sheet and a second member having at least one second adhesive sheet;
the first bonding plate on the first assembly is configured to rotate around a first center, the second bonding plate on the second assembly 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 attachment in the movement process of the first assembly and the second assembly.
In some embodiments of the present invention, the rotation direction of the first bonding plate on the first assembly is the same as the rotation direction of the second bonding plate on the second assembly.
In some embodiments of the present invention, 3 the first assembly further includes a first rotating shaft, the first rotating shaft is provided with at least one first bonding plate, 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 with a driving assembly or connected with a driving assembly respectively;
the driving assembly comprises a rack, a piston group, a gear meshed with the rack and a turntable rotating around a central axis;
one side of the turntable is provided with a connecting column;
the piston group comprises a piston pin and a piston, the piston is slidably connected in the piston pin, 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/second rotating shaft.
In some embodiments of the present invention, the first bonding sheet and the second bonding sheet are the same in size and shape.
In some embodiments of the invention, a first temperature adjusting device is arranged in the mixer, and is used for adjusting the temperature of the internal environment of the mixer; and/or
And a second temperature adjusting device is arranged in the accommodating barrel and is used for adjusting the temperature of the internal environment of the accommodating barrel.
In some embodiments of the present invention, a second pipeline communicated with the accommodating barrel is disposed at the bottom of the accommodating barrel, and the other end of the second pipeline is connected to 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 disposed at the bottom of the accommodating barrel, and the third pipeline is further connected to a pressure-reducing evaporation device, and the pressure-reducing evaporation device is configured to remove the viscous liquid and the rinsing solvent from the peeled material in the accommodating barrel.
In some embodiments of the present invention, the decompression evaporation apparatus includes a material container, a circulation cooler, and a vacuum pump, which are connected in sequence;
the circulating cooler is also connected with a viscous liquid collector, a liquid bath heater is also arranged outside the material container, and the liquid bath heater is used for heating the material container;
when the decompression evaporation device works, the vacuum pump and the liquid bath heater enable the viscous liquid and the flushing solvent in the material containing container to be vaporized under preset working conditions, the vaporized viscous liquid and the flushing solvent are cooled through the circulating cooler, and the viscous liquid and the flushing solvent 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 step of using the graphene stripping equipment, wherein the graphene stripping method comprises the following steps:
mixing the graphite material and the viscous liquid in a mixer according to a preset proportion to form a mixed material, and conveying the mixed material to the stripping device through the first pipeline for treatment;
conveying the material treated by the stripping device into the stripping device again for retreatment, and if the material treated by the retreatment does not reach the preset stripping standard, continuously conveying the stripped material into the stripping device again for stripping;
repeating the steps until the stripping effect of the material treated by the stripping device reaches a preset stripping standard;
and separating the stripping materials meeting 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 assembly and the second assembly are switched back and forth between the two states of separation and attachment, so that when the mixed material is fed into the stripping device through the first pipeline, the first bonding plate and the second bonding plate are continuously attached and separated, and thus, the mechanical structure is used for replacing the traditional tape method to apply acting force on graphene in the graphite material, the graphite material in the mixed material is stripped, and the graphene stripping efficiency 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 used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.
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 illustration of the kinematic fit of a first component (single bond plate) and a second component (single bond plate) of an embodiment of the present invention;
FIG. 3 is a schematic illustration of the kinematic fit of a first component (double bond plate) and a second component (double bond plate) of an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of a first component (a second component) according to an embodiment of the present invention;
FIG. 5 is a schematic view of the first assembly (second assembly) according to yet another embodiment of the present invention;
FIG. 6 is a schematic structural diagram of a driving assembly according to an embodiment of the present invention;
FIG. 7 is a schematic structural diagram of a mixer according to an embodiment of the present invention;
FIG. 8 is a schematic structural diagram of a mixer according to yet another embodiment of the present invention;
FIG. 9 is a schematic structural view of a feeder according to an embodiment of the present invention;
FIG. 10 is a schematic view of the position relationship between the feeder and the first assembly (second assembly) according to an embodiment of the present invention;
FIG. 11 is a schematic view showing the positional relationship between the feeder and the first module (second module) according to still another embodiment of the present invention.
