A multi-tube fully automatic carbon nanotube continuous preparation equipment

Abstract

The present invention discloses a multi-tube type fully automatic carbon nanotube continuous preparation equipment. The present invention can independently grow a single tube or simultaneously grow multiple tubes of carbon nanotubes during the growth process through the multi-tube design; a stainless steel vacuum chamber allows the entire furnace to be in a sealed space, and is used to introduce protective gas to protect the furnace tubes from being broken or cracked due to thermal vibration; two receiving reels collect the carbon nanotubes grown in two rows of furnace tubes, and an inverted collection trough is provided at the lower end of the furnace body and is sealed correspondingly to a water trough for auxiliary collection and observation; an exhaust port on the collection trough is provided with an exhaust gas anti-blocking device, which is mainly used to collect carbon nanotubes doped in the exhaust gas to prevent the exhaust port from being blocked.

Description

Technical Field

[0001] The invention relates to the technical field of carbon nanotube growth equipment, and in particular to multi-tube type fully automatic carbon nanotube continuous preparation equipment. Background Art

[0002] The main methods currently used to prepare carbon nanotubes include graphite arc method, chemical vapor deposition method and laser method. Among them, the CVD method is widely used because of its simple process, easy control of parameters, pure and controllable products, and high yield production of carbon nanotubes.

[0003] Existing carbon nanotube preparation equipment and technology often use vapor deposition method for preparation. This method decomposes carbon-containing raw compounds into carbon atoms at a relatively high temperature. Under the action of transition metal catalysts, the carbon atoms adhere to the surface of catalyst particles to form carbon nanotubes. Although this method is effective, due to the limitation of substrate size, the growth of carbon nanotubes is also limited, and carbon nanotubes cannot be grown continuously. Summary of the invention

[0004] In order to overcome the above technical problems, the purpose of the present invention is to provide a multi-tube type fully automatic carbon nanotube continuous preparation equipment. The present invention places the heating furnace in a stainless steel vacuum chamber. During the experimental heating process, the corundum furnace tube may break or crack due to thermal vibration. However, in the vacuum chamber, an inert protective atmosphere is introduced during the experiment. Even if the tube breaks during the heating process, it will not damage the thermal field, the experimental progress and the growth of carbon nanotubes. Independent liquid injection devices and growth devices can grow carbon nanotubes separately at one time or in multiple experimental methods at the same time.

[0005] The present invention uses a multi-tube design to independently grow a single tube or simultaneously grow multiple tubes of carbon nanotubes during the growth process; the stainless steel vacuum chamber allows the entire furnace to be in a sealed space, which is used to pass protective gas to protect the furnace tubes from being broken or cracked due to thermal vibration; two receiving reels collect the carbon nanotubes grown in the two rows of furnace tubes, and an inverted collection tank is provided at the lower end of the furnace body and is sealed corresponding to a water tank for auxiliary collection and observation; an exhaust port on the collection tank is provided with an exhaust gas anti-blocking device, which is mainly used to collect carbon nanotubes doped in the exhaust gas to prevent the exhaust port from being blocked.

[0006] The purpose of the present invention can be achieved by the following technical solutions:

[0007] A multi-tube type fully automatic carbon nanotube continuous preparation equipment, comprising a stainless steel vacuum chamber, a heating furnace, and a bracket, wherein the stainless steel vacuum chamber is fixedly installed on the top of the bracket, the stainless steel vacuum chamber is provided with a heating furnace, the heating furnace is provided with two rows of furnace tubes, the upper ends of the furnace tubes extend outside the stainless steel vacuum chamber, a water cooling flange is fixedly installed on the top of the furnace tube, a liquid injection port and an inner tube temperature measuring port are provided on the water cooling flange, and the liquid injection port is connected to a liquid injection pump through a pipeline; a discharge port is provided at the bottom of the furnace tube, the lower end of the furnace tube extends into an inverted collection tank, and the inverted collection tank is installed at the bottom of the stainless steel vacuum chamber; a material receiving reel is provided below the discharge port of the furnace tube and located in the inverted collection tank;

[0008] A lifting platform is provided inside the bracket, a cylinder is embedded inside the lifting platform, the top of the piston rod of the cylinder is connected to the water tank, the top of the lifting platform is connected to the water tank through a guide column, and the top of the water tank contacts the notch of the inverted collection tank.

[0009] As a further solution of the present invention: an air inlet is provided on one side of the stainless steel vacuum chamber, and an exhaust port 2 is provided on the other side of the stainless steel vacuum chamber.

[0010] As a further solution of the present invention: each row of furnace tubes is provided with three furnace tubes, and the three furnace tubes are arranged at equal distances.

