A gas intercalation reaction device

Abstract

This invention discloses a gas intercalation reaction apparatus, relating to the field of graphene preparation technology. It includes a frame, an operation panel, a reaction vessel, a stirring mechanism, a pressure preparation mechanism, a gas storage device, a gas plunger pump, and a needle valve. The reaction vessel comprises a reaction vessel body, a first plug, and a second plug. This invention features a compact design, simple operation, few steps, high automation, and an environmentally friendly, green process, enabling the rapid and efficient preparation of high-quality graphene using a gas intercalation reaction method.

Description

Technical Field

[0001] This invention relates to the field of graphene preparation technology, and in particular to production equipment for preparing graphene using a gas intercalation reaction method. Background Technology

[0002] Graphene preparation methods are generally divided into two main categories: one is obtained directly or indirectly from natural flake graphite, such as mechanical grinding, detonation, ultrasonic methods, and electrochemical intercalation; the other is synthesized from carbon-rich materials, where atomic rearrangement occurs during the preparation process, such as pulsed laser precipitation, detonation synthesis, chemical vapor deposition, and chemical synthesis. In the first category, the prepared graphene is lacking in thickness and uniformity; while in the second category, due to the rearrangement of carbon atoms, the three-dimensional scale is smaller, resulting in higher mass production costs. Furthermore, both of these methods are not only complex but also expensive, making the development of new equipment for toner preparation of unique significance. Summary of the Invention

[0003] This invention overcomes the shortcomings of the prior art and provides a gas intercalation reaction device that uses supercritical carbon dioxide or inert gas to intercalate between graphite layers, followed by rapid pressure release for exfoliation, thereby obtaining nanoscale graphene intermediate products. This solves the technical problems of complex and costly traditional graphene preparation processes.

[0004] The technical solution of the present invention:

[0005] A gas intercalation reaction device includes a frame 1, an operation panel 2, a reaction vessel 50, a stirring mechanism 60, a pressure preparation mechanism, a gas storage device 90, a gas plunger pump 70, and a needle valve 100. The gas outlet of the gas storage device 90 is connected to the gas inlet of the gas plunger pump 70 via a gas pipe, and the gas outlet of the gas plunger pump 70 is connected to the gas inlet 51 of the reaction vessel 50 via a gas pipe.

[0006] The reactor 50 includes a reactor body 8, a first plug 5, and a second plug 35, with the first plug 5 and the second plug 35 respectively disposed at both ends of the reactor 50.

[0007] The reactor 50 is fixedly connected to a first stirring shaft 11 and a second stirring shaft 19. The first stirring shaft 11 and the second stirring shaft 19 are connected to the frame 1 through a stirring bearing 10 and a stirring bearing seat 20. The stirring mechanism 60 is connected to the second stirring shaft 19.

[0008] The pressure preparation mechanism includes a pressure-applying mechanism 80 and a hydraulic mechanism. The pressure-applying mechanism 80 is connected to the hydraulic mechanism via a liquid pipe. The hydraulic mechanism includes a first hydraulic cylinder 49, a connecting rod 38, and a second piston 40. One end of the reactor body 8 near the second plug 35 is connected to one end of the first hydraulic cylinder 49 via a first bolt 16 and a support sleeve 14. One end of the connecting rod 38 is connected to the second plug 35, and the other end is connected to the second piston 40.

[0009] The hydraulic mechanism is provided with a liquid storage channel 52 connected to the needle valve 100.

[0010] Furthermore, a first pressure cap 4 is provided on the outer side of the reactor 50 near the first plug 5, and a heat insulation sleeve 3 is provided on the outer side of the first pressure cap 4; a heating ring 7 is provided on the outer side of the reactor body 8, and a heat insulation layer 6 is provided on the outer side of the heating ring 7.

[0011] Furthermore, the first plug 5 is provided with an air inlet channel, one end of which is connected to the air pipe through the air inlet 51, and the other end of which is connected to the inner cavity of the reactor 50; the second plug 35 is connected to the second pressure cap 32 at one end near the inner cavity of the reactor, and a first sealing gasket 33 and a first O-ring 34 are provided on the outside of the connection between the second pressure cap 32 and the second plug 35.

