WO2023159697A1 - Apparatus and method for purifying carbon nanotubes - Google Patents

Apparatus and method for purifying carbon nanotubes Download PDF

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Publication number
WO2023159697A1
WO2023159697A1 PCT/CN2022/081329 CN2022081329W WO2023159697A1 WO 2023159697 A1 WO2023159697 A1 WO 2023159697A1 CN 2022081329 W CN2022081329 W CN 2022081329W WO 2023159697 A1 WO2023159697 A1 WO 2023159697A1
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heating chamber
chamber
vacuum
furnace body
cooling
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PCT/CN2022/081329
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French (fr)
Chinese (zh)
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沈宇栋
万仁涛
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无锡东恒新能源科技有限公司
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Publication of WO2023159697A1 publication Critical patent/WO2023159697A1/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/168—After-treatment
    • C01B32/17—Purification
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the invention relates to a device and a good method for purifying carbon nanotubes, belonging to the technical field of chemical equipment.
  • carbon nanotubes As an excellent conductive agent, carbon nanotubes have been widely used in industries such as lithium batteries for new energy vehicles. This is due to its excellent thermal conductivity, electrical conductivity and good mechanical strength.
  • the one-dimensional structure of carbon nanotubes can enhance the bonding of active materials and improve the performance of pole pieces, so it has great application prospects in new energy batteries.
  • the metal impurity requirements of battery materials are also increased.
  • the acid solution dissolution method is mainly used at present.
  • the purity of carbon nanotubes obtained by acid purification is limited, and a large amount of waste acid wastewater is produced, which is seriously polluted.
  • the existing vacuum furnace is a horizontal large-scale vacuum furnace, which covers a large area, and the purity of materials in different areas of the furnace varies greatly due to uneven heating; and the production method is batch production, which has low processing output and low equipment utilization. Many disadvantages.
  • the present invention provides a device and method for purifying carbon nanotubes.
  • the device and method of the present invention can significantly improve production efficiency and output, and reduce energy consumption and production costs through continuous processing. Described technical scheme is as follows:
  • the present invention firstly provides a device for purifying carbon nanotubes.
  • the device of the present invention uses an improved vacuum furnace, which is specially used for purifying carbon nanotubes and avoids high emissions from pickling. Compared with the existing The production efficiency of the vacuum furnace has also been greatly improved.
  • a device for purifying carbon nanotubes includes: a first furnace body, a heating chamber, a cooling chamber, a vacuum system, a gas filling and deflation system, an air pressure system, and a control system; wherein, the first furnace body For temporary storage of materials, the first furnace body is connected to the heating chamber and the cooling chamber through pipelines in turn, and the material outlets of the first furnace body, the heating chamber, and the cooling chamber are respectively arranged There is a vacuum valve; the vacuum system is respectively connected to the first furnace body and the heating chamber for vacuuming the first furnace body and the heating chamber; the inflation and deflation system is respectively connected to the The replacement gas inlet of the first furnace body and the cooling chamber is used to provide replacement gas for the first furnace body and the cooling chamber; the air pressure system is used to provide power for the vacuum valve, the The control system is electrically connected with other systems for controlling the device.
  • the heating chamber and the cooling chamber can be provided in multiples, each heating chamber is connected to the vacuum system, and each heating chamber is respectively provided with a heating unit.
  • the first furnace body is provided with a material inlet, and is connected to a feed storage tank through a pipeline.
  • the first furnace body is also provided with a replacement gas inlet and a vacuum exhaust port, the replacement gas inlet is connected to the inflation and deflation system through a pipeline, and the vacuum exhaust port is connected through a pipeline to the vacuum system; capable of oxygen replacement; and a vacuum valve is provided at the material outlet of the lower part of the first furnace body, and is connected to the heating chamber through a pipeline.
  • the carbon nanotubes in the feed storage tank are introduced into the first furnace body through a pipeline, and the vacuum exhaust port and the replacement gas inlet of the first furnace body are opened, Oxygen replacement is carried out in the first furnace body, so that the oxygen content therein is lower than 50ppm.
  • the heating chamber includes a first heating chamber and a second heating chamber, and both the first heating chamber and the second heating chamber are provided with a vacuum exhaust port, so The communication pipe of the vacuum exhaust port is connected to a vacuum system for evacuating during the heating process of the first heating chamber and the second heating chamber to prevent oxidation of materials.
  • the first heating chamber is a negative pressure heating chamber, which is used to heat the carbon nanotube material to 500° C. while evacuating to 1000 Pa.
  • the second heating chamber is a vacuum heating purification chamber, which is used to heat the material to 2000° C., simultaneously evacuate to 3 Pa, and keep it warm for 120 minutes.
  • the cooling chamber can also be set in multiples; specifically, it includes a first cooling chamber and a second cooling chamber, the first cooling chamber is a lowering chamber, and the second cooling chamber is a lowering chamber. material room.
  • the temperature of the first cooling chamber is reduced by air cooling to reduce the temperature of the material to 500°C.
  • the second cooling chamber can be provided with a replacement gas inlet, and cold nitrogen or argon can be supplemented through the replacement gas inlet, so that the furnace pressure in the second cooling chamber can be restored to atmospheric pressure, and at the same time, the carbon The nanotubes are cooled to below 400°C, and after the cooling is completed, the vacuum valve of the material outlet of the second cooling chamber is opened to transport the purified carbon nanotubes to the discharge storage tank.