[0011] As a further solution of the present invention: two receiving reels are arranged in parallel, and each receiving reel collects carbon nanotubes grown in three furnace tubes.

[0012] As a further solution of the present invention: an exhaust gas blocking prevention device is arranged on one side of the inverted collecting tank, and the exhaust gas blocking prevention device comprises a box body, a rotating motor is fixedly installed at one end inside the box body, a filter drum is rotatably installed at the other end of the box body, a filter is wound on the filter drum, a clamping roller is arranged inside the box body and at one end close to the rotating motor, a gas inlet is opened at the contact point between the box body and the inverted collecting tank, and an exhaust port is opened on the other side of the box body.

[0013] As a further solution of the present invention: a speed regulating motor is installed on one side of the inverted collecting trough, and the output shaft of the speed regulating motor is connected to the material receiving reel.

[0014] As a further solution of the present invention, the working steps of the multi-tube type fully automatic carbon nanotube continuous preparation equipment are as follows: 200 ml of ethanol and ferrocene mixed solution is loaded into the injection pump, 150 sccm of nitrogen is introduced into the stainless steel vacuum chamber through the air inlet, and discharged through the exhaust port 2, water is added to the water tank to overflow the notch of the inverted collection tank, and the vacuum pump is used to evacuate the vacuum to 5*10 -1At pa, the carbon silicon rod in the heating furnace is turned on to raise the temperature to 1200℃. When the temperature of the inner tube temperature measuring port reaches 200℃, the injection pump is turned on to inject the mixed liquid. At the same time, the speed regulating motor is started to drive the receiving reel to rotate for receiving the material. After the reaction of the mixed liquid by the injection pump is completed, the temperature is lowered. When the temperature drops to room temperature, it starts to break through the air, lower the water tank, and collect the carbon nanotubes.

[0015] The beneficial effects of the present invention are as follows: the heating furnace is placed in a stainless steel vacuum chamber. During the experimental heating process, the corundum furnace tube may break or crack due to thermal vibration. However, in the vacuum chamber, an inert protective atmosphere is introduced during the experiment. Even if the tube breaks during the heating process, the thermal field, experimental progress and carbon nanotube growth will not be damaged. The independent liquid injection device and growth device can grow carbon nanotubes separately at one time or in multiple experimental methods at the same time.

[0016] Through the multi-tube design, carbon nanotubes can be grown independently in a single tube or simultaneously in multiple tubes during the growth process; the stainless steel vacuum chamber allows the entire furnace to be in a sealed space, which is used to pass protective gas to protect the furnace tubes from breaking or cracking due to thermal vibration; two receiving reels collect the carbon nanotubes grown in the two rows of furnace tubes, and an inverted collection trough is provided at the lower end of the furnace body and is sealed corresponding to the water trough to assist in collection and observation; an exhaust port on the collection trough is provided with an exhaust gas anti-blocking device, which is mainly used to collect carbon nanotubes doped in the exhaust gas to prevent the outlet from being blocked. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] The present invention will be further described below in conjunction with the accompanying drawings.

[0018] Figure 1 It is a front view structural schematic diagram of the present invention;

[0019] Figure 2 yes Figure 1 Schematic diagram of the structure from the middle side;

[0020] Figure 3 It is a schematic diagram of the overall structure of the tail gas anti-blocking device of the present invention.

[0021] In the figure: 1. liquid injection port; 2. inner tube temperature measuring port; 3. water-cooling flange; 4. stainless steel vacuum chamber; 5. heating furnace; 6. discharge port; 7. exhaust port 1; 8. tail gas blocking prevention device; 9. water tank; 10. material collection drum; 11. lifting platform; 12. speed regulating motor; 13. liquid injection pump; 14. air inlet; 15. exhaust port 2; 16. furnace tube; 17. inverted collecting tank; 18. bracket; 19. cylinder; 20. box; 21. rotating motor; 22. filter screen; 23. filter screen drum; 24. pressing roller. DETAILED DESCRIPTION

