CN115215326B - Pre-oxidation device for purifying carbon nano tube - Google Patents
Pre-oxidation device for purifying carbon nano tube Download PDFInfo
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- CN115215326B CN115215326B CN202210167136.6A CN202210167136A CN115215326B CN 115215326 B CN115215326 B CN 115215326B CN 202210167136 A CN202210167136 A CN 202210167136A CN 115215326 B CN115215326 B CN 115215326B
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- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/17—Purification
Abstract
The invention discloses a preoxidation device for purifying carbon nano tubes, which comprises a gas mixing unit, a preheater, a total reactor and a tail gas treatment unit, wherein the carbon nano tubes are collected in a single modeA cell and a cooling unit; one end of the gas mixing unit is connected with a first N through a pipeline respectively 2 Intake manifold and CO 2 An intake manifold, and the other end of the gas mixing unit is connected to the preheater through a pipeline, and the preheater is connected to the total reactor through a pipeline; the total reactor is provided with a feed inlet and a discharge outlet and an exhaust outlet connected to the tail gas treatment unit; the discharge port of the total reactor is connected to the carbon nanotube collecting unit, and a cooling unit is arranged outside the carbon nanotube collecting unit. The invention mixes nitrogen and carbon dioxide, preoxidizes the carbon nano tube at high temperature to purify the carbon nano tube, has simple structure, is easy to operate, and can continuously process more materials.
Description
Technical Field
The invention relates to a pre-oxidation device for purifying carbon nanotubes, and belongs to the technical field of chemical equipment.
Background
In the production process of the carbon nano tube, metals such as iron, cobalt, nickel and the like are often used as catalysts, and oxides such as magnesium oxide, aluminum oxide, silicon oxide and the like are used as catalyst carriers. In the current production of carbon nanotubes, the catalysts mainly used include chemical vapor deposition, arc deposition, etc.; and due to the use of catalysts, the carbon nanotubes produced by these methods are often accompanied by a certain content of impurities, such as amorphous carbon, carbon nanoparticles, carbon nanospheres, catalyst particles, etc. These impurities greatly hinder the physical property research and practical application of carbon nanotubes, and thus, the purification technology of carbon nanotubes is gaining more and more attention.
The existing purification method of carbon nanotubes mainly utilizes the tiny difference between carbon nanotubes and amorphous carbon and other impurities in physical or chemical aspects to achieve the purification purpose, and the common purification method comprises the following steps: chemical oxidation, gas phase oxidation, liquid phase oxidation, and the like; the gas phase oxidation method is to introduce a trace amount of oxygen-containing gas such as carbon dioxide under the protection of inert gas, and oxidize amorphous carbon or carbon nano particles at a certain temperature so as to achieve the aim of purification.
Further, a large number of carbon nanotubes are required to be purified in the industrial production process, so that a corresponding purification device is also required to achieve the purpose of mass production.
Disclosure of Invention
In order to solve the problems existing at present, the invention provides a preoxidation device for purifying carbon nanotubes, which is characterized in that nitrogen and carbon dioxide are mixed, and the carbon nanotubes are preoxidized at high temperature to purify the carbon nanotubes.
The technical scheme of the pre-oxidation device for purifying the carbon nano tube is as follows:
a pre-oxidation device for purifying carbon nanotubes comprises a gas mixing unit, a pre-heater, a total reactor, a tail gas treatment unit, a carbon nanotube collecting unit and a cooling unit; wherein one end of the gas mixing unit is connected with a first N through a pipeline respectively 2 Intake manifold and CO 2 An intake manifold, and the other end of the gas mixing unit is connected to the preheater through a pipeline, and the preheater is connected to the total reactor through a pipeline; the total reactor is provided with a feed inlet and a discharge outlet and an exhaust outlet connected to the tail gas treatment unit; the discharge port of the total reactor is connected to the carbon nanotube collecting unit, and a cooling unit is arranged outside the carbon nanotube collecting unit.