  • the vacuum system is composed of slide valve pumps, Roots pumps and pipeline valves, and the pumps are redundantly selected to achieve rapid vacuum pumping; the vacuum system can also use vacuum measurement The unit measures the vacuum of the furnace to be evacuated; and the vacuum system is connected to the condensation filtration system.
  • the vacuum measurement unit of the vacuum system adopts a two-way digital display resistance vacuum measuring instrument, which has a relatively wide measurement range (105 ⁇ 10-1Pa), and can realize the whole process of continuous vacuum measurement and measurement of the vacuum system. control.
  • the condensate filter system is a condensate filter collection tank integrating multiple functions such as storage, filtration, rough purification, and fine purification. Filter out glue, metal vapor and dust in the furnace, which can greatly improve the service life of the vacuum pump, especially suitable for occasions with a lot of dust and binder.
  • the charging and discharging system is equipped with Ar and N 2 gas charging devices for air replacement, so as to achieve the purpose of directional air flow of carrier gas in each furnace, rapid cooling and other purposes.
  • the air pressure system is a pneumatic assembly, including three components of air source treatment, that is, a filter, a pressure reducing valve, and a lubricator; and the air pressure system also includes a pressure gauge, an electromagnetic Reversing valves, pneumatic joints, pneumatic pipelines, etc.; used to control the vacuum valves of the first furnace body, heating chamber, and cooling chamber.
  • the control system takes an intelligent temperature controller, a thyristor voltage regulator, and a low-voltage transformer as the core to form an electric control system including power supply, control, monitoring, and alarm protection functions.
  • the intelligent temperature controller includes temperature measurement and control elements, and the temperature actuator adopts a continuous non-on-off thyristor voltage regulator, which is not a traditional electrical on-off type in control, but is continuously and automatically adjusted according to temperature control requirements. Heating power; high precision temperature control, no noise, no interference to the internal power grid.
  • the temperature control element adopts the digital display intelligent temperature controller of Japan's Shimaden (SHIMADEN) brand ⁇ UK Continental brand, with a control accuracy of ⁇ 0.1%.
  • the process curve can be set according to user requirements, and multiple records can be stored. Temperature process curve, multiple sets of PID parameters, and PID self-tuning function can effectively prevent temperature overshoot, and has automatic + manual control function, continuous automatic control of heating power.
  • the temperature measuring element uses thermocouples and two-color infrared to measure the temperature of each furnace body in real time. And a PT100 (0-500°C) thermocouple is set outside the heat shield to monitor the temperature of the furnace shell to ensure safe operation.
  • a set of water cooling system including water inlet distribution pipe and open water outlet bucket is also configured.
  • the first furnace body, furnace doors, furnace shells, electrodes, vacuum units, etc. of the heating chamber and cooling chamber are cooled by passing water.
  • each channel of cooling water has a manual valve, which can adjust the flow rate as required; and the water inlet pipe is equipped with an electric contact pressure gauge.
  • the control system will give an audible and visual alarm.
  • the electrode water circuit is also equipped with a water temperature switch, which will automatically cut off the power supply of the heater when the temperature is too high or the water pressure is too low.
  • the water cooling system is also equipped with a backup water interface, which is used to open the backup water source in case of emergency power failure.
  • the first furnace body is a vertical conical structure, which is welded by double-layer steel plate rolls, and a cooling water diversion plate is arranged in the interlayer, which can ensure a cooling furnace with uniform cooling water. There will be no local overheating, burning parts, etc.; and the two ends of the cylinder are welded with flanges.
  • the inner wall of the furnace is made of SUS304 heat-resistant stainless steel, and the outer wall is made of Q235A carbon steel.
  • the furnace bodies of the first heating chamber and the second heating chamber are also equipped with electrode introduction devices, pressure relief and explosion-proof devices, and are equipped with thermocouple temperature measuring holes, equipment lifting and unloading rings, etc.;
  • the door adopts double doors.
  • the furnace door is welded by inner and outer heads and flanges.
  • the inner head is made of SUS304 heat-resistant stainless steel, and the outer head is made of Q235A carbon steel. Water can be passed through the middle to cool the furnace cover; Cold air door; the furnace door is opened with a ring gear locking quick-opening door structure.
  • the ring gear that locks the furnace door is driven to rotate by a cylinder.
  • the furnace shell flange is equipped with a vacuum seal ring, and the furnace door can be vacuumed when the furnace door is closed tightly.
  • the heating chamber has a conical structure, the skeleton is welded by heat-resistant stainless steel and section steel, and carbon fiber felt is arranged inside as a thermal insulation layer, and the heating body of the heating unit can use special graphite;
  • the heating unit can also use an electric heating wire, and the heating unit can be connected to the outside through an opening provided on the furnace body of the heating chamber, and after the electrical connection is set, the above opening is sealed.
  • the heating unit is electrically connected to the control system, and the control system provides power to enable the heating unit to heat the heating chamber.
  • the cooling chamber can adopt a furnace body with the same structure as the first furnace body.
