CN111020747B - System and method for continuously preparing carbon nanotube fibers based on floating catalytic CVD method - Google Patents
System and method for continuously preparing carbon nanotube fibers based on floating catalytic CVD method Download PDFInfo
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Abstract
The invention discloses a system and a method for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method. The system includes gasification sampling device, synthetic reaction device and fibre and convolutes collection device, wherein, gasification sampling device includes gasification cavity and first heating device, first heating device is used for heating the gasification cavity, the gasification cavity has carbon source injection mouth and first carrier gas input port. The system provided by the invention can gasify the liquid carbon source/catalyst into gas in advance, and can accurately control the supply speed of the liquid carbon source/catalyst, the gasification temperature, the flow rate of the carrier gas and the temperature of the conveying pipeline, so that the gaseous carbon source/catalyst and the carrier gas are fully and uniformly mixed before entering the reaction zone of the synthesis reaction device, thereby providing the gaseous carbon source supply with accurately controllable speed, uniformity, stability and continuity for the growth of the carbon nano tube in the next step, and further realizing the continuous preparation of uniform carbon nano tube fibers.
Description
Technical Field
The invention relates to a system for preparing carbon nanotube fibers, in particular to a system and a method for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method, and belongs to the technical field of fiber synthesis.
Background
The floating catalytic CVD method is one of the most important methods for continuously preparing carbon nanotube fibers, and mainly comprises a carbon source/catalyst continuous supply system, a high-temperature reaction furnace body and a carbon nanotube fiber continuous collection system. Among these, the continuous carbon source/catalyst supply system has a critical influence on the quality of the carbon nanotube fiber product.
In the prior art, a liquid carbon source/catalyst supply device for preparing carbon nanotube fibers based on a floating catalytic CVD method mainly comprises two types: 1) directly injecting a liquid carbon source/catalyst solution into one end of a high-temperature growth furnace, and gasifying through the heat radiation of a growth area; 2) the liquid carbon source/catalyst solution can be atomized into micrometer-scale liquid drops, and the liquid drops are subjected to heat radiation of a growth area to complete the gasification process; however, if the liquid carbon source/catalyst solution is directly injected into one end of the high temperature growth furnace, the liquid carbon source/catalyst is dropwise added into the high temperature region for evaporation, and the evaporation process of the liquid drops is not continuous and uniform, so that the supply of the carbon source and the catalyst is not uniform and continuous; in addition, when the ultrasonic atomization assisted sample introduction is adopted, the liquid carbon source/catalyst is firstly atomized into micron droplets by the ultrasonic atomization device and then enters a high-temperature region for gasification, bubbles are easily formed in liquid due to the heating effect of ultrasonic waves in the ultrasonic atomization process, and particularly common low-boiling-point carbon sources such as ethanol and acetone can cause intermittent pause in the ultrasonic atomization process, so that the supply of the carbon source and the catalyst is unstable, and finally the continuity and the uniformity of the prepared carbon nanotube fiber can be influenced.
Disclosure of Invention
The invention mainly aims to provide a system and a method for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method, so as to overcome the defects in the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a system for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method, which comprises a gasification sample injection device, a synthesis reaction device and a fiber winding and collecting device, wherein the gasification sample injection device comprises a gasification chamber and a first heating device, the first heating device is used for heating the gasification chamber, the gasification chamber is provided with a carbon source injection port and a first carrier gas input port, a liquid carbon source/catalyst injected through the carbon source injection port can be heated and gasified into a gaseous state in the gasification chamber, and the gaseous carbon source/catalyst and a first carrier gas input through the first carrier gas input port are mixed in the gasification chamber to form a mixed reaction gas for synthesizing a carbon nanotube fiber precursor.
Furthermore, the gasification chamber is connected with the synthesis reaction device through a conveying pipeline, the conveying pipeline is further connected with a second heating device, and the second heating device is at least used for heating the conveying pipeline and enabling mixed reaction gas in the conveying pipeline to be kept in a gas state all the time.
