Vapor deposition graphene coating equipment based on fluidized bed

By setting up an elevation section and plunger structure in the fluidized bed reactor, uniform gas intake and stable catalyst heating are achieved, which solves the problem of the catalyst being prone to rupture or burst during the heating process, extends the service life of the catalyst and improves the optimality of the fluidized state.

CN119800325AInactive Publication Date: 2025-04-11JIANGSU WEIPU NANO TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510090756.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-21
Publication Date
2025-04-11
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

During the heating process, the fluidized bed reactor is prone to cause the catalyst to rupture or burst, affecting its life and physical strength, and it is difficult to control the heating rate.

Method used

A vapor-phase deposition graphene coating device based on a fluidized bed is designed. By setting up an elevated section and a plunger structure inside the reactor, uniform gas intake and stable catalyst heating are achieved, and the heating rate is controlled within an appropriate range.

Benefits of technology

It effectively extends the service life of the catalyst, improves the optimality of the fluidization state, and ensures that the catalyst reacts fully at a reaction temperature of 1100 degrees.

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Abstract

The invention provides a fluidized bed-based vapor deposition graphene coating equipment, which comprises a discharge module and a reactor body, a heightening section is arranged between the reactor body and the discharge module, a plunger is arranged at the joint of the lower end of the reactor body and the heightening section, the discharge module comprises a cylinder rod, a discharge valve and a cylinder, and the discharge valve is connected with the cylinder rod. The upper end and the lower end of the cylinder rod are connected with the plunger and one end of a telescopic rod of the cylinder respectively, a cavity communicated with the reactor body is formed in the heightening section, a first air inlet channel is formed in the plunger, a plurality of air holes are formed in the periphery of the first air inlet channel, a second air inlet channel is formed in the upper end of the cylinder rod, and an air inlet communicated with the second air inlet channel is formed in one side of the second air inlet channel. The invention has the following beneficial effects: by adopting the structure that the internal reaction area is raised, the reaction temperature is increased, the temperature required by the reaction is 1100 DEG C, the catalytic non-reaction effect is better, and the combined structure of the plunger and the cylinder rod is matched, so that the uniform gas inlet is realized, and the fluidization state is further optimal.
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Description

Technical Field

[0001] The present invention mainly relates to the technical field of fluidized beds, and in particular to a gas-deposited graphene coating device based on a fluidized bed. Background Art

[0002] Chemical vapor deposition (CVD) is a technology that decomposes carbon-containing compounds through chemical reactions at relatively high temperatures and then allows graphene to grow on a substrate. Usually, a transition metal (such as Cu, Co, Pt, Ir, Ru and Ni, etc.) film is formed on the surface of the substrate, and this film is used as a catalyst. Then, CH4 is used as a carbon source and the transition metal film is dissociated by gas phase dissociation, so that graphene sheets are gradually formed on the surface of the transition metal film. The metal film is then treated with a highly corrosive acidic solution to prepare graphene. This method can produce large-area, high-quality graphene sheets with good mechanical properties, and is the most likely preparation method to be industrialized.

[0003] As we all know, the direct exfoliation method for preparing graphene has low yield and complicated procedures, which is not suitable for actual industrial needs. With the emergence of chemical vapor deposition, the industrial production of graphene has become possible.

[0004] The equipment used to prepare graphene by chemical vapor deposition includes: tubular furnace, microwave plasma CVD equipment, radio frequency chemical vapor deposition equipment, etc. The chemical vapor deposition furnace equipment generally includes a furnace shell, a cooling system, an electrical control system, a vacuum system and a thermal field system.

[0005] During the specific implementation process, the inventor discovered the following defects: The thermodynamic performance of fluidized bed reactors is affected by many factors: Fluid velocity: Fluid velocity determines the fluidization state of the bed, thus affecting the heat transfer efficiency; Particle size: Smaller particles fluidize more easily but may increase pressure drop; Bed height: Bed height affects the heat transfer area and heat transfer efficiency; Operating temperature and pressure: At high temperature and pressure, both reaction rate and heat transfer rate will increase.