[0012] Furthermore, the gas intercalation reaction device also includes a lifting mechanism 301, which includes a cylinder 302 and a connecting shaft 303 connected to the lifting shaft of the cylinder 302. The connecting shaft 303 is provided with a first circular hole 304. A connecting pipe 305 is fixedly connected to the first plug 5, and a second circular hole 306 is provided on the connecting pipe 305. The connecting shaft 303 and the connecting pipe 305 cooperate with each other, and the connecting shaft 303 passes through the connecting pipe 305. The first circular hole 304 and the second circular hole 306 are in the same position, and a pin 307 is inserted into the first circular hole 304 and the second circular hole 306.

[0013] Furthermore, the pressurizing mechanism 80 includes a handle 81, a pressurizing bracket 82, a piston shaft 83, a first piston 84, and a second hydraulic cylinder 85. The handle 81 is connected to one end of the piston shaft 83, and the other end of the piston shaft 83 is connected to the first piston 84. The first piston 84 is installed inside the second hydraulic cylinder 85. Rotating the handle 81 drives the first piston 84 through the piston shaft 83, and the first piston 84 moves within the second hydraulic cylinder 85. The second hydraulic cylinder 85 is provided with an injection hole and an outlet hole. The injection hole is connected to a liquid tank 86 through a first liquid valve 861, and the outlet hole is connected to the hydraulic mechanism through a liquid pipe via a second liquid valve 862.

[0014] Furthermore, a buffer pad 44 and a third plug 47 are sequentially provided at the end of the second piston 40 away from the connecting rod 38, and a fourth pressure cap 48 is provided on the outside of the third plug 47; a liquid storage channel 52 is provided between the third plug 47 and the buffer pad 44.

[0015] Furthermore, a baffle 39 is provided at the end of the second piston 40 and around the periphery of the connecting rod 38, and the second piston 40 is provided with a piston flow channel 53.

[0016] Furthermore, the gas intercalation reaction device includes a hydraulic cylinder 15, the hydraulic mechanism is placed inside the hydraulic cylinder 15, the end of the reaction vessel 8 away from the first plug 5 is fixedly connected to a quick connector 12, the quick connector 12 is connected to one end of the hydraulic cylinder 15 through a clamp 13, and the other end of the hydraulic cylinder 15 is connected to a container bag 17.

[0017] Furthermore, the stirring mechanism 60 includes a reducer 29, a second turntable 28, a third connecting shaft 27, a first connecting shaft 26, an adjusting rod 25, an external thread bearing 21, a second connecting shaft 22, and a first turntable 23. The output end of the reducer 29 is connected to the second turntable 28, and the second turntable 28 is connected to the third connecting shaft 27. The adjusting rod 25 is respectively provided at both ends of the first connecting shaft 26. One end of the adjusting rod 25 is connected to the third connecting shaft 27, and the other end is connected to the second connecting shaft 22 through the external thread bearing 21. The second connecting shaft 22 is connected to the first turntable 23, and the first turntable 23 is connected to the second stirring shaft 19.

[0018] Furthermore, the reaction vessel body 8 is equipped with a temperature sensor 9 and a pressure sensor 18.

[0019] The beneficial effects of this invention are:

[0020] The equipment of this invention is compact, simple to use, requires few operations, has a high degree of automation, and the entire process is green and environmentally friendly. It can quickly and efficiently prepare high-quality graphene using gas intercalation reaction.

[0021] The reactor of this invention is equipped with plugs at both ends and a plug lifting mechanism, which facilitates the addition of materials and gas. When the temperature and pressure inside the reactor reach the process set value, the pneumatic needle valve is opened, and the pressure outside the plug at the other end suddenly decreases. Due to the huge pressure difference, the plug opens, and the gas in the reactor undergoes an intercalation reaction, causing the graphite powder to decompose. This can be used as an intermediate product for the preparation of nanoscale graphene.