Further, the carbon source injection port is also connected with an ultrasonic atomizer, and the ultrasonic atomizer is used for atomizing the liquid carbon source/catalyst and then inputting the atomized liquid carbon source/catalyst into the gasification chamber.
Further, the first carrier gas input port is also connected with a flow controller.
Further, the synthesis reaction device comprises a high-temperature tube furnace.
Furthermore, a second carrier gas inlet is arranged on the high-temperature tube furnace.
Furthermore, the system for continuously preparing the carbon nanotube fiber based on the floating catalytic CVD method further comprises a water sealing device, wherein the water sealing device is arranged between the synthesis reaction device and the fiber winding and collecting device and is in sealing fit with the synthesis reaction device, and the water sealing device is at least used for performing densification treatment on a synthesized carbon nanotube fiber precursor.
Further, water seal arrangement includes water seal tank and with water seal tank complex tail gas collection mechanism.
The embodiment of the invention also provides a method for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method, which comprises the following steps: firstly gasifying the liquid carbon source/catalyst into a gas state, mixing the gas carbon source/catalyst with carrier gas to form mixed reaction gas, conveying the mixed reaction gas to a synthesis reaction device for synthesis reaction to form a carbon nano tube fiber precursor, and then fiberizing and collecting the carbon nano tube fiber precursor through a fiber winding and collecting device.
Further, the method specifically comprises:
1) providing the device for continuously preparing the carbon nanotube fibers based on the floating catalytic CVD method;
2) firstly, injecting a liquid carbon source/catalyst into an ultrasonic atomizer according to a preset flow rate, atomizing the liquid carbon source/catalyst by the ultrasonic atomizer, inputting the atomized liquid carbon source/catalyst into a gasification chamber, and heating the gasification chamber by a first heating device to gasify the atomized liquid carbon source/catalyst into a gas state; simultaneously, inputting a first carrier gas into the gasification chamber through a first carrier gas input port, and uniformly mixing the gaseous carbon source/catalyst and the first carrier gas in the gasification chamber to form mixed reaction gas;
3) the mixed reaction gas is conveyed into the synthesis reaction device through a conveying pipeline to be mixed with a second carrier gas and react to form a carbon nano tube fiber precursor;
4) and performing fiberization treatment on the carbon nanotube fiber precursor by a fiber winding and collecting device to form the carbon nanotube fiber.
Compared with the prior art, the system for continuously preparing the carbon nanotube fiber based on the floating catalytic CVD method can improve the uniformity of the carbon nanotube fiber prepared by the floating catalytic CVD method, can gasify a liquid carbon source/catalyst into a gas state in advance, and can accurately control the supply speed of the liquid carbon source/catalyst, the gasification temperature, the flow rate of carrier gas and the temperature of a conveying pipeline, so that the gaseous carbon source/catalyst and the carrier gas are fully and uniformly mixed before entering a reaction zone of a synthesis reaction device, thereby providing the gaseous carbon source supply with accurately controllable, uniform, stable and continuous speed for the growth of the carbon nanotube in the next step, and further realizing the continuous preparation of the uniform carbon nanotube fiber.
Drawings
FIG. 1 is a schematic structural diagram of a system for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method according to an exemplary embodiment of the present invention;
FIG. 2 is a photograph of a carbon nanotube cylindrical intermediate grown from the system of FIG. 1;
FIG. 3a is an SEM image of the surface of a carbon nanotube fiber grown from the system of FIG. 1;
FIG. 3b is an SEM image of the interior of a carbon nanotube fiber grown from the system of FIG. 1;
fig. 4 is a photomicrograph of carbon nanotube fibers grown from the system of fig. 1.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
According to the system for continuously preparing the carbon nanotube fibers based on the floating catalytic CVD method, provided by the embodiment of the invention, the liquid carbon source/catalyst is evaporated and gasified by adopting the heating and gasifying system independent of the high-temperature growth area, is uniformly mixed with the carrier gas, and is conveyed into the high-temperature growth area through the temperature-controllable pipeline, so that the stable and continuous supply of the carbon source and the catalyst and the continuous preparation of the high-uniformity carbon nanotube fibers are realized.