[0006] The heating rate of the fluidized bed reactor is generally determined based on the stress allowance of the equipment during heating and the characteristics of the catalyst itself. It is generally required that the catalyst should not be heated too quickly. If the temperature is heated too quickly, the catalyst will easily crack or even explode, which will not only affect the life of the catalyst, but also increase the resistance to hard gas generation, thereby destroying the physical strength of the catalyst. Even if the reduced catalyst needs to be heated again for some reason, it should be controlled within a certain range, otherwise it will also cause adverse consequences. Rapid heating should be controlled within an appropriate range and must be heated in accordance with the requirements of the catalyst technical documents, otherwise the catalyst will lose its activity before reaching its service life and will have to be replaced again.

[0007] It should be noted that the above contents belong to the technical cognition scope of the inventor. Since the technical contents in this field are vast and too complicated, the above contents of this application do not necessarily constitute prior art. Summary of the invention

[0008] 1. Technical problems to be solved by the invention: The present invention provides a gas-deposited graphene coating device based on a fluidized bed, which is used to solve the technical problems existing in the above-mentioned background technology.

[0009] 2. Technical solution: To achieve the above-mentioned purpose, the technical solution provided by the present invention is: a gas-deposited graphene coating device based on a fluidized bed, comprising a discharge module and a reactor body, a heightened section is provided between the reactor body and the discharge module, and a plunger is provided at the connection between the lower end of the reactor body and the heightened section, wherein the discharge module comprises a cylinder rod, a discharge valve and a cylinder, the upper and lower ends of the cylinder rod are respectively connected to the plunger and one end of the telescopic rod of the cylinder, the heightened section has a cavity connected to the reactor body, the plunger has an air inlet channel 1, a plurality of air holes are opened around the air inlet channel 1, the upper end of the cylinder rod has an air inlet channel 2, and one side of the air inlet channel 2 is provided with an air inlet connected thereto.

[0010] Further optimized, the upper end of the elevated section is welded and fixed to the reactor body, the lower end of the elevated section is connected to the discharge valve via a welding flange, the lower end of the cavity is communicated with the discharge valve, and the cylinder rod is arranged in the cavity.

[0011] For further optimization, a fixing ring is provided at one end of the cylinder rod close to the plunger, and the plunger is threadedly connected to the cylinder rod.

[0012] Further optimized, the air intake channel 1 is connected to the air intake channel 2, and the air intake channel 1 is connected to the plurality of air holes.

[0013] Further optimized, the plunger includes a positioning portion and an air intake portion, and the air intake channel one and the plurality of air holes are all opened on the air intake portion.

[0014] Further optimized, the reactor body has a conical cavity and a reaction cavity inside, the air inlet portion is located in the conical cavity, and the positioning portion is abuttingly connected to the bottom end of the conical cavity.

[0015] Further optimized, the plurality of air holes are arranged at equal distances in the circumferential direction of the air inlet portion, and the number of the plurality of air holes is at least 20.

[0016] Further optimized, an angle a is formed between the air hole and the air inlet channel 1, and an angle b is formed between the air hole and the air inlet pipe wall.

[0017] Further optimized, the discharge valve is a downward-expanding discharge valve, and a cylinder fixing rod flange is provided between the discharge valve and the cylinder.

[0018] 3. Beneficial effects: Compared with the prior art, the technical solution provided by the present invention has the following beneficial effects: The present invention is reasonably designed. By adopting a structure in which the internal reaction zone is elevated, the reaction temperature is increased to reach 1100 degrees, which is the required reaction temperature, so that the catalytic reaction effect is better. In addition, the combined structure of the plunger and the cylinder rod is used to achieve uniform gas intake, so that the catalyst reacts better, the service life of the catalyst is extended, and the fluidization state is further optimized.