[0022] The stirring mechanism can automatically stir the materials in the reactor, making the materials more evenly heated and pressurized. Attached Figure Description

[0023] Figure 1 : Overall structural diagram of the gas intercalation reaction device of the present invention;

[0024] Figure 2 : Schematic diagram of the lifting mechanism;

[0025] Figure 3 Schematic diagram of the pressurization mechanism;

[0026] Figure 4 Left view of the pressurization mechanism;

[0027] Figure 5 Schematic diagram of the reaction vessel, hydraulic device, and stirring mechanism;

[0028] Figure 6 Enlarged view of the hydraulic mechanism.

[0029] In the diagram, 1. Frame; 2. Control panel; 3. Insulation sleeve; 4. First pressure cap; 5. First plug; 6. Insulation layer; 7. Heating coil; 8. Reactor body; 9. Temperature sensor; 10. Stirring bearing; 11. First stirring shaft; 12. Quick connector; 13. Clamp; 14. Support sleeve; 15. Hydraulic cylinder; 16. First bolt; 17. Container bag; 18. Pressure sensor; 19. Second stirring shaft; 20. Stirring bearing seat; 21. External threaded spherical bearing; 22. Second connecting shaft; 23. First turntable; 25. Adjusting rod. 26. First connecting shaft; 27. Third connecting shaft; 28. Second turntable; 29. ​​Reducer; 31. Caster; 32. Second pressure cap; 33. First sealing gasket; 34. First O-ring; 35. Second plug; 36. Third pressure cap; 38. Connecting rod; 39. Baffle; 40. Second piston; 44. Buffer pad; 47. Third plug; 48. Fourth pressure cap; 49. First hydraulic cylinder; 50. Reactor; 51. Air inlet; 52. Liquid storage channel; 53. Piston flow channel; 60. Stirring mechanism; 70. Gas plunger pump.

[0030] Pressurization mechanism 80, handle 81, pressurization bracket 82, piston shaft 83, first piston 84, second hydraulic cylinder 85, liquid tank 86, first liquid valve 861, second liquid valve 862.

[0031] Gas storage device 90, needle valve 100

[0032] Lifting mechanism 301, cylinder 302, connecting shaft 303, first round hole 304, connecting pipe 305, second round hole 306, pin 307. Detailed Implementation

[0033] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments. The following embodiments are explanations of the present invention, but the present invention is not limited to the following embodiments.

[0034] Reference Figure 1A gas intercalation reaction apparatus includes a frame 1, an operation panel 2, a reaction vessel 50, a stirring mechanism 60, a pressure preparation mechanism, a gas storage device 90, a gas plunger pump 70, a needle valve 100, and a lifting mechanism 301. The operation panel 2, lifting mechanism 301, reaction vessel 50, stirring mechanism 60, gas plunger pump 70, pressure preparation mechanism, and needle valve 100 are integrated on the frame. The frame is equipped with casters 31 for easy movement. The reaction vessel serves as the reaction container for graphite powder, which undergoes an intercalation reaction under supercritical carbon dioxide conditions, resulting in graphite powder decomposition. The pressure preparation mechanism pressurizes a storage agent such as water, which exerts pressure on the lower plug of the reaction vessel, increasing the temperature and pressure within the vessel. The stirring mechanism oscillates the reaction vessel, agitating the materials and ensuring more uniform temperature and pressure within the vessel. The gas plunger pump injects carbon dioxide into the reaction vessel.

[0035] The outlet of the gas storage device 90 is connected to the inlet of the gas plunger pump 70 via a capillary tube, and the outlet of the gas plunger pump 70 is connected to the inlet 51 of the reaction vessel 50 via a capillary tube. The gas storage device 90 can be a gas cylinder or a gas storage station, depending on the scale of production. An operation panel is mounted on the frame for monitoring and operating equipment data.

[0036] Reference Figure 5 , Figure 6 The reactor 50 includes a reactor body 8, a first plug 5, and a second plug 35, which are respectively disposed at both ends of the reactor 50. The reactor 50 is fixedly connected to a first stirring shaft 11 and a second stirring shaft 19. The first stirring shaft 11 and the second stirring shaft 19 are connected to the frame 1 via a stirring bearing 10 and a stirring bearing seat 20. The stirring mechanism 60 is connected to the second stirring shaft 19.