The embodiment of the invention provides a system for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method, which comprises a gasification sample injection device, a synthesis reaction device and a fiber winding and collecting device, wherein the gasification sample injection device comprises a gasification chamber and a first heating device, the first heating device is used for heating the gasification chamber, the gasification chamber is provided with a carbon source injection port and a first carrier gas input port, a liquid carbon source/catalyst injected through the carbon source injection port can be heated and gasified into a gaseous state in the gasification chamber, and the gaseous carbon source/catalyst and the first carrier gas input through the first carrier gas input port are mixed in the gasification chamber to form a mixed reaction gas for synthesizing a carbon nanotube fiber precursor.
The technical solution, the implementation process and the principle thereof will be further explained with reference to the drawings.
Referring to fig. 1, a system for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method according to an exemplary embodiment of the present invention includes a gasification sample injection device, a synthesis reaction device, a water seal device, and a fiber winding and collecting device, wherein the gasification sample injection device is at least used for gasifying a liquid carbon source/catalyst to form a gas phase, and pre-mixing the gaseous carbon source/catalyst with a first carrier gas to form a mixed reaction gas; the synthesis reaction device is at least used for mixing and reacting the mixed reaction gas provided by the gasification sample introduction device with a second carrier gas to form a carbon nano tube fiber precursor, and the water seal device is at least used for performing densification treatment on the synthesized carbon nano tube fiber precursor; the fiber winding and collecting device is at least used for fiberizing and collecting the densified carbon nanotube fiber precursor.
Specifically, referring to fig. 1, the gasification sample injection device includes a gasification tank 5 and a gasification tank heating jacket (i.e. the first heating device, the same below) 6, the gasification tank heating jacket 6 is used for heating the gasification tank 5, the gasification tank 5 has a carbon source injection port and a first carrier gas input port, an ultrasonic atomizer 2 is arranged at the carbon source injection port, the ultrasonic atomizer is further connected with an injection pump 1 for injecting a liquid carbon source/catalyst, and the first carrier gas input port is connected with a flow controller or a flow control valve 4; the gas outlet of the gasification tank 5 is connected to the synthesis reaction device via an output pipeline, and the output pipeline is further connected to a heating jacket (i.e. the second heating device) 7 in a heat conducting manner, wherein the heating jacket 7 is used for heating the output pipeline, so that the carbon source/catalyst in the mixed reaction gas flowing through the output pipeline is kept in a gaseous state.
Specifically, the synthesis reaction device comprises a high-temperature furnace 11 and a high-temperature reaction furnace tube 10 arranged in the high-temperature furnace, sealing flanges 9 are arranged at an inlet and an outlet of the high-temperature reaction furnace tube 10, a second carrier gas inlet is also arranged on the sealing flange 9 at the inlet, an output pipeline is communicated with the high-temperature reaction furnace tube 10 through the sealing flange 9 at the inlet, mixed reaction gas led in through the output pipeline is mixed with second carrier gas input through the second carrier gas inlet, and the mixed reaction gas is reacted in the high-temperature reaction furnace tube 10 to form a carbon nanotube fiber precursor 12.
Specifically, the water sealing device comprises a water tank 15 and a water sealing tank 13 matched with the water tank, wherein liquid such as water is contained in the water tank 15, the water sealing tank 13 is arranged in the water tank 15, and the water sealing tank 13 and the liquid level in the water tank 15 enclose to form a sealing space; the water seal box 13 is provided with an exhaust port for exhausting the tail gas 14 exhausted from the high-temperature reaction furnace tube 10.
Specifically, the fiber winding and collecting device 18 includes a collecting roller that is engaged with a roller 16 provided in the water tank 15 and is capable of drawing the carbon nanotube fiber precursor into a fiber shape, and the drawn carbon nanotube fiber is wound around the collecting roller.