Reference numerals: 100. an accommodating barrel; 101. a second temperature adjustment device; 200. a mixer; 301. a first pipeline; 302. a second pipeline; 303. a third pipeline; 400. a reduced-pressure 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 rotating shaft; 600. a second component; 601. a second adhesive sheet; 602. a second rotating shaft; 701. a turntable; 702. connecting columns; 703. a piston pin; 704. a piston; 705. a rack; 706. a gear; 800. a feeder.
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.
It should be noted that all directional indicators (such as up, down, left, right, front, back \8230;) in the embodiments of the present invention are only used to explain the relative positional relationship between the components, the motion situation, etc. in a specific posture (as shown in the attached drawings), and if the specific posture is changed, the directional indicator is changed accordingly.
In the present invention, unless otherwise expressly stated or limited, the terms "connected," "secured," and the like are to be construed broadly, and for example, "secured" may be a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In addition, if there is a description of "first", "second", etc. in an embodiment 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 relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of the feature. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
As shown in fig. 1 to 5, the present invention provides a graphene peeling apparatus for processing a mixture of a graphite material and a viscous liquid, the graphene peeling apparatus including a holding tank, a peeling device, a mixer, and a first pipeline communicating the mixer and the peeling device.
The peeling apparatus includes a first member having at least one first adhesive sheet and a second member having at least one second adhesive sheet.
One possible embodiment of the peeling apparatus is that the first bonding plate on the first assembly is configured to rotate around a first center, the second bonding plate on the second assembly 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 fit during the movement of the first assembly and the second assembly.
In this embodiment, the first assembly includes a first rotating shaft and a first adhesive plate connected to the first rotating shaft along a length direction of the first rotating shaft, the first adhesive plate may be directly connected to the first rotating shaft or may be connected to the first rotating shaft through a connecting member, and the first adhesive plate connected to the first rotating shaft rotates around the first rotating shaft by 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 above arrangement of the first and second modules, in order to enable the first and second adhesive sheets to be attached to each other, to be separated after attachment, and to be attached after separation as they are rotated, the rotation centers of the first and second rotation shafts may be arranged on the same straight line, and the interval between the first and second rotation shafts may be less than or equal to the maximum width of the first and second adhesive sheets, so that the first and second adhesive sheets may have portions that contact each other during rotation.
In the above arrangement of the first module and the second module, the first adhesive sheet and the second adhesive sheet have the same shape and size so that the first adhesive sheet and the second adhesive sheet can be attached to each other with the highest possible degree of attachment and the overlapping area of the first adhesive sheet and the second adhesive sheet can be increased for each attachment. In addition, the distance between the first rotating shaft and the second rotating shaft is set so 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 sheet is directly fixedly coupled to the first rotating shaft and the second adhesive sheet is directly fixedly coupled to the second rotating shaft, the interval between the first rotating shaft and the second rotating shaft is the width of the first adhesive sheet.
In the above arrangement of the first module and the second module, the first adhesive sheet of the first module may be rotated in the same direction as the second adhesive sheet of the second module so that the first adhesive sheet and the second adhesive sheet can be bonded to each other during their respective rotations. 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 rotating shaft is the same as that of the second rotating shaft.
Based on the above description, one skilled in the art can further adopt an embodiment in which the peeling means includes a first assembly having a first rotating shaft and a first adhesive sheet attached to the first rotating shaft; the second assembly is provided with a second rotating shaft and a second bonding plate connected to the second rotating shaft, and the size and the shape of the first bonding plate are the same as those of the second bonding plate; the first rotating shaft and the second rotating shaft are arranged at intervals, and the rotating direction and the rotating speed of the first rotating shaft are the same as those of the second rotating shaft; the first rotating shaft and the second rotating shaft are parallel to each other, and the distance between the first rotating shaft and the second rotating shaft is equal to the width of the first bonding plate.
