CN113279090A - System and method for preparing carbon nanotube fibers in large scale in safe atmosphere - Google Patents
System and method for preparing carbon nanotube fibers in large scale in safe atmosphere Download PDFInfo
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Abstract
The invention discloses a system and a method for preparing carbon nanotube fibers in a large scale in a safe atmosphere, and the system comprises a carbon nanotube fiber growth unit and a carbon nanotube fiber collection unit, wherein the carbon nanotube fiber growth unit is also matched with a carbon source injection unit and an airflow control unit, the carbon nanotube fiber growth unit comprises a plurality of growth chambers which are separated from each other, a cooling mechanism and an air sealing mechanism are arranged at the outlet of each growth chamber, the air sealing mechanism is at least used for spraying airflow to a region corresponding to the outlet of the growth chamber to form an air sealing layer, the air sealing layer can prevent ambient air from entering the growth chamber from the outlet of the growth chamber, and the cooling mechanism is at least used for cooling the region corresponding to the outlet of the growth chamber. The invention adopts the multi-tube growth chamber, improves the fiber yield and reduces the fiber cost; the growth chamber is in an open atmospheric environment, so that the operation convenience is improved; and a water cooling and air sealing device is arranged at the outlet of each growth chamber, so that the process safety in the large-scale preparation process is improved.
Description
Technical Field
The invention belongs to the technical field of carbon nanotube preparation, and particularly relates to a system and a method for preparing carbon nanotube fibers in a safe atmosphere on a large scale.
Background
Carbon nanotubes have excellent mechanical, electrical and thermal properties. The carbon nanotube fiber assembled by countless nanoscale carbon nanotubes has the characteristics of high strength, high toughness and high electric conductivity, is known as a new generation of high-performance fiber material, and has important application value in the fields of composite materials, energy devices, intelligent fabrics, artificial muscles and the like. The floating catalytic chemical vapor deposition method is a carbon nanotube fiber preparation technology with great development prospect. The method comprises the steps of continuously injecting a liquid carbon source into a high-temperature reaction tube furnace under the assistance of carrier gas in a certain proportion, gasifying and cracking the liquid carbon source at high temperature to form carbon nanotubes, assembling countless carbon nanotubes into a silk stocking shaped carbon nanotube fiber precursor in an aggregation mode, and preparing continuous carbon nanotube fibers by a specific collection and fiberization method. Generally, hydrogen is used as carrier gas in the process of synthesizing carbon nanotube fibers by a floating catalytic chemical vapor deposition method, so that the risk of the process and the complexity of the device are increased, and how to synthesize the carbon nanotube fibers on a large scale in a safe atmosphere becomes the research focus in the field.
Patent CN101696519A discloses a method for preparing carbon nanotube fiber in a safe atmosphere, and relates to a carbon nanotube fiber preparation device and a preparation method. Although the process only uses inert gas as carrier gas, the preparation device adopts a water seal structure, and the operation difficulty in the fiber preparation process is increased. And the method adopts a single furnace tube growth mode, which is not beneficial to the large-scale preparation of the carbon nano tube fiber. A doctor thesis of von Jianmin at Tianjin university in 2012, namely safe vapor phase method for preparing carbon nanotube fibers, relates to a device for preparing carbon nanotube fibers in an argon atmosphere, wherein a sealed water tank is connected below a quartz tube through a flange, and a motor is arranged on the side wall of the water tank to drive a spinning shaft to rotate so as to collect the carbon nanotube fibers. The method also adopts a water-sealed single furnace tube preparation mode, and cannot meet the large-scale preparation requirement of the carbon nanotube fiber. The articles "High-Strength Carbon Nanotube Film from improvement Alignment and degradation" and "High-Strength Carbon Nanotube fiber-like Carbon Nanotube Film with High reduction and High electrical reduction" of the professor of the university of eastern science and technology, relate to a hydrogen-free Carbon Nanotube Film and fiber preparation device, and the method is characterized in that inert gas is used as carrier gas, and the end of a growth chamber is in an open atmosphere environment. Although the process method has the advantage of convenient operation, the liquid carbon source and the pyrolysis product thereof have flammability in the process, and the temperature of the furnace tube opening is high, so that the process method has flammability risk and is not beneficial to process amplification and large-scale preparation.
In summary, the prior art mainly has the following disadvantages:
(1) the existing carbon nanotube fiber preparation device adopts a single tube growth mode, has low fiber productivity and high energy consumption and fiber preparation cost, and is very not beneficial to the large-scale preparation of carbon nanotube fibers.