Specifically, the embodiment of the invention provides a system for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method, which improves the uniformity of the carbon nanotube fibers prepared by the floating catalytic CVD method, and the specific technical process and principle are as follows:
the injection pump 1 injects the liquid carbon source/catalyst into the ultrasonic atomizer 2 according to a set flow rate, the liquid carbon source/catalyst is introduced into a gasification chamber of the gasification tank 5 after being ultrasonically atomized by the ultrasonic atomizer, the gasification tank 5 is heated to a set gasification temperature by the gasification tank heating sleeve 6, and atomized liquid carbon source/catalyst droplets are gasified into a gas state in the gasification tank;
meanwhile, the first carrier gas 3 enters the gasification tank from the first carrier gas input port at a set flow rate under the control of the flow controller 4 and is uniformly mixed with the gaseous carbon source/catalyst to form a mixed reaction gas; wherein, the gasification tank not only has the function of gasifying the liquid raw material, but also has the function of a gas mixing tank;
the uniformly mixed reaction gas is continuously and uniformly conveyed into the high-temperature reaction furnace tube 10 through a conveying pipeline, and the conveying pipeline is kept at a set temperature through a heating device 7 so as to prevent the gaseous carbon source/catalyst from being liquefied again at a lower temperature;
meanwhile, a second carrier gas 8 is introduced into the high-temperature reaction furnace tube 10 through a second carrier gas inlet at a certain flow rate, and a carbon nanotube fiber precursor (or referred to as a carbon nanotube aerogel product) 12 is generated after reaction processes such as cracking, catalytic growth and the like of a gaseous carbon source/catalyst occur in a high-temperature reaction zone in the high-temperature reaction furnace tube 10;
the carbon nanotube fiber precursor synthesized in the high-temperature reaction furnace tube 10 is subjected to water shrinkage densification in the water tank 15, and then is drawn to form the carbon nanotube fiber 17, and the carbon nanotube fiber 17 is finally collected by the fiber winding and collecting device 18.
Specifically, a photo of the carbon nanotube fiber precursor synthesized in the high-temperature reaction furnace tube 10 is shown in fig. 2, the carbon nanotube fiber precursor shown in fig. 2 is in a water-sealed box state, and the carbon nanotube fiber precursor is shown to be cylindrical and has a single-layer tube structure, so that the carbon nanotube fiber precursor is relatively uniform and clean, and no other impurities arranged in a mess are present in the tube. Fig. 3a is an SEM image of the surface of the carbon nanotube fiber, and fig. 3b is an SEM image of the inside of the fiber exposed after the surface portion of the carbon nanotube fiber is torn off by the tape, so that it can be seen that the carbon nanotubes constituting the carbon nanotube fiber 17 are well aligned along the axial direction of the fiber, and the fiber has less impurities, and is clean and uniform and has high degree of alignment. From fig. 4, it can be seen that the carbon nanotube fiber prepared by the system provided by the embodiment of the present invention has good uniformity in the axial direction.
The system for continuously preparing the carbon nanotube fiber based on the floating catalytic CVD method, which is provided by the embodiment of the invention, can improve the uniformity of the carbon nanotube fiber prepared by the floating catalytic CVD method, can gasify the liquid carbon source/catalyst into a gas state in advance, and can accurately control the supply speed, the gasification temperature, the flow rate of the carrier gas and the temperature of the conveying pipeline of the liquid carbon source/catalyst, so that the gaseous carbon source/catalyst and the carrier gas are fully and uniformly mixed before entering the reaction zone of the synthesis reaction device, thereby providing the gaseous carbon source supply with accurately controllable, uniform, stable and continuous speed for the growth of the carbon nanotube in the next step, and further realizing the continuous preparation of the uniform carbon nanotube fiber.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. A system for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method is characterized by comprising a gasification sample injection device, a synthesis reaction device, a water seal device and a fiber winding and collecting device, wherein the gasification sample injection device comprises a gasification chamber and a first heating device, the first heating device is used for heating the gasification chamber, the gasification chamber is provided with a carbon source injection port and a first carrier gas input port, a liquid carbon source/catalyst injected through the carbon source injection port can be heated and gasified into a gaseous state in the gasification chamber, and the gasified carbon source/catalyst and a first carrier gas input through the first carrier gas input port are mixed in the gasification chamber to form a mixed reaction gas for synthesizing a carbon nanotube fiber precursor; the water seal device is arranged between the synthesis reaction device and the fiber winding and collecting device and is in sealing fit with the synthesis reaction device, and the water seal device is at least used for performing densification treatment on a synthesized carbon nanotube fiber precursor;
and the carbon source injection port is also connected with an ultrasonic atomizer, the ultrasonic atomizer is used for atomizing a liquid carbon source/catalyst and then inputting the atomized liquid carbon source/catalyst into a gasification chamber, the gasification chamber is connected with the synthesis reaction device through a conveying pipeline, the conveying pipeline is also connected with a second heating device, and the second heating device is at least used for heating the conveying pipeline and enabling mixed reaction gas in the conveying pipeline to be always kept in a gas state.