According to the technical scheme of the invention, the first N is adopted in the gas mixing unit 2 Intake manifold and CO 2 The air inlet header pipes are respectively introduced with N according to a certain proportion 2 And CO 2 And after being mixed in the gas mixing unit, the two gases are conveyed to the preheater through a pipeline, the preheater heats the mixed gas, and the heated mixed gas is introduced into the total reactor through the pipeline for reaction.
According to the technical scheme of the invention, the total reactor is of a vertical structure, and the exhaust port is arranged at the top of the total reactor.
According to the technical scheme of the invention, the pipeline connected to the total reactor of the preheater enters the interior of the total reactor from the upper part of the total reactor and extends to the lower part of the total reactor.
According to the technical scheme of the invention, a valve is arranged on a pipeline of the preheater connected to the total reactor.
According to the technical scheme of the invention, the feed inlet of the total reactor is arranged at one side of the upper part of the total reactor and is used for feeding.
According to the technical scheme of the invention, the discharge port of the total reactor is arranged at the bottom of the total reactor, and a valve is arranged at the discharge port.
According to the technical scheme of the invention, the top of the total reactor is also provided with a closed observation window for real-time observation in the reaction process of the total reactor; in one embodiment, the number of the observation windows can be two, and the exhaust port is located between the two observation windows.
According to the technical scheme of the invention, the total reactor is also provided with a temperature sensor and a pressure sensor so as to monitor the temperature and the pressure in the total reactor.
According to an embodiment of the present invention, a pressure sensor may be provided on the gas mixing unit; and a pressure sensor and a temperature sensor can be arranged on the preheater.
According to the technical scheme of the invention, when the device works, the valve at the discharge port at the bottom of the total reactor is closed, the exhaust port is opened, the valve on the pipeline which is communicated with the total reactor in the preheater is opened, the gas in the preheater is communicated with the total reactor, and the gas is blown upwards from the bottom of the total reactor, so that the carbon nano tube entering from the feed port floats in the reactor, and is subjected to oxidation reaction, and the gas generated after the reaction is discharged from the upper part and is subjected to harmless treatment through the tail gas treatment unit.
According to the technical scheme of the invention, after the pre-oxidation treatment of the carbon nano tubes is finished, the pre-heater stops introducing gas into the total reactor, the treated carbon nano tubes in the total reactor fall to the bottom, the valve of the discharge port is opened, and the pre-heater again introduces gas into the total reactor, so that materials in the total reactor are driven by the air inlet pressure and conveyed to the carbon nano tube collecting unit through the pipeline of the discharge port.
According to the technical scheme of the invention, after the pre-oxidation treatment of the carbon nano tube is finished, the device can also adopt the method that the pre-heater is not closed to convey the gas into the total reactor, the top exhaust valve of the reactor is directly closed, the lower discharge valve is opened, the carbon nano tube powder can enter the storage tank of the carbon nano tube collecting unit under the driving of the air flow of the air inlet in the total reactor, and the powder of the carbon nano tube is transferred after the storage tank is cooled, so that the carbon nano tube collecting unit is communicated with the air, and therefore, nitrogen needs to be introduced.
According to the technical scheme of the invention, the carbon nano tube collecting unit is connected with a second N 2 An intake manifold, the second N 2 An air inlet header pipe is connected to the bottom of the carbon nano tube collecting unit and continuously introduces N into the carbon nano tube collecting unit 2 And the upper part of the carbon nano tube collecting unit is provided with an air outlet, and redundant oxygen in the carbon nano tube collecting unit is discharged from the air outlet.
In an embodiment, the cooling unit outside the carbon nanotube collecting unit may be a water-cooled pipe, and the water-cooled pipe is wrapped on the outer wall of the carbon nanotube collecting unit, so that the material in the carbon nanotube collecting unit may be rapidly cooled while being protected by introducing nitrogen.
According to the technical scheme of the invention, the pre-oxidation device mixes the gases in advance through the gas mixing unit, so that the proportion of the gases can be accurately controlled, and the gases are heated in advance through the preheater, so that the problem of slow temperature rise of the total reactor is solved, and the tail gas treatment unit is arranged to perform harmless treatment on the tail gas, so that the air pollution is reduced.