  • the present invention also provides a method for the purification of carbon nanotubes, the method adopts the purification device of the present invention, and the method specifically includes the following steps:
  • Step 1 Import the carbon nanotubes in the feed storage tank into the first furnace body through the material delivery pipeline, close the material delivery pipeline, open the vacuum exhaust port and the replacement gas inlet of the first furnace body, and charge and discharge
  • the gas system feeds nitrogen or argon into the first furnace body, and the gas in the first furnace body is pumped out by the vacuum system, so as to perform oxygen replacement in the first furnace body, so that the oxygen content in it is low at 50ppm;
  • Step 2 After the oxygen replacement of the first furnace body is completed, the vacuum valve of the discharge port at the lower end of the first furnace body is opened by the air pressure system, and the materials are passed into the first heating chamber, and when all the materials fall into the After the first heating chamber is described, the vacuum valve is closed; the first heating chamber is a negative pressure heating chamber, and the material is heated to 500 ° C and vacuumed to 1000 Pa at the same time;
  • Step 3 After the control system detects that the first heating chamber reaches 500°C, and the vacuum system detects that the pressure of the first heating chamber reaches 1000Pa, the air pressure system controls the temperature of the first heating chamber Open the vacuum valve so that the material in the first heating chamber falls into the second heating chamber, the second heating chamber is a vacuum heating purification chamber, heat the material to 2000 ° C, and at the same time evacuate to 3Pa, and keep it warm for 120min ;
  • Step 4 After Step 3 is completed, the vacuum valve of the second heating chamber is controlled by the air pressure system to open, so that the materials in the second heating chamber fall into the first cooling chamber, and the second heating chamber
  • the first cooling chamber is a cooling and feeding chamber, and the first cooling chamber is cooled by air to cool the material to 500°C;
  • Step five after the step four is completed, the vacuum valve of the first cooling chamber is controlled by the air pressure system to open, so that the materials in the first cooling chamber fall into the second cooling chamber, and when the materials are completely Close the vacuum valve behind, open the replacement gas inlet of the second cooling chamber, supplement cold nitrogen or argon through the replacement gas inlet, and restore the furnace pressure in the second cooling chamber to atmospheric pressure, and simultaneously make the carbon nanotubes Cool to below 400°C.
  • the carbon nanotubes are heated and evacuated through continuous feeding in a multi-stage conical vacuum furnace, which solves the obvious differences in purity at different positions of the horizontal vacuum furnace, low processing efficiency, and high energy consumption (technical problems, for the background technology
  • the disadvantages of the existing technology in the present invention the processing capacity of the unit equipment has been increased by 50%, the power consumption has been reduced by 20%, and the quality stability has also been improved.
  • Fig. 1 is the overall structure schematic diagram of device according to the present invention.
  • Fig. 2 is the specific schematic flow sheet of purification method according to the present invention.
  • the first furnace body 2. The first heating chamber; 3. The second heating chamber; 4. The first cooling chamber; 5. The second cooling chamber; 6. Vacuum system; 7. Condensation filtration system; 8. Inflatable and deflated system; 9. Vacuum system; 10. Control system.
  • the device includes: a device for purifying carbon nanotubes according to the present invention, including: a first furnace body 1, a heating chamber , cooling chamber, vacuum system 6, inflation and deflation system 8, air pressure system 9 and control system 10; wherein, the first furnace body 1 is used for temporary storage of materials, the first furnace body 1 is connected with the heating chamber, the The cooling chambers are sequentially connected by pipelines, and vacuum valves are respectively provided at the material outlets of the first furnace body 1 and the heating chamber and the cooling chamber; the vacuum system is respectively connected to the first furnace body and the first furnace body.
  • the heating chamber is used to evacuate the first furnace body and the heating chamber;
  • the inflation and deflation system is respectively connected to the replacement gas inlets of the first furnace body and the cooling chamber, and is used for The first furnace body and the cooling chamber provide replacement gas;
  • the air pressure system is used to provide power for the vacuum valve, and the control system is electrically connected to other systems for controlling the device.
  • each heating chamber is connected to the vacuum system, and each heating chamber is respectively provided with a heating unit.
  • the first furnace body is provided with a material inlet, and is connected to a feed storage tank through a pipeline.
  • the first furnace body is also provided with a replacement gas inlet and a vacuum exhaust port, the replacement gas inlet is connected to the inflation and deflation system through a pipeline, and the vacuum exhaust port is connected to the gas filling and deflation system through a pipeline Connected to the vacuum system 6, capable of oxygen replacement; and a vacuum valve is provided at the material outlet of the lower part of the first furnace body 1, and is connected to the heating chamber through a pipeline.
  • the carbon nanotubes in the feed storage tank are introduced into the first furnace body 1 through pipelines, and the vacuum exhaust port and the replacement gas inlet of the first furnace body are opened. Oxygen replacement is carried out in the middle, so that the oxygen content in it is lower than 50ppm.
  • the heating chamber includes a first heating chamber 2 and a second heating chamber 3, and both the first heating chamber 2 and the second heating chamber 3 are provided with a vacuum exhaust port, and the vacuum The exhaust port is connected to the vacuum system 6 through a pipeline, and is used for evacuating during the heating process of the first heating chamber 2 and the second heating chamber 3, so as to prevent oxidation of materials.
  • the first heating chamber 2 is a negative pressure heating chamber, which is used to heat the carbon nanotube material to 500° C. while evacuating to 1000 Pa.
  • the second heating chamber 3 is a vacuum heating purification chamber, which is used to heat the material to 2000° C. while evacuating to 3 Pa, and keep it warm for 120 minutes.
  • the cooling chamber can also be set to a plurality; specifically, it includes a first cooling chamber 4 and a second cooling chamber 5, the first cooling chamber 4 is a lowering chamber, and the second cooling chamber 5 is a cooling chamber .
  • the temperature of the first cooling chamber 4 is reduced by air cooling to reduce the temperature of the material to 500°C; specifically, an external fan can be used to cool it down.