(2) The existing device for growing carbon nano tube fiber in safe atmosphere adopts a water-sealed structure for a growth chamber in order to improve the safety of the preparation process, has the defect of inconvenient operation and is not beneficial to the large-scale preparation of the carbon nano fiber.
(3) In the existing device for growing the carbon nanotube fiber in the safe atmosphere, in order to increase the operation convenience of the preparation process, the tail end of a growth chamber is positioned in an open atmospheric environment, but a pyrolysis product of the fiber preparation process still has certain flammability, and potential safety hazards exist in the large-scale amplification process.
Disclosure of Invention
The invention mainly aims to provide a system and a method for preparing carbon nanotube fibers in a large scale in a safe atmosphere so as to overcome the defects in the prior art.
In order to achieve the above object, the embodiment of the present invention adopts a technical solution comprising:
the embodiment of the invention provides a system for preparing carbon nanotube fibers in a large scale in a safe atmosphere, which comprises a carbon nanotube fiber growth unit and a carbon nanotube fiber collection unit, wherein the carbon nanotube fiber growth unit is also matched with a carbon source injection unit and an airflow control unit, the carbon nanotube fiber growth unit comprises a plurality of growth chambers which are separated from each other, a water cooling mechanism and an air sealing mechanism are arranged at the outlets of the growth chambers, the air sealing mechanism is at least used for spraying airflow to the areas corresponding to the outlets of the growth chambers to form air sealing layers, the air sealing layers can prevent ambient air from entering the growth chambers from the outlets of the growth chambers, and the water cooling mechanism is at least used for cooling the areas corresponding to the outlets of the growth chambers.
Furthermore, the carbon nanotube fiber growth unit comprises a plurality of furnace tubes, wherein each furnace tube is distributed with one growth chamber.
Furthermore, the air sealing mechanism comprises a cylindrical structure which is connected with the outlet of the growth chamber in a surrounding and sealing mode, a plurality of air flow injection holes are distributed in the wall of the cylindrical structure, and air flow injected by each air flow injection hole points to the corresponding area of the outlet of the furnace tube.
Further, the water cooling mechanism comprises a water cooling chamber at least surrounding the area corresponding to the outlet of the growth chamber.
Furthermore, more than one gas chamber is arranged in the cylinder wall of the cylindrical structure, the gas chamber is communicated with more than one gas jet hole arranged on the inner wall surface of the cylinder wall, and the gas chamber is also communicated with a high-pressure gas inlet arranged on the outer wall surface of the cylinder wall.
Furthermore, a continuous annular gas chamber is formed in the wall of the cylindrical structure, and the annular gas chamber is communicated with a plurality of gas flow injection holes uniformly distributed on the inner wall surface of the wall and is also communicated with more than one high-pressure gas inlet arranged on the outer wall surface of the wall.
Further, the water-cooling chamber is arranged around the air sealing mechanism and communicated with a cooling water circulating device.
Furthermore, the air sealing mechanism and the water cooling mechanism are coaxially arranged with the growth chamber; and/or the air sealing mechanism and the water cooling mechanism are integrally arranged.
Furthermore, a gas-collecting hood is further arranged at the outlet of the growth chamber, and the corresponding area of the outlet of the growth chamber is enclosed in the gas-collecting hood.
Furthermore, one end face of the gas-collecting hood, which is opposite to the outlet of the growth chamber, is provided with a hollow structure.
The embodiment of the invention also provides a method for preparing the carbon nano tube fiber in a large scale in a safe atmosphere, which comprises the following steps:
providing a system for preparing the carbon nanotube fiber in a large scale in the safe atmosphere;
injecting a carbon source and an auxiliary agent into each growth chamber of the carbon nanotube fiber growth unit through a carbon source injection unit under the action of carrier gas to react, and assembling in a gas phase to generate carbon nanotube fibers;
and (3) winding the formed carbon nanotube fiber by a carbon nanotube fiber collecting unit.
Further, the carbon source comprises one or more than two of ethanol/ferrocene/thiophene mixed solution, acetone/ferrocene/thiophene mixed solution or ethanol/acetone/ferrocene/thiophene mixed solution.
Further, the injection rate of the carbon source is 5-50 ml/h;
further, the carrier gas includes one or more of argon, nitrogen, and helium.
