Preparation device of high-wrinkle graphene oxide balls

Abstract

The utility model discloses a preparation device of high-wrinkle graphene oxide balls. The preparation device comprises a nitrogen cylinder, an atomizer, a tube furnace and a beaker which are connected in sequence, the atomizer comprises an atomizing cavity and a water storage tank arranged at the bottom of the atomizing cavity, and further comprises a ceramic atomizing sheet arranged at the bottom of the water storage tank; a mist outlet pipe is arranged on one side of the top of the atomization cavity, a gas inlet pipe is arranged on the other side of the top of the atomization cavity, the gas inlet pipe is connected with the nitrogen cylinder, and the mist outlet pipe is connected with one end of a quartz tube of the tubular furnace; and the other end of the quartz tube of the tube furnace is inserted below the water liquid level at the bottom of the beaker through a hose. The device disclosed by the utility model can be used for controlling the atomization amount of the graphene oxide solution, so that the continuity of the preparation process is ensured, the wrinkle degree of the graphene oxide is convenient to adjust, and the continuous increase of the shrinkage degree of graphene oxide spheres deposited along the axial direction of the quartz tube can also be effectively ensured; the overall size is gradually reduced, so that the quality stability of the folded graphene oxide finished product is ensured.

Description

Technical Field

[0001] The utility model relates to the field of chemical industry, and in particular to a preparation device for highly wrinkled graphene oxide balls. Background Art

[0002] Graphene is a two-dimensional carbon nanomaterial composed of carbon atoms in a hexagonal honeycomb lattice with hybrid orbitals. It has many properties that ordinary materials do not have, such as good light transmittance, high thermal conductivity, high electron mobility, low resistivity and high mechanical strength. It is considered to be a revolutionary material in the future. One of the main applications of graphene is to assemble microscopic graphene oxide balls or graphene sheets into macroscopic graphene films. Wrinkled graphene balls have a unique wrinkled structure, excellent tensile properties, and can provide a high specific surface area and mesopores. Combined with the advantages of graphene itself, this material is expected to become an electrode material for flexible devices, filtration membranes, high-performance supercapacitors and lithium-ion batteries. It has good application prospects in the fields of flat panel displays, corrosion protection, electrothermal materials, energy storage, and industrial catalysis.

[0003] In the prior art, the preparation is usually carried out through chemical vapor deposition or dry-wet transfer. On the one hand, most of the preparation methods are complicated and have high preparation temperatures, resulting in high energy consumption. On the other hand, the preparation of wrinkled graphene oxide balls in the prior art is still in a relatively early stage. The structure of the wrinkled graphene oxide balls obtained is uneven, and the degree of wrinkling of the finished products is usually unstable, which in turn affects their performance in various aspects.

[0004] To this end, a device for preparing highly wrinkled graphene oxide balls is proposed to solve the above technical problems. Utility Model Content

[0005] The technical problem solved by the utility model is that in the prior art, the preparation process of wrinkled graphene balls is relatively complicated and the energy consumption is high. At the same time, the finished wrinkled graphene oxide balls obtained have uneven structures and unstable overall quality.

[0006] In order to solve the above technical problems, the technical solution adopted by the utility model is: a preparation device for highly wrinkled graphene oxide balls, comprising a nitrogen bottle, an atomizer, a tubular furnace and a beaker connected in sequence; the atomizer comprises an atomization chamber and a water storage tank arranged at the bottom of the atomization chamber, and also comprises a ceramic atomization sheet arranged at the bottom of the water storage tank; a mist outlet pipe is provided on one side of the top of the atomization chamber, and an air inlet pipe is provided on the other side of the top, the air inlet pipe is connected to the nitrogen bottle, and the mist outlet pipe is connected to one end of the quartz tube of the tubular furnace; the other end of the quartz tube of the tubular furnace is inserted below the water level at the bottom of the beaker through a hose.

[0007] Particularly, the nitrogen cylinder is provided with a pressure regulating valve.

[0008] Particularly, a partition plate located between the mist outlet pipe and the air inlet pipe is provided in the atomizing chamber, and an air passage is left at the bottom of the partition plate; and an arc-shaped guide plate is also provided on the side wall of the lower half of one side of the air inlet pipe.

[0009] Particularly, a water level sensor is provided in the water storage tank, the water level sensor is electrically connected to a PLC controller, and the PLC controller is electrically connected to a ceramic atomizing sheet.

[0010] Particularly, the connecting pipe between the mist outlet pipe and the quartz tube of the tubular furnace is a transparent hose.