  • the second cooling chamber 5 is also provided with a replacement gas inlet, and the replacement gas inlet is connected to the inflation and deflation system 8, and the inflation and deflation system 8 supplements cold nitrogen or gas through the replacement gas inlet.
  • argon to restore the furnace pressure in the second cooling chamber 5 to atmospheric pressure, and at the same time cool the carbon nanotubes therein to below 400°C, and open the vacuum at the material outlet of the second cooling chamber 5 after the cooling is completed.
  • the valve transports the purified carbon nanotubes to the discharge storage tank through the material delivery pipeline.
  • the vacuum system 6 is composed of a slide valve pump, a Roots pump, and pipeline valves. Redundant selection is used for the pumps to achieve the purpose of quickly pumping up the vacuum.
  • the vacuum system can also use vacuum measurement The unit measures the vacuum of the furnace; and the vacuum system is connected to a condensate filtration system 7 .
  • the condensate filter system 7 is a condensate filter collection tank that integrates multiple functions such as storage, filtration, rough purification, and fine purification. Filter out glue, metal vapor and dust in the furnace, which can greatly improve the service life of the vacuum pump, especially suitable for occasions with a lot of dust and binder.
  • the charging and discharging system 8 is equipped with two sets of Ar and N gas charging devices for air replacement, so as to achieve the purpose of directional air flow of carrier gas in each furnace, rapid cooling, etc. .
  • the air pressure system 9 is a pneumatic assembly, including three components for air source treatment, namely a filter, a pressure reducing valve, and a lubricator; and the air pressure system 9 also includes a pressure gauge , electromagnetic reversing valve, pneumatic joint, pneumatic pipeline, etc.; used to control the vacuum valves of the first furnace body, heating chamber, and cooling chamber;
  • Fig. 1 is an example, only shows the air pressure system 9 and the The connection of the vacuum valve of the second cooling chamber 5; although it is not shown in Fig. 1, it should be understood that the air pressure system 9 is connected with the first furnace body 1 and the first heating chamber 2 through a conventional connection mode. , the vacuum valves of the second heating chamber 3 , the first cooling chamber 4 and the first cooling chamber 5 are connected.
  • the control system 10 takes an intelligent temperature controller, a thyristor voltage regulator, and a low-voltage transformer as the core to form an electric control system including power supply, control, monitoring, and alarm protection functions.
  • the intelligent temperature controller includes temperature measurement and control elements, and the temperature actuator adopts a continuous non-on-off thyristor voltage regulator, which is not a traditional electrical on-off type in control, but is continuously and automatically adjusted according to temperature control requirements. Heating power; high precision temperature control, no noise, no interference to the internal power grid.
  • the temperature control element adopts the digital display intelligent temperature controller of Japan's Shimaden (SHIMADEN) brand ⁇ UK Continental brand, with a control accuracy of ⁇ 0.1%.
  • the process curve can be set according to user requirements, and multiple records can be stored. Temperature process curve, multiple sets of PID parameters, and PID self-tuning function can effectively prevent temperature overshoot, and has automatic + manual control function, continuous automatic control of heating power.
  • the temperature measuring element uses thermocouples and two-color infrared to measure the temperature of each furnace body in real time. And a PT100 (0-500°C) thermocouple is set outside the heat shield to monitor the temperature of the furnace shell to ensure safe operation.
  • the vacuum measurement unit of the vacuum system adopts a two-way digital display resistance vacuum measuring instrument, which has a relatively wide measurement range (105 ⁇ 10-1Pa), and can realize the whole process of continuous vacuum measurement and measurement of the vacuum system. control.
  • a set of water cooling system including water inlet distribution pipe and open water outlet bucket is also configured.
  • the first furnace body, furnace doors, furnace shells, electrodes, vacuum units, etc. of the heating chamber and cooling chamber are cooled by passing water.
  • each channel of cooling water has a manual valve, which can adjust the flow rate as required; and the water inlet pipe is equipped with an electric contact pressure gauge.
  • the control system will give an audible and visual alarm.
  • the electrode water circuit is also equipped with a water temperature switch, which will automatically cut off the power supply of the heater when the temperature is too high or the water pressure is too low.
  • the water cooling system is also equipped with a backup water interface, which is used to open the backup water source in case of emergency power failure.
  • the first furnace body 1 is a vertical conical structure, which is welded by double-layer steel plate rolls, and a cooling water diversion plate is arranged in the interlayer to ensure uniform cooling of the cooling water. All parts of the furnace body will not be overheated or burned out; and both ends of the cylinder are welded with flanges.
  • the inner wall of the furnace is made of SUS304 heat-resistant stainless steel, and the outer wall is made of Q235A carbon steel.
  • the furnace bodies of the first heating chamber 2 and the second heating chamber 3 are also provided with electrode introduction devices, pressure relief and explosion-proof devices, and thermocouple temperature measuring holes, equipment lifting and unloading rings, etc.
  • the furnace door adopts double doors, the furnace door is welded by inner and outer heads and flanges, the inner head is SUS304 heat-resistant stainless steel, the outer head is Q235A carbon steel, and water can be passed through the middle to cool the furnace cover; There is a quick cooling air door; the furnace door is opened with a ring gear locking quick door structure.
  • the gear ring that locks the furnace door is driven by a cylinder to rotate.
  • the flange of the furnace shell is equipped with a vacuum seal ring, and the furnace door can be vacuumed when the furnace door is closed tightly.