Further, the flow rate of the carrier gas in each growth chamber is 1-10L/min.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the system and the method for preparing the carbon nanotube fibers in a large scale in a safe atmosphere, a multi-tube growth chamber structure is adopted, so that simultaneous preparation and collection of multiple paths of carbon nanotube fibers can be realized, the preparation capacity of the carbon nanotube fibers is greatly improved, and the preparation cost is reduced; meanwhile, a water cooling and air sealing mechanism is arranged at the outlet position of each chamber of the carbon nanotube fiber growth unit, so that the reaction tail gas can be effectively prevented from being combusted or deflagrated at the outlet position due to high temperature, and the process safety is improved.
(2) According to the system and the method for preparing the carbon nanotube fiber in a large scale in the safe atmosphere, the safe atmosphere growth process is adopted, the multi-tube growth chamber is provided with the single-sided hollow operation surface, the fiber collection can be directly carried out in the open atmosphere environment, and the operation is simple.
(3) The invention relates to a system and a method for preparing carbon nanotube fibers in a large scale in a safe atmosphere, wherein a water cooling and air sealing mechanism adopts a cylinder structure unit, air outlet holes are dispersedly arranged on the inner side wall of the cylinder structure, nitrogen or argon is provided through a gas pipeline, gas is circularly dispersed by an internal gas interlayer, and is uniformly sprayed into the cylinder structure through the air outlet holes, so that the functions of air sealing and tail gas dilution at the mouth of a furnace pipe are realized; the cylinder structure unit is internally provided with a cooling water interlayer, and the furnace pipe opening is cooled by cooling water conveyed by a cooling water pipeline, so that combustion or deflagration caused by high temperature at the position of the furnace pipe opening in the technical process is prevented.
(4) The invention relates to a system and a method for preparing carbon nanotube fibers in a large scale in a safe atmosphere, wherein one surface of a gas-collecting hood, which is opposite to an outlet of a growth chamber, is a hollowed surface, an exhaust fan is arranged on the side surface of the gas-collecting hood, the gas-collecting hood plays a role in preventing reaction tail gas from diffusing, and the exhaust fan exhausts a carbon nanotube fiber growth unit; and the hollow surface of the gas-collecting hood is an operation surface at the same time, the carbon nanotube fiber precursor can be directly drawn out through the hollow surface, and the carbon nanotube fiber collection operation is carried out in an open atmospheric environment.
(5) The invention relates to a system and a method for preparing carbon nanotube fibers in a large scale in a safe atmosphere, wherein a carbon nanotube fiber collecting unit comprises a water tank and a fiber collecting roller which is matched with the water tank and arranged at the outer side of the water tank, a carbon nanotube fiber precursor growing in a multi-tube growth chamber contracts and fiberizes under the action of liquid in the water tank after leaving the multi-tube growth chamber under the action of carrier gas, and the fiber collecting roller is further used for winding and collecting to finish simultaneous collection of multiple rolls of carbon nanotube fibers.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a block diagram of an apparatus for mass production of carbon nanotube fibers in a safe atmosphere according to an embodiment of the present invention.
Fig. 2 is an enlarged schematic structural view of the water cooling and air sealing mechanism in fig. 1.
Fig. 3 is a diagram of a sample carbon nanotube fiber prepared in one embodiment of the present application.
Description of reference numerals: 1. the device comprises a carbon source injection unit, a carbon nanotube fiber growth unit, a carbon nanotube fiber injection flange, an electric heating furnace, a water cooling and air sealing mechanism, a gas collecting cover, a gas collecting chamber, a gas exhausting fan, a gas exhausting hole 307, a gas exhausting hole 308, a gas chamber 309, a water cooling chamber, a carbon nanotube fiber collection unit 401, a water tank, a fiber collection roller 402, a carbon nanotube fiber collection roller 403, carbon nanotube fibers, and a carbon nanotube fiber sample 5.
Detailed Description
The present invention will be more fully understood from the following detailed description, which should be read in conjunction with the accompanying drawings. Detailed embodiments of the present invention are disclosed herein; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention, which can be embodied in various forms. Therefore, specific functional details disclosed herein are not to be interpreted as limiting, but merely as a basis for the claims and as a representative basis for teaching one skilled in the art to variously employ the present invention in virtually any appropriately detailed embodiment.
In view of the defects of the prior art, the inventor of the present invention provides the technical scheme of the present invention through long-term research and a great deal of practice, and the technical scheme is mainly based on the carbon nanotube fiber preparation process under the safe atmosphere, and adopts a multi-tube growth chamber to improve the fiber yield and reduce the fiber cost; the growth chamber is in an open atmospheric environment, so that the operation convenience is improved; and a water cooling and air sealing device is arranged at the outlet position of each furnace tube of the multi-tube growth chamber, so that the process safety in the large-scale preparation process is improved. The technical solution, its implementation and principles will be further explained as follows.