Similarly, based on the above description, a person skilled in the art may further adopt an embodiment that two first adhesive plates are oppositely connected to the first rotating shaft, and an included angle between the two first adhesive plates is 180 °; two second bonding plates which are oppositely connected to the first rotating shaft are arranged on the second rotating shaft, and the included angle between the two second bonding plates is 180 degrees; the first bonding plate and the second bonding plate are bent in the same size and shape, 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 those skilled in the art is that two different motors can be used to directly drive the first rotating shaft and the second rotating shaft respectively.
Referring to fig. 6, in other possible embodiments, the first rotating shaft (and/or the second rotating shaft) is driven by a driving assembly. The driving assembly comprises a rack, a piston group, a gear meshed with the rack and a rotary turntable driven by a motor, the turntable rotates around the central axis of the turntable under the driving of the motor, and one side of the turntable is provided with a connecting column.
The piston group comprises a piston pin and a piston, the piston is connected in the piston pin in a sliding mode, 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 rotary table, one end of the piston is connected with the connecting column, so that one end of the piston can move back and forth in the piston pin; that is, the piston moves back and forth on a straight line, the other end of the piston is connected with a rack, the rack moves back and forth along with the piston, a gear connected with the first rotating shaft (or the second rotating shaft) is meshed with the rack, and when the rack moves back and forth along with the piston, the gear rotates back and forth on the rack, so that the first rotating shaft (or the second rotating shaft) is driven to rotate back and forth.
Other driving methods may be adopted by those skilled in the art to drive the first rotating shaft and the second rotating shaft, and are not described in detail herein.
It should be noted that the first bonding plate (and the second bonding plate) may be made of metal, such as stainless steel, aluminum alloy, titanium alloy, magnesium alloy, zinc alloy, polymer, such as polytetrafluoroethylene, polyurethane, polyvinyl chloride, or at least one of natural wood board, natural rubber, or related composite materials.
In some embodiments, the roughness of the first bonding plate (second bonding plate) has a profile arithmetic mean deviation Ra of 0.2 μm to 25 μm, so that excessive roughness of the surface of the bonding plate, adhesion of large-particle materials in surface gaps and further non-adhesion to reduce peeling efficiency can be avoided.
In some possible embodiments, the cross section of the first adhesive plate and/or the second adhesive plate may be rectangular or trapezoidal, in the case of only one adhesive plate or a few adhesive plates, the adhesive plate with the rectangular cross section can be tightly attached to the fan blades after being rotationally bonded, but in the case of a multi-adhesive plate, if the cross section is still rectangular, the adhesive plate can be loosely attached to the fan blades, and the trapezoidal cross section can greatly improve the attachment of the adhesive plate, so that the cross section of the adhesive plate is along the length direction of the first rotating shaft or the second rotating shaft.
According to the above, as can be understood by those skilled in the art, in the case of adopting any one of the above embodiments, the stripping device is arranged in the accommodating barrel, and the first bonding plate and the second bonding plate in the first assembly and the second assembly are switched back and forth between the two states of separation and attachment, so that when the mixed material is fed into the stripping device by the first pipeline, the first bonding plate and the second bonding plate which are continuously attached and separated realize the stripping of the graphite material in the mixed material, thereby improving the stripping efficiency of the graphene in the graphite material.
Wherein, the holding bucket is used for holding the mixed material and the material after peeling off, and stripping off device sets up in the holding bucket. The stripping device can be matched with the accommodating barrel in terms of distance, and at least one fifth of space is reserved for the bottom of the accommodating barrel to bear stripped materials.
Referring to fig. 7-8, in some possible embodiments, the mixer is used for mixing the graphite material and the viscous liquid, and is an open configuration, and may take the shape of a rectangular parallelepiped, a square, a funnel, a cylinder, an inverted cone, etc.
In order to increase the volume of the mixer, the bottom of the mixer is arranged to be straight. Wherein, the bottom of blender has seted up the discharge gate, and its discharge gate and first tube coupling carry the misce bene through first pipeline towards stripping off device.