  • the heating chamber has a conical structure, the skeleton is welded by heat-resistant stainless steel and section steel, and carbon fiber felt is arranged inside as a thermal insulation layer, and the heating body of the heating unit can use special graphite;
  • the heating unit can also use an electric heating wire, and the heating unit can be connected to the outside through an opening provided on the furnace body of the heating chamber, and after the electrical connection is set, the above opening is sealed.
  • the heating unit is electrically connected to the control system, and the control system provides power to enable the heating unit to heat the heating chamber.
  • the first cooling chamber and the second cooling chamber can adopt a furnace body with the same structure as the first furnace body.
  • This embodiment provides a method for purifying carbon nanotubes.
  • the method adopts the purification device of Embodiment 1 of the present invention, as shown in FIG. 1 and FIG. 2 , and the method specifically includes the following steps:
  • Step 1 Import the carbon nanotubes in the feed storage tank into the first furnace body through the material delivery pipeline, close the material delivery pipeline, open the vacuum exhaust port and the replacement gas inlet of the first furnace body, and charge and discharge
  • the gas system feeds nitrogen or argon into the first furnace body, and the gas in the first furnace body is pumped out by the vacuum system, so as to perform oxygen replacement in the first furnace body, so that the oxygen content in it is low at 50ppm;
  • Step 2 After the oxygen replacement of the first furnace body is completed, the vacuum valve of the discharge port at the lower end of the first furnace body is opened by the air pressure system, and the materials are passed into the first heating chamber, and when all the materials fall into the After the first heating chamber is described, the vacuum valve is closed; the first heating chamber is a negative pressure heating chamber, and the material is heated to 500 ° C and vacuumed to 1000 Pa at the same time;
  • Step 3 After the control system detects that the first heating chamber reaches 500°C, and the vacuum system detects that the pressure of the first heating chamber reaches 1000Pa, the air pressure system controls the temperature of the first heating chamber Open the vacuum valve so that the material in the first heating chamber falls into the second heating chamber, the second heating chamber is a vacuum heating purification chamber, heat the material to 2000 ° C, and at the same time evacuate to 3Pa, and keep it warm for 120min ;
  • Step 4 After Step 3 is completed, the vacuum valve of the second heating chamber is controlled by the air pressure system to open, so that the materials in the second heating chamber fall into the first cooling chamber, and the second heating chamber
  • the first cooling chamber is a cooling and feeding chamber, and the first cooling chamber is cooled by air to cool the material to 500°C;
  • Step five after the step four is completed, the vacuum valve of the first cooling chamber is controlled by the air pressure system to open, so that the materials in the first cooling chamber fall into the second cooling chamber, and when the materials are completely Close the vacuum valve behind, open the replacement gas inlet of the second cooling chamber, supplement cold nitrogen or argon through the replacement gas inlet, and restore the furnace pressure in the second cooling chamber to atmospheric pressure, and simultaneously make the carbon nanotubes Cool to below 400°C.

Abstract

An apparatus and method for purifying carbon nanotubes, which can remarkably improve the production efficiency and yield and reduce energy consumption and production cost by means of continuous processing. The apparatus comprises a first furnace (1), heating chambers (2, 3), cooling chambers (4, 5), a vacuum system (6), a gas charge/discharge system (8), an air pressure system (9), and a control system (10); the first furnace (1) is sequentially connected to the heating chambers (2, 3) and the cooling chambers (4, 5) by means of pipelines; vacuum valves are provided at material outlets of the first furnace (1), the heating chambers (2, 3), and the cooling chambers (4, 5); the vacuum system (6) is separately connected to vacuum gas outlets of the first furnace (1) and the heating chambers (2, 3), and is used for vacuumizing the first furnace (1) and the heating chambers (2, 3); the gas charge/discharge system (8) is separately connected to replacement gas inlets of the first furnace (1) and the cooling chambers (4, 5) and used for providing a replacement gas for the first furnace (1) and the cooling chambers (4, 5); the air pressure system (9) is used for providing power for the vacuum valves; the control system (10) is used for controlling the apparatus.

Description

一种用于碳纳米管提纯的装置及方法A device and method for purifying carbon nanotubes 技术领域technical field
本发明涉及一种用于碳纳米管提纯的装置及好的方法，属于化工设备技术领域。The invention relates to a device and a good method for purifying carbon nanotubes, belonging to the technical field of chemical equipment.
背景技术Background technique
碳纳米管作为优良的导电剂，已在新能源汽车锂电池等行业得到广泛应用。这是由于其具有优异的导热、导电性及较好的机械强度等优点。此外，碳纳米管的一维结构可以增强活性材料的粘结同时可以改善极片的性能，因此在新能源电池方面有很大的应用前景。As an excellent conductive agent, carbon nanotubes have been widely used in industries such as lithium batteries for new energy vehicles. This is due to its excellent thermal conductivity, electrical conductivity and good mechanical strength. In addition, the one-dimensional structure of carbon nanotubes can enhance the bonding of active materials and improve the performance of pole pieces, so it has great application prospects in new energy batteries.
随着对电池安全性要求的提高，电池材料的金属杂质要求也同时提高。为了降低碳纳米管中残留金属催化剂的含量，目前主要使用酸液溶解法，酸法提纯所得到的碳纳米管纯度有限同时产生大量废酸废水，污染较重。With the improvement of battery safety requirements, the metal impurity requirements of battery materials are also increased. In order to reduce the content of residual metal catalysts in carbon nanotubes, the acid solution dissolution method is mainly used at present. The purity of carbon nanotubes obtained by acid purification is limited, and a large amount of waste acid wastewater is produced, which is seriously polluted.