One aspect of the embodiment of the invention provides a system for preparing carbon nanotube fibers in a large scale in a safe atmosphere, which comprises a carbon nanotube fiber growth unit and a carbon nanotube fiber collection unit, wherein the carbon nanotube fiber growth unit is matched with a carbon source injection unit and an airflow control unit.
In some preferred embodiments, the carbon nanotube fiber growth unit comprises a plurality of furnace tubes, wherein each furnace tube is distributed with one growth chamber.
In some preferred embodiments, the gas sealing mechanism comprises a cylindrical structure which is connected with the outlet of the growth chamber in a surrounding and sealing manner, a plurality of gas flow injection holes are distributed on the wall of the cylindrical structure, and the gas flow injected by each gas flow injection hole points to the corresponding area of the outlet of the furnace tube.
In some preferred embodiments, the water cooling mechanism comprises a water cooling chamber disposed at least around a region corresponding to the growth chamber outlet.
In some preferred embodiments, more than one gas chamber is arranged in the wall of the cylindrical structure, the gas chamber is communicated with more than one gas flow injection hole arranged on the inner wall surface of the wall, and the gas chamber is also communicated with a high-pressure gas inlet arranged on the outer wall surface of the wall.
In some more preferred embodiments, a continuous annular gas chamber is formed in the wall of the cylindrical structure, and the annular gas chamber is communicated with a plurality of gas flow injection holes uniformly distributed on the inner wall surface of the wall and is also communicated with more than one high-pressure gas inlet arranged on the outer wall surface of the wall.
In some more preferred embodiments, the gas jet direction of the gas jet hole intersects with the tail gas output direction of the growth chamber outlet.
In some preferred embodiments, the water-cooling chamber is arranged around the air sealing mechanism, and the water-cooling chamber is communicated with a cooling water circulating device.
In some more preferred embodiments, the gas sealing mechanism and the water cooling mechanism are arranged coaxially with the growth chamber.
In some more preferred embodiments, the air sealing mechanism is integrated with the water cooling mechanism.
In some preferred embodiments, the carbon nanotube fiber growth unit comprises 2-10 furnace tubes.
In some preferred embodiments, the furnace tube has a diameter of 25-120mm and a length of 50-200 cm.
In some preferred embodiments, the plurality of furnace tubes are arranged in parallel at equal intervals or in a rectangular shape in the heating device.
In some preferred embodiments, the furnace tube is arranged horizontally or vertically.
In some more preferred embodiments, the furnace tube may include, but is not limited to, a corundum furnace tube or a quartz furnace tube.
In some preferred embodiments, a gas-collecting hood is further arranged at the outlet of the growth chamber, and the area corresponding to the outlet of the growth chamber is enclosed in the gas-collecting hood.
In some preferred embodiments, one end face of the gas-collecting hood opposite to the outlet of the growth chamber is provided with a hollow structure,
in some more preferred embodiments, the side wall of the gas collecting hood is also provided with an exhaust fan.
In some preferred embodiments, the carbon nanotube fiber collecting unit includes a water tank and a fiber collecting roller disposed outside the water tank and cooperating with the water tank.
In some preferred embodiments, the carbon source injection unit comprises a micro-injection pump and an ultrasonic atomization device which is arranged in communication with the growth chamber, and the micro-injection pump is arranged in communication with the ultrasonic atomization device through a conduit; specifically, the carbon source injection unit adopts a micro-injection pump to inject the liquid carbon source and the auxiliary agent, and the liquid carbon source and the auxiliary agent are conveyed to the ultrasonic atomization device through the guide pipe to be atomized and enter each growth chamber of the carbon nanotube fiber growth unit under the action of carrier gas.
In some preferred embodiments, the carbon source injection unit comprises an injection pump and a heating evaporation device which is arranged in communication with the growth chamber, and the injection pump is arranged in communication with the heating evaporation device through a conduit; specifically, the carbon source injection unit adopts an injection pump to inject the liquid carbon source and the auxiliary agent, and conveys the liquid carbon source and the auxiliary agent to the heating evaporation device for gasification through a conduit, the temperature of the heating evaporation device is set within the range of 200-300 ℃, and the liquid carbon source and the auxiliary agent enter each growth chamber of the carbon nanotube fiber growth unit through a heating pipeline under the action of carrier gas.
In some preferred embodiments, the airflow control unit may include, but is not limited to, a mass flow meter; specifically, the gas flow control unit uses a mass flow meter to precisely control the flow of carrier gas into the multi-tube growth chamber.