[0022] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] See also Figure 1-3 As shown, a multi-tube fully automatic carbon nanotube continuous preparation equipment includes a liquid injection port 1, an inner tube temperature measuring port 2, a water cooling flange 3, a stainless steel vacuum chamber 4, a heating furnace 5, a discharge port 6, an exhaust port 1 7, an exhaust gas blocking prevention device 8, a water tank 9, a material receiving reel 10, a lifting platform 11, a speed regulating motor 12, a liquid injection pump 13, an air inlet 14, an exhaust port 2 15, a furnace tube 16, an inverted collecting tank 17, and a bracket 18. A stainless steel vacuum chamber 4 is fixedly installed on the top of the bracket 18 to keep the entire furnace in a sealed space to prevent gas leakage. A heating furnace 5 is arranged inside the stainless steel vacuum chamber 4. Silicon carbon rods are installed in the heating furnace 5. The silicon carbon rods are heated , the heating temperature can reach 1400°C, two rows of furnace tubes 16 are arranged inside the heating furnace 5, the upper ends of the furnace tubes 16 extend to the outside of the stainless steel vacuum chamber 4, a water-cooling flange 3 is fixedly installed on the top of the furnace tube 16, the water-cooling flange 3 plays a sealing role, a liquid injection port 1 and an inner tube temperature measuring port 2 are provided on the water-cooling flange 3, and the liquid injection port 1 is connected to the liquid injection pump 13 through a pipeline; a discharge port 6 is provided at the bottom of the furnace tube 16, and the lower end of the furnace tube 16 extends to an inverted collecting tank 17, and the inverted collecting tank 17 is installed at the bottom of the stainless steel vacuum chamber 4; a material receiving reel 10 is provided below the discharge port 6 of the furnace tube 16 and in the inverted collecting tank 17;

[0024] A lifting platform 11 is provided inside the bracket 18, and a cylinder 19 is embedded and installed inside the lifting platform 11. The top of the piston rod of the cylinder 19 is connected to the water tank 9. The top of the lifting platform 11 is connected to the water tank 9 through a guide column, and the top of the water tank 9 contacts the notch of the inverted collecting tank 17.

[0025] An air inlet 14 is provided on one side of the stainless steel vacuum chamber 4 to allow inert gas to enter the vacuum chamber, and an exhaust port 15 is provided on the other side of the stainless steel vacuum chamber 4 to exhaust the inert gas from the vacuum chamber.

[0026] Each row of furnace tubes 16 is provided with three furnace tubes 16 , and the three furnace tubes 16 are arranged at equal distances.

[0027] Two receiving reels 10 are arranged in parallel, and each receiving reel 10 collects carbon nanotubes grown in three furnace tubes 16 .

[0028] An exhaust gas blocking prevention device 8 is provided on one side of the inverted collection tank 17. The exhaust gas blocking prevention device 8 includes a box 20. A rotating motor 21 is fixedly installed at one end of the box 20. A winding roller is installed on the output shaft of the rotating motor 21. A filter screen reel 23 is rotatably installed on the other end of the box 20. A filter screen 22 is wound on the filter screen reel 23. A pressing roller 24 is provided at one end of the box 20 near the rotating motor 21. A gas inlet is provided at the contact point between the box 20 and the inverted collection tank 17. An exhaust port 7 is provided on the other side of the box 20. Gas enters the gas inlet, and the filter screen 22 is filtered, driving the rotating motor 21 to rotate. The filter screen 22 after use is wound by the winding roller, ensuring a better filtering effect of the filter screen 22, and preventing the exhaust port 7 from being blocked by the carbon nanotubes doped with the exhaust gas.

[0029] A speed regulating motor 12 is installed on one side of the inverted collecting trough 17 , and an output shaft of the speed regulating motor 12 is connected to the receiving reel 10 .

[0030] The working steps of the multi-tube type fully automatic carbon nanotube continuous preparation equipment are as follows: 200 ml of ethanol and ferrocene mixed solution is loaded into the injection pump, 150 sccm of nitrogen is introduced into the stainless steel vacuum chamber 4 through the air inlet 14, and discharged through the exhaust port 15, water is added to the water tank 9 to overflow the notch of the inverted collection tank 17, and the vacuum pump is used to evacuate the vacuum to 5*10 -1 At pa, the heating furnace 5 is turned on to raise the temperature of the carbon silicon rods in the furnace to 1200°C. When the temperature of the inner tube temperature measuring port 2 reaches 200°C, the injection pump is turned on to inject the mixed liquid. At the same time, the speed regulating motor 12 is started to drive the material receiving reel 10 to rotate for receiving the material. After the reaction of the mixed liquid by the injection pump is completed, the temperature is lowered. When the temperature drops to room temperature, it starts to break through the air. The lifting platform 11 lowers the water tank to collect the carbon nanotubes.

[0031] The working principle of the present invention is as follows: the heating furnace is placed in a stainless steel vacuum chamber. During the experimental heating process, the corundum furnace tube may break or crack due to thermal vibration. However, in the vacuum chamber, an inert protective atmosphere is introduced during the experiment. Even if the tube breaks during the heating process, it will not damage the thermal field, the experimental progress and the growth of carbon nanotubes. The independent liquid injection device and the growth device can grow carbon nanotubes separately at one time or in multiple experimental methods at the same time.