现有的真空炉是卧式大型真空炉，占地面积大，炉膛内不同区域物料由于受热不均匀纯度也差异较大；并且生产方式为间歇式生产，存在处理产量低、设备利用率低等诸多缺点。The existing vacuum furnace is a horizontal large-scale vacuum furnace, which covers a large area, and the purity of materials in different areas of the furnace varies greatly due to uneven heating; and the production method is batch production, which has low processing output and low equipment utilization. Many disadvantages.
发明内容Contents of the invention
为了解决目前存在的上述问题，本发明提供了一种用于碳纳米管提纯的装置及方法，本发明的装置及方法通过连续处理，可以显著提高生产效率和产量，降低能耗和生产成本。所述技术方案如下：In order to solve the above existing problems, the present invention provides a device and method for purifying carbon nanotubes. The device and method of the present invention can significantly improve production efficiency and output, and reduce energy consumption and production costs through continuous processing. Described technical scheme is as follows:
本发明首先提供的一种用于碳纳米管提纯的装置，本发明的装置使用一种改进的真空炉，专门用于提纯处理碳纳米管，避免了酸洗的高排放，相对于现有的真空炉在生产效率也有较大的改进。The present invention firstly provides a device for purifying carbon nanotubes. The device of the present invention uses an improved vacuum furnace, which is specially used for purifying carbon nanotubes and avoids high emissions from pickling. Compared with the existing The production efficiency of the vacuum furnace has also been greatly improved.
根据本发明提供的一种用于碳纳米管提纯的装置，包括：第一炉体、加热室、冷却室、真空***、充放气***、空压***以及控制***；其中，第一炉体用于临时存储物料，所述第一炉体与所述加热室、所述冷却室依次通过管道连接，并且在所述第一炉体与所述加热室、所述冷却室的物料出口分别设置有真空阀门；所述真空***分别连接至所述第一炉体与所述加热室，用于为所述第一炉体和所述加热室抽真空；所述充放气***分别连接至所述第一炉体和所述冷却室的置换气体入口，用于为所述第一炉体与所述冷却室提供置换气体；所述空压***用于为所述真空阀门提供动力，所述控制***与其他***电性连接，用于对所述装置进行控制。A device for purifying carbon nanotubes according to the present invention includes: a first furnace body, a heating chamber, a cooling chamber, a vacuum system, a gas filling and deflation system, an air pressure system, and a control system; wherein, the first furnace body For temporary storage of materials, the first furnace body is connected to the heating chamber and the cooling chamber through pipelines in turn, and the material outlets of the first furnace body, the heating chamber, and the cooling chamber are respectively arranged There is a vacuum valve; the vacuum system is respectively connected to the first furnace body and the heating chamber for vacuuming the first furnace body and the heating chamber; the inflation and deflation system is respectively connected to the The replacement gas inlet of the first furnace body and the cooling chamber is used to provide replacement gas for the first furnace body and the cooling chamber; the air pressure system is used to provide power for the vacuum valve, the The control system is electrically connected with other systems for controlling the device.
根据本发明的装置，所述加热室和所述冷却室能够设置为多个，每个加热室均连接至所 述真空***，并且每个加热室中分别设置有加热单元。According to the device of the present invention, the heating chamber and the cooling chamber can be provided in multiples, each heating chamber is connected to the vacuum system, and each heating chamber is respectively provided with a heating unit.
根据本发明的装置，所述第一炉体上设置有物料入口，并通过管道连接至进料储罐。According to the device of the present invention, the first furnace body is provided with a material inlet, and is connected to a feed storage tank through a pipeline.
根据本发明的装置，所述第一炉体还设置有置换气体入口，以及真空排气口，所述置换气体入口通过管道连接至所述充放气***，所述真空排气口通过管道连接至所述真空***；能够进行氧气置换；并且所述第一炉体的下部的物料出口处设置有真空阀门，并通过管道连接至加热室。According to the device of the present invention, the first furnace body is also provided with a replacement gas inlet and a vacuum exhaust port, the replacement gas inlet is connected to the inflation and deflation system through a pipeline, and the vacuum exhaust port is connected through a pipeline to the vacuum system; capable of oxygen replacement; and a vacuum valve is provided at the material outlet of the lower part of the first furnace body, and is connected to the heating chamber through a pipeline.
根据本发明的装置，在一种实施方式中，将进料储罐中的碳纳米管通过管道导入第一炉体中，并打开所述第一炉体的真空排气口和置换气体入口，在第一炉体中进行氧气置换，使其中含氧量低于50ppm。According to the device of the present invention, in one embodiment, the carbon nanotubes in the feed storage tank are introduced into the first furnace body through a pipeline, and the vacuum exhaust port and the replacement gas inlet of the first furnace body are opened, Oxygen replacement is carried out in the first furnace body, so that the oxygen content therein is lower than 50ppm.
根据本发明的装置，在一种实施方式中，所述加热室包括第一加热室和第二加热室，所述第一加热室和所述第二加热室均设置有真空排气口，所述真空排气口沟通管道连接至真空***，用于在所述第一加热室和所述第二加热室进行加热的过程中抽真空，以防止物料氧化。According to the device of the present invention, in one embodiment, the heating chamber includes a first heating chamber and a second heating chamber, and both the first heating chamber and the second heating chamber are provided with a vacuum exhaust port, so The communication pipe of the vacuum exhaust port is connected to a vacuum system for evacuating during the heating process of the first heating chamber and the second heating chamber to prevent oxidation of materials.