Another aspect of the embodiments of the present invention further provides a method for large-scale preparation of carbon nanotube fibers in a safe atmosphere, including:
providing a system for preparing the carbon nanotube fiber in a large scale in the safe atmosphere;
injecting a carbon source and an auxiliary agent into each growth chamber of the carbon nanotube fiber growth unit through a carbon source injection unit under the action of carrier gas to react, and assembling in a gas phase to generate carbon nanotube fibers;
and (3) winding the formed carbon nanotube fiber by a carbon nanotube fiber collecting unit.
In some preferred embodiments, the carbon source may include one or more of an ethanol/ferrocene/thiophene mixed solution, an acetone/ferrocene/thiophene mixed solution, an ethanol/acetone/ferrocene/thiophene mixed solution, and the like, but is not limited thereto.
In some preferred embodiments, the injection rate of the carbon source is 5-50 ml/h.
In some preferred embodiments, the carrier gas may include one or more of argon, nitrogen, helium, and the like, but is not limited thereto.
In some preferred embodiments, the flow rate of the carrier gas in each growth chamber is 1-10L/min.
In some preferred embodiments, the temperature of the carbon nanotube fiber growth unit is 1000-.
In some preferred embodiments, the collection rate of the carbon nanotube fiber collection unit is 3 to 30 m/min.
In some more specific embodiments, the system and the method for preparing carbon nanotube fibers in a large scale in a safe atmosphere provided by the invention specifically include the following steps:
(1) the device comprises a carbon source injection unit, an air flow control unit, a carbon nanotube fiber growth unit and a carbon nanotube fiber collection unit.
(2) The carbon source injection unit adopts a micro-injection pump to inject liquid carbon source and auxiliary agent, and the liquid carbon source and the auxiliary agent are conveyed to the ultrasonic atomization device through a guide pipe to be atomized and enter the multi-pipe growth chamber under the action of carrier gas; the carbon source injection unit can also adopt an injection pump to inject the liquid carbon source and the auxiliary agent, and the liquid carbon source and the auxiliary agent are conveyed to the heating evaporation device through the guide pipe to be gasified, the temperature of the heating evaporation device is set to be within the range of 200-300 ℃, and the liquid carbon source and the auxiliary agent enter the multi-pipe growth chamber through the heating pipeline under the action of the carrier gas. The carbon source injection of the growth chamber of the carbon nanotube fiber growth unit is controlled individually.
(3) The airflow control unit adopts a mass flow meter to accurately control the flow of carrier gas entering a growth chamber of the carbon nano tube fiber growth unit, the airflow in the multi-tube growth chamber is independently controlled, and the flow range of the carrier gas in each furnace tube is 1-10L/min.
(4) The carbon nanotube fiber growth unit mainly comprises a flange, a furnace tube, an electric heating furnace, a water cooling and air sealing mechanism, a gas collecting hood and an exhaust fan.
Each growth chamber adopts an independent furnace tube made of corundum or quartz, the diameter of each furnace tube is 25-120mm, the length is 50-200cm, the number is 2-10, the furnace tubes penetrate through the electric heating furnace in a penetrating mode, the temperature of the electric heating furnace is set to 1000-1400 ℃, a plurality of furnace tubes are arranged in parallel at equal intervals or in a rectangular mode in the electric heating furnace, and the furnace tubes are horizontally arranged or vertically arranged.
The water cooling and air sealing mechanism is mainly used for reducing the temperature of the mouth of the reaction furnace and preventing ambient air from entering the reaction furnace tube. Each reaction furnace pipe opening adopts a cooling and gas sealing cylinder structure unit with the same structure. The cooling and gas seal cylinder structure unit inside wall distributed arrangement has the venthole, provides nitrogen gas or argon gas through gas pipeline, and gas is surrounded the dispersion by inside gas intermediate layer, through even spraying to cylinder structure inside of venthole, realizes furnace mouth of pipe gas seal and tail gas dilution function. The cooling and air-sealing cylinder structure unit is internally provided with a cooling water interlayer, and the furnace tube opening is cooled by cooling water conveyed by a cooling water pipeline, so that combustion or deflagration caused by high temperature at the furnace tube opening position in the technical process is prevented.
