CN220976597U - Device for stripping graphene nano-sheets based on supercritical carbon dioxide - Google Patents

Device for stripping graphene nano-sheets based on supercritical carbon dioxide Download PDF

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CN220976597U
CN220976597U CN202322738431.5U CN202322738431U CN220976597U CN 220976597 U CN220976597 U CN 220976597U CN 202322738431 U CN202322738431 U CN 202322738431U CN 220976597 U CN220976597 U CN 220976597U
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net
stirring blade
reaction kettle
puddler
impact
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朱宏跃
刘一鸣
王启搏
周丹
路荣荣
李娜
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Taiyuan University of Science and Technology
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Taiyuan University of Science and Technology
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Abstract

The utility model relates to a device for stripping graphene nano sheets based on supercritical carbon dioxide, which belongs to the technical field of graphene preparation and specifically comprises a hollow speed reduction motor arranged at the top of a reaction kettle, wherein a first stirring rod is arranged on an output shaft of the hollow speed reduction motor, the first stirring rod extends into the reaction kettle, a speed reduction motor is arranged on the hollow speed reduction motor, a second stirring rod is arranged on an output shaft of the speed reduction motor, the second stirring rod is positioned in the first stirring rod, the bottom of the second stirring rod protrudes out of the first stirring rod, stirring blades are arranged at the bottom of the second stirring rod, and an impact net component is arranged on the first stirring rod.