[0019] It should be noted that the structures not introduced in the present invention are the same as the prior art or can be implemented by using the prior art, and are not described in detail here because they do not involve the design points and improvement directions of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a schematic diagram of the overall structure of the present invention; Figure 2 It is a partial structural cross-sectional view of the present invention; Figure 3 Another partial structural cross-sectional view of the present invention; Figure 4 It is a cross-sectional view of the plunger structure of the present invention; Figure 5 This is a cross-sectional view of the plunger structure from another angle of the present invention.

[0021] Reference numerals: 1. Reactor body; 101. Conical cavity; 102. Reaction cavity; 2. Heightened section; 201. Cavity; 3. Plunger; 301. Positioning part; 302. Air inlet part; 303. Air inlet channel 1; 304. Air hole; 4. Cylinder rod; 401. Air inlet channel 2; 402. Air inlet; 5. Discharge valve; 6. Cylinder; 7. Fixing ring; 8. Welding flange; 9. Cylinder fixing rod flange. DETAILED DESCRIPTION

[0022] To facilitate understanding of the present invention, the present invention will be described more comprehensively below with reference to the relevant drawings. Several embodiments of the present invention are shown in the drawings. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thorough and comprehensive.

[0023] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "page", "bottom", "inside", "outside", "clockwise", "counterclockwise" and the like indicating orientations or positional relationships are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as limiting the present invention.

[0024] In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present invention, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0025] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", "fixed", "provided with", "provided on" and the like should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances. Example

[0026] See attached Figure 1-5A gas-phase deposited graphene coating device based on a fluidized bed comprises a discharge module and a reactor body 1, a heightened section 2 is provided between the reactor body 1 and the discharge module, a plunger 3 is provided at the connection between the lower end of the reactor body 1 and the heightened section 2, wherein the discharge module comprises a cylinder rod 4, a discharge valve 5 and a cylinder 6, the upper and lower ends of the cylinder rod 4 are respectively connected to the plunger 3 and one end of the telescopic rod of the cylinder 6, the heightened section 2 comprises a cavity 201 connected to the reactor body 1, the plunger 3 comprises an air inlet channel 1 303, a plurality of air holes 304 are provided around the air inlet channel 1 303, the upper end of the cylinder rod 4 comprises an air inlet channel 2 401, and one side of the air inlet channel 2 401 is provided with an air inlet port 402 connected thereto.

[0027] See attached Figure 1-5 The upper end of the heightened section 2 is welded and fixed to the reactor body 1, and the lower end of the heightened section 2 is connected to the discharge valve 5 through a welding flange 8. The lower end of the cavity 201 is connected to the discharge valve 5, and the cylinder rod 4 is arranged in the cavity 201. The heightened section 2 is welded and fixed at the top and bottom, and a connecting structure is formed after being sealed and connected to the inside of the reactor body 1 and the discharge valve 5. The connecting design between the heightened section 2 and the reactor body 1 can increase the reaction temperature and enable the catalyst reactor to achieve a stable heating rate. The heating rate is controlled within the range permitted by the equipment stress and the characteristics of the catalyst itself to ensure that the temperature required for the reaction reaches 1100 degrees inside the reactor, so that the catalyst can achieve a more sufficient reaction and the fluidized bed has a good initial fluidized state. If the temperature is increased too quickly, it is easy to cause the catalyst to split or even burst, which not only affects the life of the catalyst, but also increases the resistance of the reactor, thereby destroying the physical strength of the catalyst and preventing the catalyst from losing its activity before reaching its service life.