The gas-collecting hood is a square outer cover, the cage hood tail gas water-cooling and gas-sealing mechanism, one surface of the gas-collecting hood, which is opposite to the outlet of the furnace tube, is a hollow surface, and the side surface of the gas-collecting hood is provided with an exhaust fan. The gas-collecting hood plays the purpose of preventing the reaction tail gas from diffusing, and discharges the carbon nanotube fiber growth unit through the exhaust fan. The hollow surface of the gas-collecting hood is an operation surface at the same time, and the carbon nanotube fiber precursor can be directly drawn out through the hollow surface, so that the carbon nanotube fiber collection operation can be carried out in an open atmospheric environment.
(5) The carbon nanotube fiber collecting unit includes a water tank and a fiber collecting drum. After the carbon nanotube fiber precursor growing in the multi-tube growth chamber leaves the multi-tube growth chamber under the action of carrier gas, the carbon nanotube fiber precursor shrinks and fiberizes under the action of liquid in the water tank, and a fiber collecting roller is further used for winding and collecting, so that the simultaneous collection of multiple rolls of carbon nanotube fibers is completed.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
Examples
Referring to fig. 1, the apparatus for preparing carbon nanotube fibers in a large scale in a safe atmosphere according to the embodiment of the present invention includes a carbon source injection unit 1, an airflow control unit 2, a carbon nanotube fiber growth unit 3, and a carbon nanotube fiber collection unit 4, wherein the carbon nanotube fiber growth unit 3 includes an electric heating furnace 303 and 2 to 10 furnace tubes 302 penetrating through the electric heating furnace 303, and a plurality of the furnace tubes 302 are arranged in parallel or in a rectangular shape at equal intervals in the electric heating furnace 303, each of the furnace tubes 302 has a diameter of 25 to 120mm and a length of 50 to 200cm, wherein the furnace tubes 302 are arranged horizontally, the furnace tubes 302 may be corundum furnace tubes or quartz furnace tubes, an injection flange 301 is provided at an inlet of each growth furnace tube 302, and each injection flange 301 is further communicated and matched with the carbon source injection unit 1 and the airflow control unit 2.
Wherein, a growth chamber is distributed in each furnace tube 302, a water-cooling and air-sealing mechanism 304 is arranged at the outlet of the growth chamber, the air-sealing mechanism is at least used for spraying airflow to the area corresponding to the outlet of the growth chamber to form an air-sealing layer, the air-sealing layer can prevent ambient air from entering the growth chamber from the outlet of the growth chamber, and the water-cooling mechanism is at least used for cooling the area corresponding to the outlet of the growth chamber; in a specific implementation process, as shown in fig. 2, the gas sealing mechanism includes a cylindrical structure which is connected with the outlet of the growth chamber in a surrounding and sealing manner, a plurality of gas injection holes 307 are distributed on the cylindrical wall of the cylindrical structure, gas flow injected from each gas injection hole 307 points to a corresponding area of the outlet of the furnace tube 302, and the water cooling mechanism includes a water cooling chamber 309 which is at least arranged around the corresponding area of the outlet of the growth chamber; more than one gas chamber 308 is arranged in the wall of the cylindrical structure, so that a continuous annular gas chamber 308 is formed in the wall of the cylindrical structure, and the annular gas chamber 308 is communicated with a plurality of gas flow injection holes 307 uniformly distributed on the inner wall surface of the wall of the cylindrical structure and is also communicated with more than one high-pressure gas inlet arranged on the outer wall surface of the cylindrical wall.
In this embodiment, the airflow injection direction of the airflow injection hole 307 intersects with the tail gas output direction of the outlet of the growth chamber, the water-cooling chamber 309 is disposed around the air sealing mechanism, and the water-cooling chamber 309 is communicated with the cooling water circulation device.
In this embodiment, the carbon source injection unit 1 may use a micro injection pump to inject the liquid carbon source and the auxiliary agent, and the liquid carbon source and the auxiliary agent are transported to the ultrasonic atomization device through a conduit to be atomized and enter each growth furnace tube 302 of the carbon nanotube fiber growth unit under the action of the carrier gas; the carbon source injection unit 1 can also adopt an injection pump to inject liquid carbon source and auxiliary agent, and convey the liquid carbon source and auxiliary agent to the heating evaporation device for gasification through a conduit, wherein the temperature setting range of the heating evaporation device is between 200 and 300 ℃, and the liquid carbon source and auxiliary agent enter each growth furnace tube 302 of the carbon nanotube fiber growth unit through a heating pipeline under the action of carrier gas; the gas flow control unit 2 precisely controls the flow of the carrier gas entering each growth furnace tube 302 of the carbon nanotube fiber growth unit by using a mass flow meter.