Description

Device for stripping graphene nano-sheets based on supercritical carbon dioxide
Technical Field
The utility model relates to a device for stripping graphene nano sheets based on supercritical carbon dioxide, and belongs to the technical field of graphene preparation.
Background
Graphene is used as a typical two-dimensional layered material, and has a wide application prospect. In 2004, andreheight (ANDRE GEIM) and Constant's No Wo Xiao love (Konstantin Novoselov) from the highly oriented pyrolytic graphite were peeled off the monolayer graphene sheets by the "tape-tearing" method to obtain the physical prize of norbeol 2010, thereby initiating a two-dimensional materials study hot-dip.
Graphene is a hexagonal two-dimensional material with honeycomb lattice and composed of carbon atoms in sp2 hybridization orbits, and is used as a basic unit of a graphite material, can be recombined into other carbon materials through deformation, and can form zero-dimensional fullerene through curling into balls; the one-dimensional carbon nanotubes can be formed by curling into a barrel and can be divided into single-wall and multi-wall carbon nanotubes according to different graphene layers; three-dimensional graphite is formed by stacking multiple layers.
The common preparation methods of graphene mainly include two main types: firstly, a bottom-up method including a chemical vapor deposition method, an epitaxial growth method, an arc discharge method, a redox method and the like is adopted; the other is a top-down method using methods including electrochemical stripping, mechanical stripping, and liquid phase stripping. The bottom-up growth method can obtain the graphene with large size and controllable thickness, but has the defects of high production cost, severe growth temperature and the like. Although the top-down exfoliation method can obtain high yield graphene, uniformity is poor. Therefore, developing a preparation method with high efficiency, high quality and low cost is a key for realizing large-scale application of graphene.
At present, the existing graphene preparation device is low in reaction efficiency, poor in using effect and poor in stripping effect in the production process of graphene.
Disclosure of utility model
In order to solve the technical problems in the prior art, the utility model provides a device for stripping graphene nano sheets based on supercritical carbon dioxide, which has high reaction efficiency and good use effect and can greatly improve stripping effect.
In order to achieve the above purpose, the technical scheme adopted by the utility model is that the device for stripping graphene nano sheets based on supercritical carbon dioxide comprises a reaction kettle, wherein a heating jacket is arranged outside the reaction kettle, and the device is characterized in that: the utility model discloses a reaction kettle, including reaction kettle, gear motor, first puddler, second puddler, stirring vane, striking net subassembly, first puddler, second puddler, first puddler is installed at cavity gear motor's top installs cavity gear motor, install cavity gear motor on the top of reaction kettle, install first puddler on cavity gear motor's the output shaft, the second puddler is located first puddler, the first puddler of bottom protrusion of second puddler, and stirring vane is installed to the bottom of second puddler, install the striking net subassembly on the first puddler.
Preferably, the impact net assembly comprises a connecting sleeve sleeved on the first stirring rod, connecting plates fixed on two sides of the connecting sleeve and an impact net fixed on the connecting plates, and the connecting sleeve is fixed on the first stirring rod through screws.
Preferably, the impact net component and the stirring blade rotate in the same direction or in opposite directions, and the rotating speed of the impact net component and the stirring blade is 500-5000 rpm when the impact net component and the stirring blade rotate in the same direction; during the reverse rotation, the rotation speed of the impacting net assembly is 500-5000 rpm, and the rotation speed of the stirring blade is 500-2000 rpm.
Preferably, the impact net is a strip net or a hole net or a composite net formed by combining the strip net and the hole net, when the impact net is a hole net, the mesh number is 100-3000 meshes, and when the impact net is a strip net, the net strip number is 100-200.
Preferably, the ratio of the width of the impact net assembly to the inner diameter of the reaction kettle is smaller than 0.9, the ratio of the height of the impact net assembly to the depth of the reaction kettle is smaller than 0.7, and the vertical distance between the bottommost part of the impact net assembly and the uppermost end of the stirring blade is not smaller than 2cm.
Preferably, a through hole is formed in the upper right corner of the impact net, and the size of the through hole corresponds to the width of the impact net assembly.
Preferably, the stirring blade is a paddle type, a cloth Lu Majin type, a turbine type, a propelling type, an anchor type, a frame type, a ribbon type or a screw type blade.
Preferably, the stirring blade is a paddle blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:2-1:1.25, when the stirring blade is a cloth Lu Majin type blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:2-1:1.25, when the stirring blade is a turbine type blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:6-1:3, and when the stirring blade is a propelling type blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:4-1:3.
Preferably, the reaction kettle is also provided with a pressure sensor and a temperature sensor.
Compared with the prior art, the utility model has the following technical effects: the supercritical carbon dioxide intercalation stripping and dynamic impact strengthening stripping are combined together, so that the intercalation, impact and stripping are cooperatively and effectively carried out in the graphene preparation process, the layout of a graphene production line is more concise and compact, the equipment cost is reduced, the graphene production efficiency and the uniformity stability of products are obviously improved, the prepared graphene structure is ensured not to be damaged, and meanwhile, the used instrument and equipment are simple and common, and the method has the advantages of low cost and easiness in popularization, and is particularly suitable for large-scale industrial production.