[0037] Reference Figure 3 , Figure 4 , Figure 5 , Figure 6 The pressure preparation mechanism includes a pressurizing mechanism 80 and a hydraulic mechanism. The pressurizing mechanism 80 is connected to the hydraulic mechanism via a capillary tube. The hydraulic mechanism includes a first hydraulic cylinder 49, a connecting rod 38, a second piston 40, a third plug 47, and a fourth pressure cap 48. The end of the reactor body 8 near the second plug 35 is connected to one end of the first hydraulic cylinder 49 via a first bolt 16 and a support sleeve 14. One end of the connecting rod 38 is connected to the second plug 35, and the other end is connected to the second piston 40. The use of the first bolt 16 and the support sleeve 14 facilitates the disassembly of the hydraulic mechanism.

[0038] The liquid storage channel 52 of the pressurizing mechanism 80 is connected to the pneumatic needle valve 100. During pressurization, the pneumatic needle valve 100 is closed, and the water pressure in the liquid storage channel 52 increases. Before the flash explosion reaction, the pneumatic needle valve 100 is opened, the water pressure drops instantaneously, and the second piston drives the second plug to open the reaction vessel via the connecting rod. The supercritical carbon dioxide and graphite powder in the reaction vessel undergo a flash explosion reaction, and the graphite powder decomposes.

[0039] Reference Figure 5 The reactor 50 is provided with a first pressure cap 4 on the outer side of the end near the first plug 5, and a heat insulation sleeve 3 is provided on the outer side of the first pressure cap 4; a heating ring 7 is provided on the outer side of the reactor body 8, and a heat insulation layer 6 is provided on the outer side of the heating ring 7.

[0040] The first plug 5 is provided with an air inlet channel. One end of the air inlet channel is connected to a capillary tube through the air inlet 51, and the other end of the air inlet channel is connected to the inner cavity of the reaction vessel 50. (Refer to...) Figure 6 The second plug 35 is connected to a second pressure cap 32 at one end near the inner cavity of the reactor. A first sealing gasket 33 and a first O-ring 34 are provided on the outer side of the connection between the second pressure cap 32 and the second plug 35. The second pressure cap 32 and the second plug 35 are fixedly connected by slotted countersunk screws. The second pressure cap 32 serves to protect the second plug and can be easily replaced if damaged. Due to the high temperature and pressure inside the reactor, the first sealing gasket and the first O-ring seal the reactor.

[0041] Reference Figure 2 The gas intercalation reaction apparatus further includes a lifting mechanism 301, which includes a cylinder 302 and a connecting shaft 303 connected to the lifting shaft of the cylinder 302. The connecting shaft 303 has a first circular hole 304. A connecting pipe 305 is fixedly connected to the first plug 5, and the connecting pipe 305 has a second circular hole 306. The connecting shaft 303 and the connecting pipe 305 cooperate with each other, with the connecting shaft 303 passing through the connecting pipe 305. The first circular hole 304 and the second circular hole 306 are at the same horizontal position, and a pin 307 is inserted into the first circular hole 304 and the second circular hole 306. The lifting mechanism uses a cylinder as a power source to lift the reactor lid up and down.

[0042] Reference Figure 3 , Figure 4The pressurizing mechanism includes a handle 81, a pressurizing bracket 82, a piston shaft 83, a first piston 84, and a second hydraulic cylinder 85. The handle 81 is connected to one end of the piston shaft 83, and the other end of the piston shaft 83 is connected to the first piston 84. The first piston 84 is installed inside the second hydraulic cylinder 85. Rotating the handle 81 drives the first piston 84 through the piston shaft 83, and the first piston 84 moves within the second hydraulic cylinder 85. The second hydraulic cylinder 85 is provided with an injection port and an outlet port. The injection port is connected to a liquid tank 86 through a first liquid valve 861, and the outlet port is connected to the hydraulic mechanism through a capillary tube via a second liquid valve 862.

