CN-120817597-B - Method and reaction system for continuous preparation of single-walled carbon nanotubes

CN120817597BCN 120817597 BCN120817597 BCN 120817597BCN-120817597-B

Abstract

The invention belongs to the technical field of nanotubes, and discloses a method and a reaction system for continuously preparing single-walled carbon nanotubes, wherein the method and the reaction system comprise a reaction furnace, a vacuum pump is arranged on the side wall of the reaction furnace, an air pipe is arranged on the side wall of the reaction furnace on one side of the vacuum pump, an anode feeding module and a cathode feeding module are arranged on the side wall of the reaction furnace above the vacuum pump, a pressure sensor is arranged in the reaction furnace, a first receiving tank is arranged below the reaction furnace, a first cyclone separator is connected above the reaction furnace through a conduit, a second receiving tank is arranged below the first cyclone separator, a second cyclone separator is connected above the first cyclone separator through a conduit, a third receiving tank is arranged below the second cyclone separator, a fan is connected above the second cyclone separator through a conduit, the outlet end of the fan is connected with the lower part of a reaction arc, and the first receiving tank is positioned at the lower side of the outlet of the fan.

Inventors

FANG BUSI
YE SONGSHOU
You Ruibin
WEI PING

Assignees

福建中禾新材料有限公司

Dates

Publication Date: 20260505
Application Date: 20250724

Claims (4)

1. The utility model provides a reaction system for serialization preparation of single-walled carbon nanotube, including reaction furnace (1), a serial communication port, be equipped with vacuum pump (2) on reaction furnace (1) lateral wall, vacuum pump (2) and reaction furnace (1) inner chamber intercommunication, be equipped with trachea (3) on reaction furnace (1) lateral wall of vacuum pump (2) one side, be equipped with positive pole feeding module (4) and negative pole feeding module (5) on reaction furnace (1) lateral wall above vacuum pump (2), be equipped with pressure sensor in reaction furnace (1), reaction furnace (1) below is equipped with first receipts material jar (6), reaction furnace (1) top is connected with one-level cyclone (7) through the pipe, the below of one-level cyclone (7) is equipped with second receipts material jar (8), the top of one-level cyclone (7) is connected with second level cyclone (9) through the pipe, the below of second level cyclone (9) is equipped with third receipts material jar (10), the top of second level cyclone (9) is connected with fan (11) through the pipe, fan (11) exit end and the lower part of reaction is connected with first receipts material jar (6) side arc of export; the anode feeding module (4) comprises a circular tube (12), the circular tube (12) is fixed with the side wall of the reaction furnace (1), one end of the round tube (12) is positioned in the reaction furnace (1), the other end of the round tube is positioned at the outer side of the reaction furnace (1), the outer end of the round tube (12) is higher than the inner end, a nut (13) is arranged at the outer end of the round tube (12) in a rotating way, a sealing gasket is arranged between the nut (13) and the round tube (12), a ball valve (14) is arranged in the middle of the round tube (12) at the outer side of the reaction furnace (1), the ball valve (14) can isolate inner cavities of the round tubes (12) at two sides, rollers (15) are arranged in the round tube (12) at two sides of the ball valve (14), a rotating shaft of the rollers (15) extends out of the round tube (12) and is connected with a first motor (16), two first motors (16) are both fixed with the round tube (12), a valve is arranged above the second receiving tank (8) and the third receiving tank (10), a tank body below the valve is connected with a vacuum pump (2) and the air tube (3), discharge ports capable of being opened and closed are arranged on the side walls of the second receiving tank (8) and the third receiving tank (10), the cathode feeding module (5) comprises a cylinder (17), the cylinder (17) and the cylinder (17) is fixed with the side wall of the reaction furnace (1) at one end of the reaction furnace (17) and the other end of the reaction furnace (1), the material pipe (18) can axially slide relative to the cylinder (17), the inner wall of the cylinder (17) in the reaction furnace (1) is provided with a plurality of layers of rubber rings, the rubber rings are in contact with the outer wall of the material pipe (18), a second motor (19) is arranged on the outer side of the shell, a friction wheel (20) is arranged on a rotating shaft of the second motor (19), the outer wall of the material pipe (18) on the outer side of the reaction furnace (1) is in contact with the friction wheel (20), the friction wheel (20) can drive the material pipe (18) to axially move when rotating, a third motor (21) is coaxially fixed at the outer end of the material pipe (18), and the third motor (21) is in sealing connection with the end part of the material pipe (18).
2. The reaction system according to claim 1, wherein the inner cavity of the circular tube (12) between the nut (13) and the ball valve (14) is connected with the vacuum pump (2) and the air tube (3).
3. The reaction system of claim 1, wherein the side wall of the reaction furnace (1) is provided with a rectangular opening, and glass is arranged in the rectangular opening.
4. A method for continuous production of single-walled carbon nanotubes, characterized by using the reaction system of claim 1, comprising the steps of: s1, communicating an argon cylinder or a helium cylinder with a gas pipe (3), locking each valve, and checking the air tightness; S2, starting a vacuum pump (2), pumping the vacuum degree in the furnace to 0.1pa, then introducing helium or argon into the furnace to wash the furnace, and after 3 times of continuous operation, completing the furnace washing; S3, inflating the reaction furnace (1) through an argon bottle or a helium bottle, and inflating the reaction furnace to 500-800mbar, wherein the system has the function of automatically balancing the pressure, automatically stamping the reaction furnace when the pressure in the reaction chamber is insufficient, starting a vacuum pump (2) when the pressure is too high, sucking part of gas and balancing the pressure; S4, setting the voltage to be 30-50V, filling the anode and the cathode with the current of 70-150A, starting the first motor (16) and the second motor (19), and generating an electric arc at the position of the observation window by the cathode and the anode; S5, after the anode is consumed, firstly opening a nut (13), putting a new anode into the circular tube (12), screwing a ball valve (14) to enable the new anode to slide downwards, and driving the anode to take over through a first motor (16) to finish continuous feeding; And S6, firstly closing valves above the second material receiving tank (8) and the third material receiving tank (10), opening a material port, taking out materials in the materials, sealing the material port, starting a vacuum pump (2) to vacuumize the second material receiving tank (8) and the third material receiving tank (10), then filling inert gas, and finally opening the valves.