[0032] Through the multi-tube design, carbon nanotubes can be grown independently in a single tube or simultaneously in multiple tubes during the growth process; the stainless steel vacuum chamber allows the entire furnace to be in a sealed space, which is used to pass protective gas to protect the furnace tubes from breaking or cracking due to thermal vibration; two receiving reels collect the carbon nanotubes grown in the two rows of furnace tubes, and an inverted collection trough is provided at the lower end of the furnace body and is sealed corresponding to the water trough to assist in collection and observation; an exhaust port on the collection trough is provided with an exhaust gas anti-blocking device, which is mainly used to collect carbon nanotubes doped in the exhaust gas to prevent the outlet from being blocked.

[0033] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0034] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.

Claims

1. A multi-tube fully automatic carbon nanotube continuous preparation equipment, characterized in that: The invention comprises a stainless steel vacuum chamber (4), a heating furnace (5), and a bracket (18), wherein the stainless steel vacuum chamber (4) is fixedly mounted on the top of the bracket (18), the interior of the stainless steel vacuum chamber (4) is provided with a heating furnace (5), the interior of the heating furnace (5) is provided with two rows of furnace tubes (16), the upper ends of the furnace tubes (16) extend outside the stainless steel vacuum chamber (4), the top of the furnace tubes (16) is fixedly mounted with a water cooling flange (3), and the water cooling flange (3 ) is provided with a liquid injection port (1) and an inner tube temperature measuring port (2), the liquid injection port (1) being connected to a liquid injection pump (13) through a pipeline; a discharge port (6) is provided at the bottom of the furnace tube (16), the lower end of the furnace tube (16) extending into an inverted collection tank (17), the inverted collection tank (17) being installed at the bottom of the stainless steel vacuum chamber (4); a material receiving reel (10) is provided below the discharge port (6) of the furnace tube (16) and located in the inverted collection tank (17); A lifting platform (11) is provided inside the bracket (18), a cylinder (19) is embedded and installed inside the lifting platform (11), the top of the piston rod of the cylinder (19) is connected to the water tank (9), the top of the lifting platform (11) is connected to the water tank (9) via a guide column, and the top of the water tank (9) is in contact with the notch of the inverted collection tank (17); An air inlet (14) is provided on one side of the stainless steel vacuum chamber (4), and a second exhaust port (15) is provided on the other side of the stainless steel vacuum chamber (4); Each row of furnace tubes (16) is provided with three furnace tubes, and the three furnace tubes (16) are arranged at equal distances; Two of the material receiving reels (10) are arranged in parallel, and each of the material receiving reels (10) collects the carbon nanotubes grown by three furnace tubes (16); A speed regulating motor (12) is installed on one side of the inverted collecting trough (17), and an output shaft of the speed regulating motor (12) is connected to a material receiving reel (10).

2. The multi-tube fully automatic carbon nanotube continuous preparation equipment according to claim 1, characterized in that: An exhaust gas blocking prevention device (8) is arranged on one side of the inverted collection tank (17), and the exhaust gas blocking prevention device (8) comprises a box body (20), a rotating motor (21) is fixedly mounted on one end of the box body (20), a filter screen reel (23) is rotatably mounted on the other end of the box body (20), a filter screen (22) is wound around the filter screen reel (23), a pressing roller (24) is arranged inside the box body (20) and at one end close to the rotating motor (21), a gas inlet is provided at a contact point between the box body (20) and the inverted collection tank (17), and an exhaust port (7) is provided on the other side of the box body (20).

3. A working method of the multi-tube fully automatic carbon nanotube continuous preparation equipment according to claim 1 or 2, characterized in that: The working steps of the multi-tube type fully automatic carbon nanotube continuous preparation equipment are as follows: 200 ml of ethanol and ferrocene mixed solution is loaded into the injection pump, 150 sccm of nitrogen is introduced into the stainless steel vacuum chamber (4) through the air inlet (14), and discharged through the second exhaust port (15), water is added to the water tank (9) to overflow the notch of the inverted collection tank (17), and the vacuum pump is used to evacuate the vacuum to a vacuum of 5×10 -1 At pa, the heating furnace (5) is turned on to raise the temperature of the carbon silicon rod in the furnace to 1200°C. When the temperature of the inner tube temperature measuring port (2) reaches 200°C, the liquid injection pump is turned on to inject the mixed liquid. At the same time, the speed regulating motor (12) is started to drive the material receiving reel (10) to rotate to receive the material. After the reaction of the mixed liquid in the liquid injection pump is completed, the temperature is lowered. When the temperature drops to room temperature, it starts to break through the air, lowers the water tank, and collects the carbon nanotubes.

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