[0043] Reference Figure 6 A buffer pad 44 and a third plug 47 are sequentially arranged at the end of the second piston 40 away from the connecting rod 38. A fourth pressure cap 48 is arranged on the outside of the third plug 47. A liquid storage channel 52 is provided between the third plug 47 and the buffer pad 44, and a piston flow channel 53 is provided for the second piston 40. The piston flow channel 53 can finely adjust the pressure in the first hydraulic cylinder 49. The buffer pad 44 is used to protect the second piston and the third plug. A baffle 39 is provided at the end of the second piston and around the periphery of the connecting rod. The baffle 39 is connected to the second piston through a countersunk screw, and one side of the baffle is embedded in the periphery of the connecting rod. This device serves to connect the second piston and the connecting rod and also to provide a seal. When the water pressure in the liquid storage channel 52 increases, it pushes the second piston upward, thereby pushing the second plug towards the reactor under the action of the connecting rod, blocking the reactor.

[0044] Reference Figure 5 The gas intercalation reaction device includes a hydraulic cylinder 15, with the hydraulic mechanism housed within it. A quick-connect coupling 12 is fixedly connected to one end of the reaction vessel 8 away from the first plug 5. The quick-connect coupling 12 is connected to one end of the hydraulic cylinder 15 via a clamp 13. The other end of the hydraulic cylinder 15 is connected to a container bag 17. This structure allows for easy disassembly of the hydraulic cylinder. After a flash explosion reaction, the pyrolyzed graphite powder enters the container bag through the hydraulic cylinder.

[0045] Reference Figure 5The stirring mechanism 60 includes a reducer 29, a second turntable 28, a third connecting shaft 27, a first connecting shaft 26, an adjusting rod 25, an external threaded joint bearing 21, a second connecting shaft 22, and a first turntable 23. The output end of the reducer 29 is connected to the second turntable 28, and the second turntable 28 is connected to the third connecting shaft 27. The adjusting rod 25 is respectively installed at both ends of the first connecting shaft 26. One end of the adjusting rod 25 is connected to the third connecting shaft 27, and the other end is connected to the second connecting shaft 22 through the external threaded joint bearing 21. The second connecting shaft 22 is connected to the first turntable 23, and the first turntable 23 is connected to the second stirring shaft 19. This mechanism can realize the oscillation function of the reaction vessel, thereby stirring the materials in the reaction vessel.

[0046] Reference Figure 5 The reactor body 8 is equipped with a temperature sensor 9 and a pressure sensor 18. The temperature sensor 9 and the pressure sensor 18 are connected to the operation panel 2 via wires, which can display the temperature and pressure changes inside the reactor.

Claims

1. A gas intercalation reaction apparatus, comprising a frame (1), an operation panel (2), a reaction vessel (50), a stirring mechanism (60), a pressure preparation mechanism, a gas storage device (90), a gas plunger pump (70), and a needle valve (100), characterized in that, The outlet of the gas storage device (90) is connected to the inlet of the gas plunger pump (70) via a gas pipe, and the outlet of the gas plunger pump (70) is connected to the inlet (51) of the reaction vessel (50) via a gas pipe. The reactor (50) includes a reactor body (8), a first plug (5), and a second plug (35), with the first plug (5) and the second plug (35) respectively disposed at both ends of the reactor (50); The reactor (50) is fixedly connected to the first stirring shaft (11) and the second stirring shaft (19). The first stirring shaft (11) and the second stirring shaft (19) are connected to the frame (1) through the stirring bearing (10) and the stirring bearing seat (20). The stirring mechanism (60) is connected to the second stirring shaft (19). The pressure preparation mechanism includes a pressure-increasing mechanism (80) and a hydraulic mechanism. The pressure-increasing mechanism (80) is connected to the hydraulic mechanism through a liquid pipe. The hydraulic mechanism includes a first hydraulic cylinder (49), a connecting rod (38), and a second piston (40). The end of the reactor body (8) near the second plug (35) is connected to one end of the first hydraulic cylinder (49) through a first bolt (16) and a support sleeve (14). One end of the connecting rod (38) is connected to the second plug (35), and the other end is connected to the second piston (40). The hydraulic mechanism is provided with a liquid storage channel (52) connected to the needle valve (100); The reactor (50) has a first pressure cap (4) on the outer side of the end near the first plug (5), and a heat insulation sleeve (3) is provided on the outer side of the first pressure cap (4); a heating ring (7) is provided on the outer side of the reactor body (8), and a heat insulation layer (6) is provided on the outer side of the heating ring (7); The first plug (5) is provided with an air inlet channel. One end of the air inlet channel is connected to the air pipe through the air inlet (51), and the other end of the air inlet channel is connected to the inner cavity of the reactor (50). The second plug (35) is connected to the second pressure cap (32) at one end near the inner cavity of the reactor. A first sealing gasket (33) and a first O-ring (34) are provided on the outside of the connection between the second pressure cap (32) and the second plug (35). A buffer pad (44) and a third plug (47) are sequentially provided at the end of the second piston (40) away from the connecting rod (38), and a fourth pressure cap (48) is provided on the outside of the third plug (47); the third plug (47) and the buffer pad (44) provide the liquid storage channel (52). The end of the second piston (40) and the periphery of the connecting rod (38) are provided with baffles (39), and the second piston (40) is provided with piston flow channels (53).