[0028] See attached Figure 1-5 , a fixing ring 7 is further provided at one end of the cylinder rod 4 close to the plunger 3, the plunger 3 is threadedly connected to the cylinder rod 4, the air inlet channel 1 303 is communicated with the air inlet channel 2 401, and the air inlet channel 1 303 is communicated with a plurality of air holes 304, the plunger 3 includes a positioning portion 301 and an air inlet portion 302, the air inlet channel 1 303 and the plurality of air holes 304 are all provided on the air inlet portion 302, in this technical solution, the cylinder rod 4 plays the role of air intake and upper and lower connection of the plunger 3 and the cylinder 6, the gas is input through the air inlet port 402 provided on the cylinder rod 4, after the gas enters the air inlet channel 2 401, it is transported upward to the air inlet channel 1 301 on the plunger 3, and finally the gas is discharged from a plurality of evenly distributed air holes 304; See attached Figure 1-5The lower end of the cylinder rod 4 is moved up and down in the heightened section 2 through the extension and contraction of the cylinder 6, driving the plunger 3 threadedly connected thereto to move up and down, which is used to control the opening and closing of the catalyst discharge channel. When the reactor is working, the plunger 3 is in an ascending state, and when the reactor stops working, the plunger 3 is in a descending state, which is used to catalyze the discharge of the catalyst and replace the catalyst; the plunger 3 drives the cylinder rod 4 to descend through the cylinder 6, and the lower port of the reactor body flows out, and the inactive catalyst falls downward from the conical cavity 101 into the cavity 201 of the heightened section 2, and is finally discharged from the discharge valve 5.

[0029] See attached Figure 1-5 The reactor body 1 has a conical cavity 101 and a reaction cavity 102 inside, the air inlet 302 is located in the conical cavity 101, and the positioning portion 302 is connected to the bottom end of the conical cavity 101 in abutment with each other. The reactor body 1 adopts an open conical cavity 101 structure with a diameter gradually expanding upward, and a gas distribution plate is installed between the conical cavity 101 and the reaction cavity 102. The gas distribution plate has the function of uniformly distributing the gas, and at the same time, its pressure drop is small. The catalyst is placed on the gas distribution plate, and the gas distribution plate is used to ensure that the fluidized bed has good and stable fluidization. Therefore, the conical cavity 101 is in an empty state, and the mouth of the lower end of the conical cavity 101 is movably connected to the positioning portion 302 of the plunger 3, and the air inlet 302 is placed in the conical cavity 101 as a whole, so that the upper end of the air inlet 302 is as close to the catalyst as possible.

[0030] See attached Figure 1-5 , multiple air holes 304 are arranged at equal distances in the circumferential direction of the air inlet part 302, and the spacing between the upper and lower parts is also arranged at equal distances. The number of multiple air holes 304 is at least 20, which not only meets the intake flow rate, but also ensures the uniformity of the gas. The air holes 304 are uniform small holes with a diameter of 0.5 mm. There is an angle a between the air holes 304 and the air inlet channel 1 303, and there is an angle b between the air holes 304 and the tube wall of the air inlet part 302. Multiple air holes 304 are evenly distributed on the column of the air inlet part 302, connected with the air inlet channel 1 303, and are arranged to be tilted downward to form an angle a of 10°-15°, and are arranged around the air inlet part 302, all deviating from the radial direction to form an angle b of 20°-25°. After the gas flows out of the air holes 304, a downward, rotating and upward airflow is formed, so that the gas intake is more uniform when entering the reactor. The rotating airflow can better hold up the catalyst particles, make the particles violently stirred, and achieve a better fluidized state.

[0031] In this embodiment, by adding a heightened section 2 between the reactor body 1 and the discharge module, the effect of increasing the reaction temperature can be achieved, ensuring that the catalyst inside the reactor reaches the required reaction temperature of 1100 degrees, so that the catalyst can achieve a more sufficient and better reaction effect; in addition, by providing a plunger 3 and a cylinder rod 4 connecting structure at the bottom of the reactor body 1, the cylinder 6 retracts during discharge, driving the cylinder rod 4 and the plunger 3 to descend, and when air is inhaled, the cylinder 6 extends to push the cylinder rod 4 and the plunger 3 upward until the plunger 3 enters the conical cavity 10 of the reactor body 1. 1, the gas supply system is connected through the air inlet 402 on the cylinder rod 4 to intake air into the reactor, realizing the switching effect of the air inlet channel and the catalyst discharge channel; a plurality of uniform air holes 304 with a diameter of 0.5 mm are opened on the plunger 3. After the gas enters the air inlet channel 1 301 on the plunger 3 through the air inlet 402 on the cylinder rod 4 and the air inlet channel 2 401, it is discharged from the plurality of air holes 304 arranged at equal distances. The gas enters the reactor body 1 in a downward, rotating and upward path, realizing uniform gas intake, improving the fluidized state, and extending the service life of the catalyst.