Drawings
Fig. 1 is a schematic structural view of the present utility model.
Fig. 2 is a view of the mounting structure of the impact net assembly of the present utility model.
Fig. 3 is a schematic view of the impact net according to the present utility model.
Fig. 4 is a Transmission Electron Microscope (TEM) image of graphene prepared according to the present utility model.
Fig. 5 is a Transmission Electron Microscope (TEM) image of graphene prepared according to the present utility model.
In the figure: 1 is a reaction kettle, 2 is a heating jacket, 3 is a hollow gear motor, 4 is a gear motor, 5 is a first stirring rod, 6 is a second stirring rod, 7 is a stirring blade, 8 is an impact net component, 9 is a connecting sleeve, 10 is a connecting plate, 11 is an impact net, 12 is a through hole, 13 is a pressure sensor, and 14 is a temperature sensor.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the utility model is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the utility model.
As shown in fig. 1 to 3, a device for stripping graphene nano sheets based on supercritical carbon dioxide comprises a reaction kettle 1, wherein a heating jacket 2 is arranged at the outer part of the reaction kettle 1, a hollow gear motor 3 is arranged at the top of the reaction kettle 1, a first stirring rod 5 is arranged on an output shaft of the hollow gear motor 3, the first stirring rod 5 extends to the inside of the reaction kettle 1, a gear motor 4 is arranged on the hollow gear motor 3, a second stirring rod 6 is arranged on an output shaft of the gear motor 4, the second stirring rod 6 is positioned in the first stirring rod 5, a first stirring rod 5 protrudes from the bottom of the second stirring rod 6, stirring blades 7 are arranged at the bottom of the second stirring rod 6, an impact net assembly 8 is arranged on the first stirring rod 5, and a pressure sensor 13 and a temperature sensor 14 are also arranged on the reaction kettle 1.
In the utility model, the impact net component and the stirring blade are respectively driven by two motors, and the stirring blade is positioned below the impact net component. The impact net assembly 8 comprises a connecting sleeve 9 sleeved on the first stirring rod 5, connecting plates 10 fixed on two sides of the connecting sleeve and an impact net 11 fixed on the connecting plates, wherein the connecting sleeve 9 is fixed on the first stirring rod 5 through screws. The impact net component adopts a detachable structure, can be freely detached and assembled, and is convenient for replacing impact nets in different shapes. The impact net component 8 and the stirring blades rotate in the same direction or in opposite directions, and the rotation speed of the impact net component 8 and the stirring blades is 500-5000 rpm when the impact net component and the stirring blades rotate in the same direction; during the reverse rotation, the rotation speed of the impacting net assembly 8 is 500-5000 rpm, and the rotation speed of the stirring blade is 500-2000 rpm. The impact net 11 is a strip net or a hole net, or a composite net formed by combining a strip net and a hole net, such as a rectangle, a square, a diamond, etc. When the impact net 11 is a hole-shaped net, the mesh number is 100-3000 meshes, and when the impact net 11 is a bar-shaped net, the net scroll number is 100-200. The ratio of the width of the impact net assembly 8 to the inner diameter of the reaction kettle is smaller than 0.9, the ratio of the height of the impact net assembly 8 to the depth of the reaction kettle is smaller than 0.7, and the vertical distance between the bottommost part of the impact net assembly 8 and the uppermost end of the stirring blade is not smaller than 2 cm. The upper right corner of the impact net 11 is provided with a through hole 12, and the size of the through hole 12 corresponds to the width of the impact net assembly 8.
The stirring blade 7 is a paddle type, a cloth Lu Majin type, a turbine type, a propelling type, an anchor type, a frame type, a spiral type or a screw type blade. The stirring blade 7 is a paddle blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:2-1:1.25, when the stirring blade is a cloth Lu Majin type blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:2-1:1.25, when the stirring blade is a turbine type blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:6-1:3, and when the stirring blade is a propelling type blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:4-1:3.
When the device is specifically used, graphite of 5 g is added into a reaction kettle 1, after the reaction kettle is sealed, a certain amount of carbon dioxide liquid is filled into the reaction kettle 1, a heating jacket 2 is adopted to heat the reaction kettle, a temperature sensor 14 is used for measuring the temperature of the reaction kettle, a stirring blade 7 is a paddle type stirring paddle, the ratio of the diameter to the inner diameter of the reaction kettle is 1:2, the type of an impact net 11 is a diamond net, the mesh number is 2000 meshes, the ratio of the width of the impact net 11 to the inner diameter of the reaction kettle is 0.85, the ratio of the height of the impact net to the depth of the reaction kettle is 0.65, and the vertical distance from the bottommost part of the impact net 11 to the uppermost end of the stirring blade 7 is 2 cm. After the reaction kettle 1 is heated to 50 ℃ and the pressure reaches 25 MPa, respectively starting an impact net 11 and a stirring blade 7, respectively controlling the rotation speeds of the impact net 11 and the stirring blade 7 through two motors, wherein the impact net 11 rotates clockwise, the rotation speed is 3000 rpm, the stirring blade 11 rotates anticlockwise, the rotation speed is 1000 rpm, after the reaction is performed for 4 h, the laminar carbon material is peeled off under the combined action of supercritical carbon dioxide intercalation and impact mechanical energy of the impact net, and the graphene material is obtained through pressure relief.
The foregoing description of the preferred embodiment of the utility model is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the utility model.