Description

Method and reaction system for continuous preparation of single-walled carbon nanotubes Technical Field The invention belongs to the technical field of nanotubes, and particularly relates to a method and a reaction system for continuously preparing single-walled carbon nanotubes. Background The single-wall carbon nano tube is used in the field of batteries due to ultrahigh conductivity and large specific surface area, is used in the field of robot skins due to softness and biocompatibility, is used in the field of aerospace due to tensile strength which is one hundred times that of steel, so that the single-wall carbon nano tube has excellent performance, can be applied to more and more fields, but the yield of the domestic single-wall carbon nano tube is always insufficient, market gaps are continuously expanded, how stable nano tubes are obtained by each research room becomes one layer of obstruction for restraining research progress, the process for preparing the single-wall carbon nano tube by an arc method is simple and mature, the equipment requirement is low, the crystallization quality is remarkably superior to that of a vapor deposition method, and the method is particularly suitable for small-scale use of the research rooms, however, continuous feeding and discharging cannot be realized at the current stage of the single-time yield is too low and is only milligrams to gram, so that if the continuous feeding and discharging of the arc method can be realized, the defect of too low yield can be made up, and the yield dilemma can be relieved. Disclosure of Invention The invention aims to provide a method and a reaction system for continuously preparing single-walled carbon nanotubes, which are used for solving the problem that the single-walled carbon nanotubes cannot be continuously fed and discharged by an arc method. In order to achieve the above purpose, the present invention adopts the following technical scheme: The utility model provides a method and reaction system for serialization preparation of single-walled carbon nanotube, including the reacting furnace, be equipped with the vacuum pump on the reacting furnace lateral wall, the vacuum pump communicates with the reacting furnace inner chamber, be equipped with the trachea on the reacting furnace lateral wall of vacuum pump one side, be equipped with positive pole feeding module and negative pole feeding module on the reacting furnace lateral wall of vacuum pump top, be equipped with pressure sensor in the reacting furnace, the reacting furnace below is equipped with first receipts material jar, there is one-level cyclone above the reacting furnace through the pipe connection, one-level cyclone's below is equipped with the second receipts material jar, there is second cyclone above the one-level cyclone through the pipe connection, the below of second cyclone is equipped with the third receipts material jar, there is the fan above the second cyclone through the pipe connection, the fan exit end is connected with the lower part of reaction arc, and first receipts material jar is located the downside of fan export. As a further description of the above technical solution: The anode feeding module comprises a circular tube, the circular tube is fixed with the side wall of the reaction furnace, one end of the circular tube is positioned in the reaction furnace, the other end of the circular tube is positioned outside the reaction furnace, the outer end of the circular tube is higher than the inner end of the circular tube, a nut is arranged at the outer end of the circular tube in a rotating mode, a sealing gasket is arranged between the nut and the circular tube, a ball valve is arranged in the middle of the circular tube outside the reaction furnace, the ball valve can isolate inner cavities of the circular tube at two sides, rollers are arranged in the circular tubes at two sides of the ball valve, a roller rotating shaft extends out of the circular tube and is connected with a first motor, and the two first motors are fixed with the circular tube. As a further description of the above technical solution: the inner cavity of the circular tube between the nut and the ball valve is connected with the vacuum pump and the air tube, so that the gas environment is ensured during continuous feeding. As a further description of the above technical solution: The cathode feeding module comprises a cylinder, wherein the cylinder is fixed with the side wall of the reaction furnace, one end of the cylinder is positioned in the reaction furnace, the other end of the cylinder is positioned at the outer side of the reaction furnace, a material pipe is arranged in the cylinder and can axially slide relative to the cylinder, a multi-layer rubber ring is arranged on the inner wall of the cylinder in the reaction furnace and is in contact with the outer wall of the material pipe, a second motor is arranged on the outer side of the shell, a friction wheel is arr