On the other hand, a washing solvent can be stored in the mixer for washing the accommodating barrel and the stripping device. Wherein the rinsing solvent may be at least one of water or ethanol, xylene, glycerol, and ethylene glycol. The mixer is used for containing a flushing solvent to flush the stripping device of the stripping component, when the viscosity of the viscous liquid is too high, the mixture flows slowly and aggregates on the bonding plate, or the graphite material is bonded and aggregated on the bonding plate and does not flow along with the mixture, the flushing solvent is used for flushing the bonding plate, the viscosity of the mixture is properly adjusted, and the flowing of the mixture and the further stripping of the graphite material are facilitated.
In some possible embodiment modes, at least one stirring device is arranged in the mixer, wherein the stirring device comprises a motor and a stirring blade connected with the motor. In order to ensure that the stirring blades do not damage the graphite material in the stirring process, the rotating speed of the stirring blades 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 adjusting device including a heating wire and a cooling circulation pipe, and the mixer may be provided therein with a double-layered hollow structure in which the heating wire or the cooling circulation pipe is provided, and the temperature inside the mixer is adjusted by the heating wire or the cooling circulation pipe. Specifically, the temperature adjusting range is 5-200 ℃.
Referring to fig. 1, in other possible embodiments, a second temperature adjusting device including a heating wire and a cooling circulation pipe is disposed in the receiving tub, and the receiving tub may be configured in a double-layered hollow structure in which the heating wire or the cooling circulation pipe is disposed, and the temperature inside the receiving tub is adjusted by the heating wire or the cooling circulation pipe. Specifically, the temperature adjusting range is 5-200 ℃.
It should be noted that the temperature of the mixed material is adjusted by adjusting the temperature of the viscous liquid and the graphite material in the holding tank or the mixer, and the limit between the two is further adjusted.
Based on the above description, those skilled in the art may further adopt an embodiment in which a second pipeline communicated with the accommodating barrel is disposed at the bottom of the barrel body of 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.
Referring to fig. 9 to 11, based on the above description, a person 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 means, and the mixed material delivered from the mixer is dispersed onto the first bonding plate and/or the second bonding plate through the feeder. The charging means can be the cavity cylinder type, and first pipeline is connected to the upper end, and the lower extreme then is provided with the gap opening, towards first bonding board or second bonding board, 1mm is no less than to the gap opening to guarantee that the misce bene normally flows out.
In some possible embodiments, the feeder is fixed to either one side of the first adhesive sheet or the second adhesive sheet obliquely above by a fixing frame.
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 above technical solution can also be adopted for the connection of the second pipeline and the stripping device.
In other embodiments, the pipe section part of one end of the second pipeline connected with the stripping device is provided with a plurality of injection ports, so that the materials in the second pipeline are injected on the first bonding plate and the second bonding plate.
In other embodiments, the pipe section of the end of the second pipeline connected with the stripping device is in a ring shape, and a plurality of jet ports distributed at intervals are arranged in the ring-shaped part, and each jet port is arranged corresponding to one first bonding plate or one second bonding plate. It can be understood that the second pipeline is adopted to strip the stripped materials in the accommodating barrel again, so that the stripping success rate can be improved.
It is noted that the material in the containment drum is transferred to the stripping assembly in the second conduit using pump pressure as the driving force.
In some embodiments, the pump pressure supply device is a compound pump or a diaphragm pump, which has no fan blade or gear and can not damage the particle size of the graphite material, and particularly, the graphene with the size of more than 100 μm is preferably stripped by a reciprocating pump or a diaphragm pump, the pump circulation pressure is 0.101MPa to 10 MPa, and the pipeline diameter is 2mm to 50mm.
In some embodiments, the 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 the pipeline pressure requirement and ensure that the device works normally for a long time.
The same arrangement is made for the first line, as can be seen by those skilled in the art.