根据本发明的装置，在一种实施方式中，所述第一加热室为负压加热室，用于将碳纳米管物料加热至500℃、同时抽真空至1000Pa。According to the device of the present invention, in one embodiment, the first heating chamber is a negative pressure heating chamber, which is used to heat the carbon nanotube material to 500° C. while evacuating to 1000 Pa.
根据本发明的装置，在一种实施方式中，所述第二加热室为真空加热提纯室，用于将物料加热至2000℃、同时抽真空至3Pa，并保温120min。According to the device of the present invention, in one embodiment, the second heating chamber is a vacuum heating purification chamber, which is used to heat the material to 2000° C., simultaneously evacuate to 3 Pa, and keep it warm for 120 minutes.
根据本发明的装置，所述冷却室也能够设置为多个；具体包括第一冷却室和第二冷却室，所述第一冷却室为降温下料室，所述第二冷却室为降温出料室。According to the device of the present invention, the cooling chamber can also be set in multiples; specifically, it includes a first cooling chamber and a second cooling chamber, the first cooling chamber is a lowering chamber, and the second cooling chamber is a lowering chamber. material room.
在一种实施方式中，所述第一冷却室通过风冷降温，使物料降温至500℃。In one embodiment, the temperature of the first cooling chamber is reduced by air cooling to reduce the temperature of the material to 500°C.
在一种实施方式中，所述第二冷却室能够设置置换气体入口，并通过所述置换气体入口补充冷氮气或氩气，使所述第二冷却室内的炉膛压力恢复至大气压，同时使碳纳米管冷却至400℃以下，并在冷却完成后打开所述第二冷却室的物料出口的真空阀门，将提纯后的碳纳米管输送至出料储罐中。In one embodiment, the second cooling chamber can be provided with a replacement gas inlet, and cold nitrogen or argon can be supplemented through the replacement gas inlet, so that the furnace pressure in the second cooling chamber can be restored to atmospheric pressure, and at the same time, the carbon The nanotubes are cooled to below 400°C, and after the cooling is completed, the vacuum valve of the material outlet of the second cooling chamber is opened to transport the purified carbon nanotubes to the discharge storage tank.
在一种实施方式中，所述真空***由滑阀泵、罗茨泵及管路阀门构成，并且对泵采用冗余选择，以达到快速抽起真空目的；所述真空***还能够采用真空测量单元对需抽真空的炉体进行真空测量；并且所述真空***连接至冷凝过滤***。In one embodiment, the vacuum system is composed of slide valve pumps, Roots pumps and pipeline valves, and the pumps are redundantly selected to achieve rapid vacuum pumping; the vacuum system can also use vacuum measurement The unit measures the vacuum of the furnace to be evacuated; and the vacuum system is connected to the condensation filtration system.
在一种实施方式中，所述真空***的真空测量单元采用二路数显电阻真空测量仪，其具有相当宽的测量范围(105～10-1Pa)，可对真空***实现全程连续真空测量和控制。In one embodiment, the vacuum measurement unit of the vacuum system adopts a two-way digital display resistance vacuum measuring instrument, which has a relatively wide measurement range (105 ~ 10-1Pa), and can realize the whole process of continuous vacuum measurement and measurement of the vacuum system. control.
在一种实施方式中，所述冷凝过滤***是一种积储集、过滤、粗净化、精净化等多种功能于一体的冷凝过滤器收积罐。滤除炉内胶类、金属蒸气及粉尘，能够极大提高真空泵使用 寿命，特别适用粉尘、粘结剂含量多的场合。In one embodiment, the condensate filter system is a condensate filter collection tank integrating multiple functions such as storage, filtration, rough purification, and fine purification. Filter out glue, metal vapor and dust in the furnace, which can greatly improve the service life of the vacuum pump, especially suitable for occasions with a lot of dust and binder.
在一种实施方式中，所述充放气***配置有Ar、N 2贰组气体充入装置，用以进行空气置换，以实现各个炉体中载气定向气流排杂、快速冷却等目的。 In one embodiment, the charging and discharging system is equipped with Ar and N 2 gas charging devices for air replacement, so as to achieve the purpose of directional air flow of carrier gas in each furnace, rapid cooling and other purposes.
在一种实施方式中，所述空压***为气动组件，包括气源处理三联件，即过滤器、减压阀、油雾器三个部件；并且所述空压***还包括压力表、电磁换向阀、气动接头、气动管路等；用于可对第一炉体、加热室、冷却室的真空阀门进行控制。In one embodiment, the air pressure system is a pneumatic assembly, including three components of air source treatment, that is, a filter, a pressure reducing valve, and a lubricator; and the air pressure system also includes a pressure gauge, an electromagnetic Reversing valves, pneumatic joints, pneumatic pipelines, etc.; used to control the vacuum valves of the first furnace body, heating chamber, and cooling chamber.