2. The system for continuously preparing carbon nanotube fiber according to claim 1, wherein: the first carrier gas input port is also connected to a flow controller.
3. The system for continuously preparing carbon nanotube fiber according to claim 1, wherein: the synthesis reaction device comprises a high-temperature tube furnace.
4. The system for continuously preparing carbon nanotube fiber according to claim 3, wherein: and a second carrier gas inlet is also arranged on the high-temperature tube furnace.
5. The system for continuously preparing carbon nanotube fiber according to claim 1, wherein: the water sealing device comprises a water sealing box and a tail gas collecting mechanism matched with the water sealing box.
6. A method for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method is characterized by comprising the following steps: 1) Providing a system for continuously preparing carbon nanotube fibers based on a floating catalytic CVD method according to any one of claims 1 to 5;
2) firstly, injecting a liquid carbon source/catalyst containing a carbon source and a catalyst into an ultrasonic atomizer, atomizing the liquid carbon source/catalyst by the ultrasonic atomizer, inputting the atomized liquid carbon source/catalyst into a gasification chamber, and heating the gasification chamber by a first heating device to gasify the atomized liquid carbon source/catalyst into a gas state; simultaneously, inputting a first carrier gas into the gasification chamber through a first carrier gas input port, and uniformly mixing the gaseous carbon source/catalyst and the first carrier gas in the gasification chamber to form mixed reaction gas;
3) the mixed reaction gas is conveyed into the synthesis reaction device through a conveying pipeline to be mixed with a second carrier gas and react to form a carbon nano tube fiber precursor;
4) and performing fiberization treatment on the carbon nanotube fiber precursor by a fiber winding and collecting device to form the carbon nanotube fiber.
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| CN112410924B (en) * | 2020-10-27 | 2023-06-30 | 江西省纳米技术研究院 | Carbon nano tube/conductive polymer composite fiber, continuous preparation method and continuous preparation system thereof |
| CN112357908A (en) * | 2020-11-12 | 2021-02-12 | 江西铜业技术研究院有限公司 | Continuous preparation device and process for single-walled carbon nanotubes |
| CN114477143B (en) * | 2022-03-25 | 2023-09-22 | 江西省纳米技术研究院 | Reaction furnace tube of carbon nano tube material and growth device and method |
| CN114540987B (en) * | 2022-03-30 | 2023-04-18 | 江西省纳米技术研究院 | Thin-diameter carbon nanotube fiber, reaction furnace tube thereof, preparation equipment and preparation method |
| CN114808196B (en) * | 2022-04-19 | 2023-06-23 | 江西省纳米技术研究院 | Carbon nanotube preparation device, injection assembly thereof and carbon nanotube preparation method |
| CN115180614A (en) * | 2022-08-02 | 2022-10-14 | 武汉市碳翁科技有限公司 | Continuous carbon nanotube aggregate synthesis device and use method |
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| CN101613895B (en) * | 2009-06-04 | 2011-08-24 | 天津大学 | Processing method for preparing carbon nanotube fiber in inert atmosphere based on chemical vapor flow spinning method |
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