The invention has the beneficial effects that:
1. the pre-oxidation device of the invention is provided with a gas mixing unit and N is respectively arranged 2 Intake manifold and CO 2 And the air inlet manifold can accurately control the components of the mixed gas in the gas mixing unit.
2. According to the pre-oxidation device, the pre-heater is arranged to heat the reaction gas in advance, so that the temperature of the total reactor is raised faster, and the influence of the ambient temperature on the temperature in the total reactor is extremely low.
3. The pre-oxidation device provided by the invention is provided with the tail gas treatment unit, so that the tail gas generated after the reaction is subjected to harmless treatment, and the environmental pollution is reduced.
4. The pre-oxidation device can reduce the cooling time of the carbon nano tube by arranging the cooling unit on the carbon nano tube collecting unit, can perform the next process more quickly, and has high production efficiency.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic view showing the general structure of a pre-oxidizing apparatus of the present invention;
wherein 1. First N 2 Intake manifold, 2.CO 2 An air inlet header pipe, a gas mixing unit, a preheater, a total reactor, a tail gas treatment unit, a carbon nano tube collecting unit, a cooling water inlet, a cooling water outlet and a cooling water outlet, wherein the total reactor is the same as the total reactor, the tail gas treatment unit is the same as the tail gas treatment unit, the carbon nano tube collecting unit is the carbon nano tube collecting unit, the cooling water inlet is the cooling water inlet, the cooling water outlet is the cooling water outlet, and the second N is the second N 2 The main gas inlet pipe, the feed inlet, the discharge outlet and the total reactor gas inlet are respectively arranged at the two sides of the main gas inlet pipe, the feed inlet, the discharge outlet and the total reactor gas inlet; 14. and an air outlet.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the embodiments of the present invention will be described in further detail with reference to the accompanying drawings.
Embodiment one:
the embodiment provides a pre-oxidation device for purifying carbon nanotubes, which comprises a gas mixing unit 3 and a pre-heater 4A total reactor 5, a tail gas treatment unit 6, a carbon nanotube collecting unit 7 and a cooling unit; wherein the gas mixing units are respectively connected with a first N 2 Intake manifold 1 and CO 2 An intake manifold 2, and the gas mixing unit 3 is connected to a preheater 4 through a pipe, the preheater 4 is connected to a total reactor 5 through a pipe, a feed port 11 and a discharge port 12 are provided on the total reactor 5, and an exhaust port connected to an exhaust gas treatment unit 6 is provided; the discharge port 12 of the total reactor 5 is connected to the carbon nanotube collecting unit 7, and a cooling unit is provided outside the carbon nanotube collecting unit 7.
According to the technical scheme of the invention, the gas mixing unit 3 is provided with a first N 2 Intake manifold 1 and CO 2 The air inlet header pipe 2 is respectively introduced with N according to a certain proportion 2 And CO 2 And after the two gases are mixed in the gas mixing unit, the mixed gases are conveyed to the preheater 4 through a pipeline, the preheater 4 heats the mixed gases, and the heated mixed gases are introduced into the total reactor through the pipeline for reaction.
According to the present embodiment, the total reactor 5 is of a vertical structure, and an exhaust port is provided at the top of the total reactor.
According to the present embodiment, the pipe of the preheater 4 connected to the total reactor enters the interior of the total reactor 5 from the upper part of the total reactor and extends to the lower part of the total reactor, and as shown in fig. 1, the pipe ends with a total reactor inlet 13.
According to the present embodiment, the feed port 11 of the total reactor is provided at one side of the upper portion of the total reactor 5 for feeding.
According to the present embodiment, the outlet 12 of the total reactor is provided at the bottom of the total reactor, and a valve is provided at the outlet.
According to this embodiment, a closed observation window is further provided at the top of the total reactor 5, for performing real-time observation during the reaction process of the total reactor; in one embodiment, the number of the observation windows can be two, and the exhaust port is located between the two observation windows.
According to this embodiment, a temperature sensor and a pressure sensor are further disposed on the total reactor 5 to monitor the temperature and pressure in the total reactor.