The outlet of the growth chamber is also provided with a square gas-collecting hood 305 in a matching way, the corresponding area of the outlet of the growth chamber is surrounded in the gas-collecting hood 305, one end surface of the gas-collecting hood 305 opposite to the outlet of the growth chamber is provided with a hollow structure, the side wall of the gas-collecting hood 305 is also provided with an exhaust fan 306, the gas-collecting hood 305 plays a role in preventing the diffusion of reaction tail gas, and the carbon nanotube fiber growth unit 3 is exhausted through the exhaust fan 306; the carbon nanotube fiber collection unit 4 is disposed at one end of the outlet of the furnace tube 302 in a matching manner, and the carbon nanotube fiber collection unit 4 includes a water tank 401 and a fiber collection roller 402 disposed outside the water tank 401 in a matching manner.
The method for preparing the carbon nanotube fiber in a large scale in a safe atmosphere based on the preparation device provided by the embodiment of the invention specifically comprises the following steps:
(1) the carbon source injection unit 1 adopts a micro-injection pump to inject ethanol/ferrocene/thiophene mixed solution (acetone/ferrocene/thiophene mixed solution or ethanol/acetone/ferrocene/thiophene mixed solution) and an auxiliary agent, and conveys the solution to an ultrasonic atomization device through a conduit for atomization, and the solution enters each furnace tube 302 of the carbon nanotube fiber growth unit 3 under the action of carrier gas (one or more of argon, nitrogen, helium and the like), and the flow range of the carrier gas in each furnace tube 302 is 1-10L/min;
(2) the furnace temperature of the electric heating furnace 303 is set to be 1000-;
(3) after the carbon nanotube fiber sample 5 growing in the growth furnace tube 302 leaves the growth furnace tube 302 under the action of the carrier gas, the carbon nanotube fiber sample shrinks and fiberizes under the action of the liquid in the water tank 401, and further the fiber collection roller 402 is used for winding and collecting, so that simultaneous collection of a plurality of rolls of carbon nanotube fibers 403 is completed.
In addition, the inventors of the present invention have also made experiments with other materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
While the invention has been described with reference to illustrative embodiments, it will be understood by those skilled in the art that various other changes, omissions and/or additions may be made and substantial equivalents may be substituted for elements thereof without departing from the spirit and scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed for carrying out this invention, but that the invention will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. The utility model provides a system for safe atmosphere scale preparation carbon nanotube fibre, includes carbon nanotube fibre growth unit and carbon nanotube fibre collection unit, carbon nanotube fibre growth unit still pours into unit and air current control unit cooperation into with the carbon source, its characterized in that, carbon nanotube fibre growth unit is including a plurality of growth chambers of mutual separation, the exit of growth chamber is provided with water-cooling mechanism and atmoseal mechanism, atmoseal mechanism is used for at least to correspond regional injection air current in order to form the atmoseal to the chamber export that grows, the atmoseal can prevent that ambient air from growing the chamber export and getting into the chamber that grows, water-cooling mechanism is used for cooling to the chamber export that grows corresponds the region at least.
2. The system for preparing the carbon nanotube fiber in a large scale in the safe atmosphere according to claim 1, wherein: the carbon nano tube fiber growth unit comprises a plurality of furnace tubes, wherein each furnace tube is internally distributed with one growth chamber; and/or the air sealing mechanism comprises a cylindrical structure which is connected with the outlet of the growth chamber in a surrounding and sealing manner, a plurality of air flow injection holes are distributed on the wall of the cylindrical structure, and air flow injected by each air flow injection hole points to the corresponding area of the outlet of the furnace tube; and/or the water cooling mechanism comprises a water cooling chamber at least surrounding the area corresponding to the outlet of the growth chamber.
3. The system for preparing the carbon nanotube fiber in a large scale in the safe atmosphere according to claim 2, wherein: the cylinder wall of the cylindrical structure is internally provided with more than one gas chamber, the gas chamber is communicated with more than one gas jet hole arranged on the inner wall surface of the cylinder wall, and the gas chamber is also communicated with a high-pressure gas inlet arranged on the outer wall surface of the cylinder wall.
4. The system for preparing the carbon nanotube fiber in a large scale in the safe atmosphere according to claim 3, wherein: a continuous annular gas chamber is formed in the wall of the cylindrical structure, and is communicated with a plurality of gas flow injection holes uniformly distributed on the inner wall surface of the wall of the cylindrical structure and more than one high-pressure gas inlet arranged on the outer wall surface of the cylindrical wall; and/or the gas jet direction of the gas jet hole is crossed with the tail gas output direction of the growth chamber outlet.