2. The gas intercalation reaction apparatus according to claim 1, characterized in that, The gas intercalation reaction device further includes a lifting mechanism (301), which includes a cylinder (302) and a connecting shaft (303) connected to the lifting shaft of the cylinder (302). The connecting shaft (303) is provided with a first circular hole (304). A connecting pipe (305) is fixedly connected to the first plug (5), and a second circular hole (306) is provided on the connecting pipe (305). The connecting shaft (303) and the connecting pipe (305) cooperate with each other. The connecting shaft (303) passes through the connecting pipe (305). The first circular hole (304) and the second circular hole (306) are in the same position. A pin (307) is inserted into the first circular hole (304) and the second circular hole (306).

3. The gas intercalation reaction apparatus according to claim 1, characterized in that, The pressurizing mechanism (80) includes a handle (81), a pressurizing bracket (82), a piston shaft (83), a first piston (84), and a second hydraulic cylinder (85). The handle (81) is connected to one end of the piston shaft (83), and the other end of the piston shaft (83) is connected to the first piston (84). The first piston (84) is installed in the second hydraulic cylinder (85). Rotating the handle (81) drives the first piston (84) through the piston shaft (83), and the first piston (84) moves in the second hydraulic cylinder (85). The second hydraulic cylinder (85) is provided with an injection hole and an outlet hole. The injection hole is connected to the liquid tank (86) through a first liquid valve (861), and the outlet hole is connected to the hydraulic mechanism through a second liquid valve (862) and a liquid pipe.

4. The gas intercalation reaction apparatus according to claim 1, characterized in that, The gas intercalation reaction device includes a hydraulic cylinder (15), the hydraulic mechanism is placed inside the hydraulic cylinder (15), the reactor body (8) is fixedly connected to a quick connector (12) at one end away from the first plug (5), the quick connector (12) is connected to one end of the hydraulic cylinder (15) by a clamp (13), and the other end of the hydraulic cylinder (15) is connected to a container bag (17).

5. The gas intercalation reaction apparatus according to claim 1, characterized in that, The stirring mechanism (60) includes a reducer (29), a second turntable (28), a third connecting shaft (27), a first connecting shaft (26), an adjusting rod (25), an external tooth joint bearing (21), a second connecting shaft (22), and a first turntable (23). The output end of the reducer (29) is connected to the second turntable (28), and the second turntable (28) is connected to the third connecting shaft (27). The adjusting rod (25) is provided at both ends of the first connecting shaft (26). One end of the adjusting rod (25) is connected to the third connecting shaft (27), and the other end is connected to the second connecting shaft (22) through the external tooth joint bearing (21). The second connecting shaft (22) is connected to the first turntable (23), and the first turntable (23) is connected to the second stirring shaft (19).

6. The gas intercalation reaction apparatus according to claim 1, characterized in that, The reactor body (8) is equipped with a temperature sensor (9) and a pressure sensor (18).

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