According to the embodiment, when the device works, the valve at the discharge port at the bottom of the total reactor is closed, the exhaust port is opened, the valve on the pipeline which is introduced into the total reactor in the preheater is opened, the gas in the preheater is introduced into the total reactor, and the gas is blown upwards from the bottom of the total reactor, so that the carbon nano tube which enters from the feed port floats in the reactor and is subjected to oxidation reaction, and the gas generated after the reaction is discharged from the upper part and is subjected to harmless treatment through the tail gas treatment unit.
According to this embodiment, after the pre-oxidation treatment is completed on the carbon nanotubes, the pre-heater 4 stops introducing gas into the total reactor 5, the treated carbon nanotubes in the total reactor 5 drop to the bottom, and the valve of the discharge port 12 is opened, and the pre-heater 4 again introduces gas into the total reactor 5, so that the materials in the total reactor 5 are driven by the air inlet pressure and are conveyed to the carbon nanotube collecting unit through the pipeline of the discharge port.
According to this embodiment, after the pre-oxidation treatment is performed on the carbon nanotubes, the device may also be configured to directly close the top exhaust valve of the reactor without closing the gas delivery from the pre-heater to the total reactor, and simultaneously open the lower exhaust valve, so that the carbon nanotube powder may enter the storage tank of the carbon nanotube collecting unit under the driving of the air flow entering the total reactor, and transfer the powder of the carbon nanotubes after the cooling of the storage tank, so that the carbon nanotube collecting unit is communicated with air, and nitrogen needs to be introduced.
According to the embodiment, the carbon nanotube collecting unit is connected with a second N 2 Intake manifold 10, the second N 2 An air inlet header pipe 10 is connected to the bottom of the carbon nanotube collecting unit 7, and continuously introduces N into the carbon nanotube collecting unit 7 2 To get toThe carbon nanotube collecting unit 7 is subjected to oxygen discharge treatment, an air outlet 14 is provided at the upper part of the carbon nanotube collecting unit 7, and the excessive oxygen in the carbon nanotube collecting unit is discharged from the air outlet.
In one embodiment, the cooling unit outside the carbon nanotube collecting unit may adopt a water cooling pipe, wherein the water cooling pipe is wrapped on the outer wall of the carbon nanotube collecting unit, and is provided with a cooling water inlet 8 and a cooling water outlet 9.
According to the embodiment, the materials in the carbon nanotube collecting unit can be rapidly cooled while being protected by the nitrogen.
According to the embodiment, the pre-oxidation device mixes the gases in advance through the gas mixing unit, so that the proportion of the gases can be accurately controlled, the gases are heated in advance through the preheater, the problem that the temperature of the total reactor is low is solved, the tail gas treatment unit is arranged, the tail gas is subjected to harmless treatment, and the air pollution is reduced.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (7)
1. A pre-oxidation apparatus for purifying carbon nanotubes, the pre-oxidation apparatus comprising: the device comprises a gas mixing unit, a preheater, a total reactor, a tail gas treatment unit, a carbon nano tube collecting unit and a cooling unit; one end of the gas mixing unit is connected with a first N2 air inlet main pipe and a CO2 air inlet main pipe through pipelines respectively, the other end of the gas mixing unit is connected to the preheater through a pipeline, the preheater is connected to the total reactor through a pipeline, a feed inlet and a discharge port are arranged on the total reactor, an exhaust port is arranged on the total reactor, and the exhaust port is connected to the tail gas treatment unit; the discharge port of the total reactor is connected to a carbon nano tube collecting unit through a pipeline, and the cooling unit is arranged outside the carbon nano tube collecting unit;
the total reactor is of a vertical structure, and an exhaust port is arranged at the top of the total reactor; the feed inlet is arranged at one side of the upper part of the total reactor; the discharge port is arranged at the bottom of the total reactor, and a valve is arranged at the discharge port;
the pipeline of the preheater connected to the total reactor enters the total reactor from the upper part of the total reactor and extends to the lower part of the total reactor, and a valve is arranged on the pipeline of the preheater connected to the total reactor;
the carbon nanotube collecting unit is connected with a second N2 air inlet manifold, the second N2 air inlet manifold is connected to the bottom of the carbon nanotube collecting unit, N2 is continuously introduced into the carbon nanotube collecting unit so as to perform oxygen discharge treatment on the carbon nanotube collecting unit, an air outlet is formed in the upper portion of the carbon nanotube collecting unit, and redundant oxygen in the carbon nanotube collecting unit is discharged from the air outlet.