[0011] Compared with the prior art, the utility model has the following advantages and beneficial effects: the utility model device can control the atomization amount of the graphene oxide solution by controlling the nitrogen gas flow rate and the vibration frequency of the ceramic atomizing plate, thereby ensuring the continuity of the preparation process and facilitating the adjustment of the wrinkle degree of the graphene oxide ball, and can also effectively ensure that the shrinkage degree of the graphene oxide ball deposited along the axis direction of the quartz tube is continuously improved, and its overall size is gradually reduced, thereby ensuring the stability of the quality of the finished wrinkled graphene oxide ball. In addition, the preparation temperature can be reduced from 800 degrees Celsius to 400 degrees Celsius, effectively reducing the preparation energy consumption and saving the preparation cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 It is a schematic diagram of the overall structure of the utility model device.

[0013] Figure 2 Schematic diagram of the internal structure of the atomizer.

[0014] The meanings of the numbers in the figure are: nitrogen bottle—1; atomizer—2; tubular furnace—3; beaker—4; water storage tank—5; ceramic atomizer—6; mist outlet pipe—7; air inlet pipe—8; pressure regulating valve—9; partition plate—10; air duct—11; arc guide plate—12. DETAILED DESCRIPTION

[0015] The following will clearly and completely describe the technical solutions in the embodiments of the utility model in conjunction with the accompanying drawings in the embodiments of the utility model, so as to have a further understanding of the concept of the utility model, the technical problems solved, the technical features constituting the technical solutions and the technical effects brought about.

[0016] like Figure 1~Figure 2As shown, a preparation device for highly wrinkled graphene oxide balls comprises a nitrogen bottle 1, an atomizer 2, a tubular furnace 3 and a beaker 4 connected in sequence; the atomizer 2 comprises an atomization chamber and a water storage tank 5 arranged at the bottom of the atomization chamber, and also comprises a ceramic atomization sheet 6 arranged at the bottom of the water storage tank 5; a mist outlet pipe 7 is arranged on one side of the top of the atomization chamber, and an air inlet pipe 8 is arranged on the other side of the top, the air inlet pipe 8 is connected to the nitrogen bottle 1, and the mist outlet pipe 7 is connected to one end of the quartz tube of the tubular furnace 3; the other end of the quartz tube of the tubular furnace 3 is inserted below the water level at the bottom of the beaker 4 through a hose.

[0017] In the utility model, the main use process is as follows: first, use an ultrasonic cleaner to ultrasonically treat the graphene oxide mixed in water for 30 minutes to make it evenly dispersed, and then add the dispersed liquid into the water storage tank 5. Connect the utility model device with a hose in the order of nitrogen bottle 1-atomizer 2-tube furnace 3-beaker 4, and slowly introduce nitrogen after the connection is completed. Check whether there is corresponding gas discharge from the end of the hose extending below the water level at the bottom of the beaker 4, and observe whether the gas discharged from the end of the hose in the beaker 4 increases synchronously after increasing the nitrogen input, so as to complete the inspection of the airtightness and sealing of the device. Then, nitrogen is introduced normally for ten minutes to exhaust the air inside the device, and the temperature of the tube furnace 3 is set, and the heating rate is 3°C / min to avoid uneven heating of the quartz tube of the tube furnace 3 and cause cracking. When the temperature of the tube furnace 3 reaches 400°C, it is maintained for at least 2 hours to complete the preheating. Then, the atomizer 2 is turned on, and the atomized dispersion is introduced into the tubular furnace 3 under the action of nitrogen flow. Due to the high temperature in the tubular furnace 3, the water vapor evaporates quickly to generate capillary force, causing the graphene oxide nanosheets to shrink and become a sphere with wrinkles similar to a crumpled paper ball. Since the crumpled graphene balls (denoted as CGB-1, Crumpled Graphene Balls) at the front end of the quartz tube of the tubular furnace have a short heating time, some of them are in the form of sheets and are larger in size; while the crumpled graphene balls (denoted as CGB-2) at the rear end of the quartz tube have a high degree of shrinkage and agglomeration due to the long heating time, thereby achieving the purpose of effectively ensuring the overall quality of the crumpled graphene products.

[0018] As a preferred embodiment, the nitrogen cylinder 1 is provided with a pressure regulating valve 9.

[0019] In this embodiment, a specific method for adjusting the nitrogen flow rate is provided. The nitrogen flow rate can be accurately adjusted by the pressure regulating valve 9, thereby coordinating the output power of the ceramic atomizing plate 6 to achieve the purpose of adjusting the amount of dispersion entering the quartz tube of the tubular furnace 3 per unit time.

[0020] As a preferred embodiment, a partition plate 10 is provided in the atomizing chamber between the mist outlet pipe 7 and the air inlet pipe 8 , and an air passage 11 is left at the bottom of the partition plate 10 ; and an arc-shaped guide plate 12 is also provided on the lower half of the side wall of the air inlet pipe 8 .