5. The system for preparing the carbon nanotube fiber in a large scale in the safe atmosphere according to claim 2, wherein: the water-cooling cavity is arranged around the air sealing mechanism and is communicated with a cooling water circulating device; and/or the air sealing mechanism and the water cooling mechanism are coaxially arranged with the growth chamber; and/or the air sealing mechanism and the water cooling mechanism are integrally arranged.
6. The system for preparing the carbon nanotube fiber in a large scale in the safe atmosphere according to claim 2, wherein: the carbon nano tube fiber growth unit comprises 2-10 furnace tubes; and/or the diameter of the furnace tube is 25-120mm, and the length of the furnace tube is 50-200 cm; and/or the plurality of furnace tubes are arranged in parallel at equal intervals or are arranged in the heating device in a rectangular shape; and/or the furnace tube is horizontally or vertically arranged; and/or the furnace tube comprises a corundum furnace tube or a quartz furnace tube.
7. The system for preparing the carbon nanotube fiber in a large scale in the safe atmosphere according to claim 1, wherein: the outlet of the growth chamber is also provided with a gas-collecting hood, and the area corresponding to the outlet of the growth chamber is surrounded in the gas-collecting hood;
and/or one end surface of the gas-collecting hood opposite to the outlet of the growth chamber is provided with a hollow structure; and/or an exhaust fan is also arranged on the side wall of the gas collecting hood.
8. The system for preparing the carbon nanotube fiber in a large scale in the safe atmosphere according to claim 1, wherein: the carbon nano tube fiber collecting unit comprises a water tank and a fiber collecting roller which is matched with the water tank and is arranged outside the water tank;
and/or the carbon source injection unit comprises a micro-injection pump and an ultrasonic atomization device communicated with the growth chamber, and the micro-injection pump is communicated with the ultrasonic atomization device through a conduit; and/or the carbon source injection unit comprises an injection pump and a heating evaporation device communicated with the growth chamber, and the injection pump is communicated with the heating evaporation device through a conduit;
and/or the gas flow control unit comprises a mass flow meter.
9. A method for preparing carbon nanotube fibers in a large scale in a safe atmosphere is characterized by comprising the following steps:
providing a safe atmosphere scale-up carbon nanotube fiber production system according to any one of claims 1-8;
injecting a carbon source and an auxiliary agent into each growth chamber of the carbon nanotube fiber growth unit through a carbon source injection unit under the action of carrier gas to react, and assembling in a gas phase to generate carbon nanotube fibers;
and (3) winding the formed carbon nanotube fiber by a carbon nanotube fiber collecting unit.
10. The method for preparing carbon nanotube fibers in a large scale in a safe atmosphere according to claim 9, wherein the method comprises the following steps: the carbon source comprises one or more than two of ethanol/ferrocene/thiophene mixed solution, acetone/ferrocene/thiophene mixed solution or ethanol/acetone/ferrocene/thiophene mixed solution, and/or the injection rate of the carbon source is 5-50 ml/h;
and/or the carrier gas comprises one or more of argon, nitrogen and helium, and/or the flow of the carrier gas in each growth chamber is 1-10L/min;
and/or the temperature of the carbon nano tube fiber growth unit is 1000-1400 ℃; and/or the collection speed of the carbon nano tube fiber collection unit is 3-30 m/min.
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| JP2003201630A (en) * | 2001-12-26 | 2003-07-18 | Nikkiso Co Ltd | Method for post-treating carbon nanofiber and method for producing graphitized carbon nanofiber |
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| WO2015082936A1 (en) * | 2013-12-05 | 2015-06-11 | Q-Flo Limited | Process and apparatus for the production of carbon nanotubes |
| CN110685039A (en) * | 2019-10-08 | 2020-01-14 | 常州大学 | Method for producing carbon nano tube fibers in batch |
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|---|---|---|---|---|
| JP2003201630A (en) * | 2001-12-26 | 2003-07-18 | Nikkiso Co Ltd | Method for post-treating carbon nanofiber and method for producing graphitized carbon nanofiber |
| JP2006290698A (en) * | 2005-04-14 | 2006-10-26 | Yamaguchi Univ | Method of manufacturing carbon nanofiber |
| WO2015082936A1 (en) * | 2013-12-05 | 2015-06-11 | Q-Flo Limited | Process and apparatus for the production of carbon nanotubes |
| CN110685039A (en) * | 2019-10-08 | 2020-01-14 | 常州大学 | Method for producing carbon nano tube fibers in batch |
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