2. The apparatus according to claim 1, wherein N2 and CO2 are introduced into the gas mixing unit through a first N2 gas inlet manifold and a CO2 gas inlet manifold, respectively, and the two gases are mixed in the gas mixing unit and then transferred to the preheater through a pipe, the preheater heats the mixed gas, and the heated mixed gas is introduced into the total reactor through the pipe for reaction.
3. The apparatus of claim 1, wherein the top of the total reactor is further provided with a closed viewing window for real-time viewing during the reaction of the total reactor.
4. The device according to claim 1, wherein a temperature sensor and a pressure sensor are also arranged on the total reactor to monitor the temperature and the pressure in the total reactor; and a pressure sensor is arranged on the gas mixing unit; and a pressure sensor and a temperature sensor are arranged on the preheater.
5. The apparatus according to claim 1, wherein the valve at the discharge port at the bottom of the total reactor is closed, the exhaust port is opened, the valve on the pipe passing into the total reactor in the preheater is opened, the gas in the preheater is passed into the total reactor, and the gas is blown upward from the bottom of the total reactor, so that the carbon nanotubes entering from the feed port float in the reactor, and oxidation reaction is performed, and the gas generated after the reaction is discharged from the upper part and is subjected to harmless treatment by the tail gas treatment unit.
6. The apparatus according to claim 1, wherein after the pre-oxidation treatment of the carbon nanotubes is completed, the pre-heater stops introducing gas into the total reactor, the treated carbon nanotubes in the total reactor fall to the bottom, and the valve of the discharge port is opened, and the pre-heater again introduces gas into the total reactor, so that the materials in the total reactor are driven by the air inlet pressure to be conveyed to the carbon nanotube collecting unit through the pipeline of the discharge port.
7. The device according to claim 1, wherein the cooling unit outside the carbon nanotube collecting unit can adopt a water cooling pipe, and the water cooling pipe is wrapped on the outer wall of the carbon nanotube collecting unit, so that the material in the carbon nanotube collecting unit can be rapidly cooled while being protected by introducing nitrogen.
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| KR20070018128A (en) * | 2007-01-19 | 2007-02-13 | 한국전자통신연구원 | Purification solution for carbon nano tube and method for purifying carbon nano tube thereby |
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| JP3713561B2 (en) * | 2001-06-26 | 2005-11-09 | 独立行政法人科学技術振興機構 | Method for synthesizing highly aligned aligned carbon nanotubes using organic liquid and apparatus for synthesizing the same |
| CN105060271A (en) * | 2015-07-30 | 2015-11-18 | 惠州集越纳米材料技术有限责任公司 | Carbon nano-tube purification method |
| CN106268636B (en) * | 2016-08-12 | 2019-01-11 | 东华大学 | The carbon nano-fiber adsorbent material and preparation method thereof of aminated carbon nano tube doping |
| CN106365146A (en) * | 2016-08-22 | 2017-02-01 | 赖世权 | Impurity removal method of carbon nanotubes |
| CN106315560A (en) * | 2016-08-22 | 2017-01-11 | 赖世权 | Carbon nanotube purification method |
| CN109650379B (en) * | 2019-02-19 | 2020-08-18 | 厦门大学 | Single-walled carbon nanotube gradient oxidation purification method |
| CN112142038A (en) * | 2020-08-28 | 2020-12-29 | 西安交通大学 | Carbon nanotube batch preparation system with tail gas waste heat recycling device |
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| KR20070018128A (en) * | 2007-01-19 | 2007-02-13 | 한국전자통신연구원 | Purification solution for carbon nano tube and method for purifying carbon nano tube thereby |
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