[0021] In this embodiment, a partition plate 10 is provided in the atomizing chamber to separate the mist outlet pipe 7 and the air inlet pipe 8, thereby dividing the entire chamber into two half chambers, and the two half chambers are connected through the airway 11 at the bottom of the partition plate 10, thereby artificially changing the flow path of the nitrogen gas to ensure that the dispersed liquid droplets at the bottom of the atomizing chamber can be taken out of the atomizing chamber together. The purpose of providing the arc-shaped guide plate 12 is to improve the flow of nitrogen in the atomizing chamber, avoid the fluctuation of the dispersed liquid level caused by the direct impact of nitrogen on the liquid surface, and also avoid turbulence of the nitrogen gas flow, which causes the dispersed liquid droplets to merge with each other again and affect the atomization effect.

[0022] As a preferred embodiment, a water level sensor is provided in the water storage tank 5 , and the water level sensor is electrically connected to a PLC controller, and the PLC controller is electrically connected to a ceramic atomizing sheet 6 .

[0023] In this embodiment, the function of the PLC controller is to determine the disconnection state according to the detection signal of the water level sensor. When the dispersion liquid is less than a certain scale, the PLC controller controls the ceramic atomizing sheet 6 to stop working, thereby preventing the atomizer 2 from idling. In addition, the output power of the ceramic atomizing sheet 6 can be controlled by the PLC controller according to the nitrogen flow rate and the temperature of the tubular furnace 3, thereby effectively adjusting the overall preparation speed.

[0024] As a preferred embodiment, the connecting pipe between the mist outlet pipe 7 and the quartz tube of the tubular furnace 3 is a transparent hose.

[0025] In this embodiment, by making the connecting tube between the mist outlet pipe 7 and the quartz tube of the tubular furnace 3 a transparent hose, it is possible to judge whether the atomizer 2 is working normally by the deposition of graphene balls on the wall of the transparent hose during the preparation process of the wrinkled graphene oxide balls, thereby avoiding idling of the entire preparation equipment in the event of an unexpected situation.

[0026] The words “connection” and “fixation” appearing in the description of the present invention may refer to fixed connection, processing and forming, welding, or mechanical connection. The specific meanings of the above terms in the present invention shall be understood according to the specific circumstances.

[0027] In the description of the present invention, the terms "center", "upper", "lower", "horizontal", "inner", "outer", etc., which indicate the orientation or position relationship, are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying a specific orientation that the device or element referred to must have, and therefore cannot be understood as a limitation on the present invention.

[0028] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the utility model, rather than to limit it. Although the utility model has been described in detail with reference to the aforementioned embodiments, ordinary technicians in the field should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the utility model.

Claims

1. A device for preparing highly wrinkled graphene oxide balls, characterized in that: The invention comprises a nitrogen bottle (1), an atomizer (2), a tubular furnace (3) and a beaker (4) which are connected in sequence; the atomizer (2) comprises an atomizing chamber and a water storage tank (5) arranged at the bottom of the atomizing chamber, and also comprises a ceramic atomizing sheet (6) arranged at the bottom of the water storage tank (5); a mist outlet pipe (7) is arranged on one side of the top of the atomizing chamber, and an air inlet pipe (8) is arranged on the other side of the top; the air inlet pipe (8) is connected to the nitrogen bottle (1), and the mist outlet pipe (7) is connected to one end of a quartz tube of the tubular furnace (3); the other end of the quartz tube of the tubular furnace (3) is inserted below the water level at the bottom of the beaker (4) through a hose.

2. A device for preparing highly wrinkled graphene oxide balls according to claim 1, characterized in that: The nitrogen cylinder (1) is provided with a pressure regulating valve (9).

3. A device for preparing highly wrinkled graphene oxide balls according to claim 1, characterized in that: The atomizing chamber is provided with a partition plate (10) located between the mist outlet pipe (7) and the air inlet pipe (8), and an air passage (11) is left at the bottom of the partition plate (10); and also includes an arc-shaped guide plate (12) located on the lower half of the side wall of one side of the air inlet pipe (8).

4. A device for preparing highly wrinkled graphene oxide balls according to claim 1, characterized in that: A water level sensor is provided in the water storage tank (5); the water level sensor is electrically connected to a PLC controller; and the PLC controller is electrically connected to a ceramic atomizing sheet (6).

5. A device for preparing highly wrinkled graphene oxide balls according to claim 1, characterized in that: The connecting pipe between the mist outlet pipe (7) and the quartz tube of the tubular furnace (3) is a transparent hose.

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