Based on the above description, a person skilled in the art may further adopt an embodiment in which a third pipeline communicated with the accommodating barrel is disposed at the bottom of the accommodating barrel, and the third pipeline is further connected with a pressure-reducing evaporation device, and the pressure-reducing evaporation device is used to remove the viscous liquid and the rinsing solvent in the material peeled off from the accommodating barrel.
The viscous liquid is a substance having a boiling point of less than 400 ℃ or removable by distillation under reduced pressure; it can be stearic acid, paraffin, vaseline, etc., or long chain carboxylic acid or hydrocarbon, or glycerol, or polyvinylpyrrolidone, polyethylene glycol, etc. Because the viscous liquid is used for stripping the graphite material, if the viscous liquid is not easy to remove after stripping, the graphene is sealed in the viscous liquid and loses further utilization value, or the viscous liquid is removed by means of high-temperature burning and the like, the damage to the surface of the graphene is easily caused, and the quality and the yield of the graphene are reduced, therefore, substances with boiling points lower than 400 ℃ or substances which can be removed under reduced pressure are used, and the viscous liquid is removed by a reduced-pressure distillation device under relatively mild conditions after stripping is finished, so that 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 rinsing solvent from the effluent to obtain pure graphene material.
Referring to fig. 1, based on the above technical solution, a person skilled in the art may further adopt an embodiment that the reduced-pressure evaporation apparatus includes a material container, a circulation cooler, and a vacuum pump, which are connected in sequence. The circulating cooler is also connected with a viscous liquid collector; the material container is also provided with a liquid bath heater outside, and the liquid bath heater is used for heating the material container. When the decompression evaporation device works, the vacuum pump and the liquid bath heater enable the viscous liquid and the flushing solvent in the material 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 container.
Specifically, the accommodating barrel is connected with the material container through a third pipeline, so that discharged materials in the accommodating barrel are collected in the material container.
After the discharged materials enter the decompression evaporation device through the third pipeline, the mixed materials container is filled with the discharged materials, 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 materials container, and the viscous liquid after boiling and vaporization is cooled by the circulating cooler and enters the collector.
Because the boiling point of the viscous liquid at normal temperature and normal pressure is usually more than 150 ℃, the liquid has viscosity, the limit negative pressure of a vacuum pump of the device is less than or equal to 0.001MPa, and the liquid is heated relatively uniformly, liquid bath heating is adopted, the heating temperature is between room temperature and 300 ℃, and the temperature provided by a circulating cooler is between 50 ℃ below zero and room temperature.
The room temperature is in the range of 5 ℃ to 30 ℃.
Based on the above technical solution, a person skilled in the art may further adopt an embodiment that the graphene production stripping apparatus includes a plurality of sequentially connected accommodating barrels, when the plurality of accommodating barrels are sequentially connected, stripping devices in the plurality of accommodating barrels are sequentially connected, and a stripping device in one accommodating barrel is used to strip a material processed by a stripping device in an accommodating barrel connected to the previous barrel again, and convey the material to a stripping device connected to the next barrel or a reduced pressure evaporation device connected to the next barrel after the stripping process is completed.
The invention further provides a graphene stripping method based on the graphene stripping equipment, and the graphene stripping method comprises the following steps:
s100, mixing a 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 through a first pipeline for processing.
S200, conveying the material processed by the stripping device into the stripping device again for reprocessing, and if the reprocessed material does not reach the preset stripping standard, continuously conveying the stripped material into 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.
S400, separating the stripping materials meeting the preset stripping standard to obtain the graphene material.
It should be noted that the graphite material and the viscous liquid are mixed in a predetermined ratio, where the predetermined ratio is the volume (V) of the viscous liquid Mucus Per unit L) and the mass of the graphite material (W) Graphite The ratio per unit g).
In some embodiments, the volume of viscous liquid (V) Mucus Per unit L) and the mass of the graphite material (W) Graphite The ratio per unit g) is V Mucus :W Graphite ≥0.047。
When volume of viscous liquid (V) Mucus Per unit L) and the mass of the graphite material (W) Graphite The ratio of the total amounts per unit g) is adjusted by adding a rinsing solvent if the ratio is not at the desired ratio.