Claims (9)

1. The utility model provides a device based on supercritical carbon dioxide peels off graphite alkene nanometer piece, includes reation kettle, reation kettle's externally mounted has heating jacket, its characterized in that: the utility model discloses a reaction kettle, including reaction kettle, gear motor, first puddler, second puddler, stirring vane, striking net subassembly, first puddler, second puddler, first puddler is installed at cavity gear motor's top installs cavity gear motor, install cavity gear motor on the top of reaction kettle, install first puddler on cavity gear motor's the output shaft, the second puddler is located first puddler, the first puddler of bottom protrusion of second puddler, and stirring vane is installed to the bottom of second puddler, install the striking net subassembly on the first puddler.
2. The supercritical carbon dioxide-based graphene nanoplatelet stripping device according to claim 1, wherein: the impact net assembly comprises a connecting sleeve sleeved on the first stirring rod, connecting plates fixed on two sides of the connecting sleeve and an impact net fixed on the connecting plates, and the connecting sleeve is fixed on the first stirring rod through screws.
3. The supercritical carbon dioxide-based graphene nanoplatelet stripping device according to claim 1 or 2, wherein: the impact net component and the stirring blade rotate in the same direction or in opposite directions, and the rotating speed of the impact net component and the stirring blade is 500-5000 rpm when the impact net component and the stirring blade rotate in the same direction; during the reverse rotation, the rotation speed of the impacting net assembly is 500-5000 rpm, and the rotation speed of the stirring blade is 500-2000 rpm.
4. The supercritical carbon dioxide-based graphene nanoplatelet stripping device according to claim 2, wherein: the impact net is a strip net or a hole net or a composite net formed by combining the strip net and the hole net, when the impact net is a hole net, the mesh number is 100-3000 meshes, and when the impact net is a strip net, the net scroll number is 100-200.
5. The supercritical carbon dioxide-based graphene nanoplatelet stripping device according to claim 2, wherein: the ratio of the width of the impact net component to the inner diameter of the reaction kettle is smaller than 0.9, the ratio of the height of the impact net component to the depth of the reaction kettle is smaller than 0.7, and the vertical distance between the bottommost part of the impact net component and the uppermost end of the stirring blade is not smaller than 2 cm.
6. The supercritical carbon dioxide-based graphene nanoplatelet stripping device according to claim 2, wherein: the upper right corner of the impact net is provided with a through hole, and the size of the through hole corresponds to the width of the impact net assembly.
7. The supercritical carbon dioxide-based graphene nanoplatelet stripping device according to claim 1, wherein: the stirring blade is a paddle type, a cloth Lu Majin type, a turbine type, a propelling type, an anchor type, a frame type, a spiral belt type or a screw type blade.
8. The supercritical carbon dioxide-based graphene nanoplatelet stripping apparatus of claim 7, wherein: the stirring blade is a paddle blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:2-1:1.25, when the stirring blade is a fabric Lu Majin type blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:2-1:1.25, when the stirring blade is a turbine type blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:6-1:3, and when the stirring blade is a propelling type blade, the ratio of the diameter of the stirring blade to the inner diameter of the reaction kettle is 1:4-1:3.
9. The supercritical carbon dioxide-based graphene nanoplatelet stripping device according to claim 1, wherein: and a pressure sensor and a temperature sensor are also arranged on the reaction kettle.
CN202322738431.5U 2023-10-12 2023-10-12 Device for stripping graphene nano-sheets based on supercritical carbon dioxide Active CN220976597U (en)

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CN202322738431.5U CN220976597U (en) 2023-10-12 2023-10-12 Device for stripping graphene nano-sheets based on supercritical carbon dioxide

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Application Number Priority Date Filing Date Title
CN202322738431.5U CN220976597U (en) 2023-10-12 2023-10-12 Device for stripping graphene nano-sheets based on supercritical carbon dioxide

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