[0032] In summary, by adopting a structure in which the internal reaction zone is elevated, the reaction temperature can be increased to reach the reaction requirement of 1100 degrees, so that the catalytic reaction effect is better, and the combined structure of the plunger and the cylinder rod can achieve uniform gas intake, so that the catalyst reacts better, the service life of the catalyst is extended, and the fluidization state is further optimized.

[0033] The above-described embodiments only express a certain implementation mode of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the patent scope of the present invention. It should be pointed out that, for ordinary technicians in this field, several modifications and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be based on the attached claims.

Claims

1. A fluidized bed-based gas-phase deposited graphene coating device, comprising a discharge module and a reactor body (1), characterized in that: A raised section (2) is provided between the reactor body (1) and the discharge module, and a plunger (3) is provided at the connection between the lower end of the reactor body (1) and the raised section (2), wherein the discharge module comprises a cylinder rod (4), a discharge valve (5) and a cylinder (6), the upper and lower ends of the cylinder rod (4) being respectively connected to the plunger (3) and one end of the telescopic rod of the cylinder (6), the raised section (2) having a cavity (201) connected to the reactor body (1), the plunger (3) having an air inlet channel 1 (303), a plurality of air holes (304) being provided around the air inlet channel 1 (303), and the upper end of the cylinder rod (4) having an air inlet channel 2 (401), a side of which is provided with an air inlet port (402) connected thereto.

2. The device for coating graphene by vapor deposition based on a fluidized bed according to claim 1, characterized in that: The upper end of the raised section (2) is welded and fixed to the reactor body (1), the lower end of the raised section (2) is connected to the discharge valve (5) via a welding flange (8), the lower end of the cavity (201) is connected to the discharge valve (5), and the cylinder rod (4) is arranged in the cavity (201).

3. The device for coating graphene by vapor deposition based on a fluidized bed according to claim 1, characterized in that: A fixing ring (7) is also provided at one end of the cylinder rod (4) close to the plunger (3), and the plunger (3) is threadedly connected to the cylinder rod (4).

4. The device for coating graphene by vapor deposition based on a fluidized bed according to claim 1, characterized in that: The air inlet channel one (303) is connected to the air inlet channel two (401), and the air inlet channel one (303) is connected to the plurality of air holes (304).

5. The device for coating graphene by vapor deposition based on a fluidized bed according to claim 1, characterized in that: The plunger (3) comprises a positioning portion (301) and an air intake portion (302), and the air intake channel 1 (303) and the plurality of air holes (304) are all provided on the air intake portion (302).

6. The device for coating graphene by vapor deposition based on a fluidized bed according to claim 5, characterized in that: The reactor body (1) has a conical cavity (101) and a reaction cavity (102) inside, the air inlet portion (302) is located inside the conical cavity (101), and the positioning portion (302) is abuttingly connected to the bottom end of the conical cavity (101).

7. The device for coating graphene by vapor deposition based on a fluidized bed according to claim 6, characterized in that: The plurality of air holes (304) are arranged at equal distances in the circumferential direction of the air inlet portion (302), and the number of the plurality of air holes (304) is at least 20.

8. The device for coating graphene by vapor deposition based on a fluidized bed according to claim 7, characterized in that: An included angle a is formed between the air hole (304) and the first air inlet channel (303), and an included angle b is formed between the air hole (304) and the tube wall of the air inlet portion (302).

9. The graphene coating device based on fluidized bed vapor deposition according to claim 1, characterized in that: The discharge valve (5) is a downward-expanding discharge valve, and a cylinder fixing rod flange (9) is provided between the discharge valve (5) and the cylinder (6).