It can be understood that: after the graphite material is stripped into single-layer or multi-layer graphene, the graphene is spontaneously arranged or changed in morphology in the modes of fluctuation, bending, folding and the like of layer surfaces to reduce the surface energy, so that the distance between graphene layers is increased, and the volume of a corresponding stripping product is increased; the graphite has a true density of 2.09-2.33g/cm 3 (g/mL), the volume of 1g of flake graphite is about 2.09mL-2.33mL, the interlayer spacing of graphite single layers is expanded from initial 0.33nm to 3.3nm and expands about 10 times, the volume of 1g of flake graphite after being completely stripped is expanded to 20.9mL-23.3mL, the interlayer spacing of graphite single layers is expanded from initial 0.33nm to 33nm and expands about 100 times, the volume of 1g of flake graphite after being completely stripped is expanded to 209mL-233mL, actually, because long-range folds exist, the spacing between two layers of graphene at macroscopic angles is far larger than 3.3nm (expands 10 times), for example, the expandable graphite becomes the expanded graphite after being heated, and the volume can basically reach more than 100 times before; therefore, the volume of the graphene material after the graphite material is peeled and expanded is required to be less than that of the viscous liquid, the volume advantage of the viscous liquid is required to be ensured, excessive graphene after peeling is prevented from being attached to the surface of mucus in a large amount to block and hinder further peeling, and the transport property of the viscous liquid is required to be maintained, so that the volume of the mucus is required to be more than 2 times of the volume of 10 times of graphite expansion.
In the step S100 of mixing the graphite material and the viscous liquid in a mixer according to a predetermined ratio to form a mixed material, and conveying the mixed material to a stripping device through a first pipeline for processing, the method may further include the steps of:
s101 adding a graphite material and a viscous liquid to a mixer.
S102 the viscosity of the viscous liquid can be changed by adjusting the temperature inside the mixer by the first temperature adjusting device.
S103, starting a stirring device in the mixer, and mixing the graphite material and the viscous liquid.
It should be noted that step S101, step S102, and step S103 may be performed simultaneously.
In some embodiments, the viscosity of the viscous liquid is adjusted to 0.5 pas to 30 pas.
And in other embodiments, step S102 may alternatively adjust the viscosity of the viscous liquid by adding an adjusting solvent, which may be water or at least one of xylene, glycerol, ethylene glycol.
In other embodiments, the ratio of the total amount of the graphite material to the viscous liquid is dynamically adjusted, and in this embodiment, the graphene stripping method based on the graphene stripping device comprises the following steps:
s100, adding a 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 through a first pipeline for processing.
S200, conveying the material processed by the stripping device into the stripping device again for reprocessing, and if the reprocessed material does not meet the preset stripping standard, continuously conveying the stripped material into 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, adding a flushing solvent or a regulating solvent into the mixer to enable the viscous liquid and the graphite material to reach a second preset proportion.
S400, separating the stripping materials meeting the preset stripping standard to obtain the graphene material.
It should be noted thatThe first and second predetermined ratios are both viscous liquid volumes (V) Mucus Per unit L) and the mass of the graphite material (W) Graphite The ratio per unit g). Because the whole stripping process of the graphite material is progressive stripping, the volume of the graphene at the initial stripping stage is not expanded, the volume of mucus in the initial process can be reduced correspondingly, and a rinsing solvent or an adjusting solvent is additionally added through a later-stage circulating system to adjust V Mucus :W Graphite Ratio, thus adjusting V Mucus :W Graphite The ratio can be adjusted in step S100, or it can be adjusted in step S300 by adding a rinsing solvent or adjusting a solvent.
It should be noted that, in the first and second preset ratios, V Mucus :W Graphite ≥0.047。
In other embodiments, the material processed by the stripping device is conveyed to the stripping device again for reprocessing at S200, and if the reprocessed material does not meet the preset stripping standard, the stripped material is continuously conveyed to the stripping device again for stripping, and the material processed by the stripping device is conveyed to the stripping device through the second pipeline.
In other embodiments, S400 separates the stripping material meeting the preset stripping criteria to obtain the graphene material, which includes separating the graphene and the viscous liquid and washing the solvent by using the reduced-pressure evaporation apparatus.
The above description is only an alternative embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the contents of the present specification and the accompanying drawings, or directly/indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A graphite alkene stripping equipment for handling the mixture of graphite material and viscous liquid, its characterized in that includes:
an accommodating barrel;
the stripping device is arranged in the accommodating barrel;
a first pipeline communicated with the mixer is arranged between the mixer and the stripping device, and the first pipeline is used for feeding the mixed materials in the mixer into the stripping device;
the peeling apparatus includes a first assembly having at least one first adhesive sheet and a second assembly having at least one second adhesive sheet;
the first bonding plate on the first assembly is configured to rotate around a first center, the second bonding plate on the second assembly 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 attachment in the movement process of the first assembly and the second assembly.
2. The graphene peeling apparatus of claim 1, wherein a rotation direction of the first bonding plate on the first assembly is the same as a rotation direction of the second bonding plate on the second assembly.
3. The graphene peeling apparatus according to claim 1, wherein the first assembly further includes a first rotating shaft on which at least one of the first bonding plates is disposed, the first rotating shaft driving 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.
4. The graphene stripping apparatus according to claim 2, wherein the first rotating shaft and the second rotating shaft are connected to one driving assembly in common or one driving assembly in each case;
the driving assembly comprises a rack, a piston group, a gear meshed with the rack and a turntable rotating around a central axis;
one side of the turntable is provided with a connecting column;
the piston group comprises a piston pin and a piston, the piston is slidably connected in the piston pin, 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/second rotating shaft.
5. The graphene peeling apparatus of claim 1, wherein the first bonding plate and the second bonding plate are the same in size and shape.
6. The graphene stripping apparatus according to claim 1, wherein a first temperature adjusting device is disposed in the mixer, and the first temperature adjusting device is configured to adjust a temperature of an internal environment of the mixer; and/or
And a second temperature adjusting device is arranged in the accommodating barrel and is used for adjusting the temperature of the internal environment of the accommodating barrel.
7. The graphene peeling apparatus according to claim 1, wherein a second pipeline communicated with the accommodating barrel is arranged at the bottom of the accommodating barrel, 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 barrel to the peeling device.
8. The graphene stripping device according to claim 1, wherein a third pipeline communicated with the accommodating barrel is arranged at the bottom of the accommodating barrel, and is further connected with a pressure-reducing evaporation device, and the pressure-reducing evaporation device is used for removing the viscous liquid and the flushing solvent in the stripped material in the accommodating barrel.
9. The graphene stripping apparatus according to claim 8, wherein the reduced-pressure evaporation device comprises a material container, a circulation cooler and a vacuum pump which are connected in sequence;
the circulating cooler is also connected with a viscous liquid collector, a liquid bath heater is also arranged outside the material container, and the liquid bath heater is used for heating the material container;
when the decompression evaporation device works, the vacuum pump and the liquid bath heater enable the viscous liquid and the flushing solvent in the material container to be vaporized under preset working conditions, and the vaporized viscous liquid and the flushing solvent are cooled by the circulating cooler and are liquefied and collected in the collector, so that the stripped graphene material is obtained in the material container.
10. A graphene peeling method comprising using the graphene peeling apparatus of any one of claims 1 to 9, the graphene peeling method comprising the steps of:
mixing the graphite material and the viscous liquid in a mixer according to a preset proportion to form a mixed material, and conveying the mixed material to the stripping device through the first pipeline for treatment;
conveying the material treated by the stripping device into the stripping device again for retreatment, and if the material treated by the retreatment does not reach the preset stripping standard, continuously conveying the stripped material into the stripping device again for stripping;
repeating the steps until the stripping effect of the material treated by the stripping device reaches a preset stripping standard;
and separating the stripping materials meeting the preset stripping standard to obtain the graphene material.
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