在一种实施方式中，所述控制***以智能化温控仪、可控硅电压调整器、低压变压器为核心，构成包括供电、控制、监视、报警保护功能在内的电控***。智能化温控仪包括温度测量和控制元件，并且温度执行元件采用连续非通断式可控硅调压器，其在控制时不是传统的电气通断式，而是根据温控要求连续自动调节加热功率；对温度控制精度高，无噪音，对内部电网无干扰。In one embodiment, the control system takes an intelligent temperature controller, a thyristor voltage regulator, and a low-voltage transformer as the core to form an electric control system including power supply, control, monitoring, and alarm protection functions. The intelligent temperature controller includes temperature measurement and control elements, and the temperature actuator adopts a continuous non-on-off thyristor voltage regulator, which is not a traditional electrical on-off type in control, but is continuously and automatically adjusted according to temperature control requirements. Heating power; high precision temperature control, no noise, no interference to the internal power grid.
在一种实施方式中，温度控制元件采用日本岛电(SHIMADEN)品牌\英国欧陆品牌数显智能化温控仪，控制精度±0.1％，可根据用户要求设定的工艺曲线，并存储多条温度工艺曲线，多组PID参数，以及PID自整定功能，有效的防止温度过冲，并具有自动+手动控制功能，连续自动控制加热功率。In one embodiment, the temperature control element adopts the digital display intelligent temperature controller of Japan's Shimaden (SHIMADEN) brand\UK Continental brand, with a control accuracy of ±0.1%. The process curve can be set according to user requirements, and multiple records can be stored. Temperature process curve, multiple sets of PID parameters, and PID self-tuning function can effectively prevent temperature overshoot, and has automatic + manual control function, continuous automatic control of heating power.
在一种实施方式中，温度测量元件采用热电偶以及双色红外的方式对各个炉体进行实时温度测量。并且隔热屏外设置一支PT100(0～500℃)热电偶监测炉壳温度，确保运行安全。In one embodiment, the temperature measuring element uses thermocouples and two-color infrared to measure the temperature of each furnace body in real time. And a PT100 (0-500°C) thermocouple is set outside the heat shield to monitor the temperature of the furnace shell to ensure safe operation.
根据本发明的装置，还配置有一套包括进水分配管和开放式出水斗的水冷***。在所述装置工作之前，对第一炉体、加热室及冷却室的炉门、炉壳、电极、真空机组等进行通水冷却。According to the device of the present invention, a set of water cooling system including water inlet distribution pipe and open water outlet bucket is also configured. Before the device works, the first furnace body, furnace doors, furnace shells, electrodes, vacuum units, etc. of the heating chamber and cooling chamber are cooled by passing water.
在一种实施方式中，每路冷却水都有手动阀门，可以按需要调节流量大小；并且进水管上设有电接点压力表，当水压低于设定值时，控制***会声、光报警，同时电极水路还设有水温开关，超温或水压过低时都会自动切断加热器电源。所述水冷***还配置有备用水接口，用于紧急停电时打开备用水源。In one embodiment, each channel of cooling water has a manual valve, which can adjust the flow rate as required; and the water inlet pipe is equipped with an electric contact pressure gauge. When the water pressure is lower than the set value, the control system will give an audible and visual alarm. , At the same time, the electrode water circuit is also equipped with a water temperature switch, which will automatically cut off the power supply of the heater when the temperature is too high or the water pressure is too low. The water cooling system is also equipped with a backup water interface, which is used to open the backup water source in case of emergency power failure.
在一种实施方式中，所述第一炉体为立式圆锥体结构，由双层钢板卷筒后焊接而成，夹层内设有冷却水导流隔板，能够确保冷却水均匀的冷却炉体各个部位，不会出现局部过热，烧坏部件等现象；并且筒体两端与法兰焊接，炉体内壁为SUS304耐热不锈钢制造，外壁为Q235A碳素钢制造。In one embodiment, the first furnace body is a vertical conical structure, which is welded by double-layer steel plate rolls, and a cooling water diversion plate is arranged in the interlayer, which can ensure a cooling furnace with uniform cooling water. There will be no local overheating, burning parts, etc.; and the two ends of the cylinder are welded with flanges. The inner wall of the furnace is made of SUS304 heat-resistant stainless steel, and the outer wall is made of Q235A carbon steel.
在一种实施方式中，所述第一加热室和第二加热室的炉体上还设置有电极引入装置，泄压防爆装置，并且开设有热电偶测温孔、设备吊卸环等；炉门采用双开门，炉门由内外封头 和法兰焊成，内封头为SUS304耐热不锈钢，外封头为Q235A碳素钢，中间可通水冷却炉盖；炉门上还设有快冷风门；炉门开启采用齿圈锁紧快开门结构，锁紧炉门的齿圈由气缸驱动旋转，炉壳法兰上装有真空密封圈，关紧炉门即可抽真空。In one embodiment, the furnace bodies of the first heating chamber and the second heating chamber are also equipped with electrode introduction devices, pressure relief and explosion-proof devices, and are equipped with thermocouple temperature measuring holes, equipment lifting and unloading rings, etc.; The door adopts double doors. The furnace door is welded by inner and outer heads and flanges. The inner head is made of SUS304 heat-resistant stainless steel, and the outer head is made of Q235A carbon steel. Water can be passed through the middle to cool the furnace cover; Cold air door; the furnace door is opened with a ring gear locking quick-opening door structure. The ring gear that locks the furnace door is driven to rotate by a cylinder. The furnace shell flange is equipped with a vacuum seal ring, and the furnace door can be vacuumed when the furnace door is closed tightly.
在一种实施方式中，所述加热室为锥形结构，骨架由耐热不锈钢和型钢组焊成，内部设置有碳纤维毡作为保温隔热层，加热单元的加热体可采用特种石墨；在一种替代方案中，所述加热单元还可采用电加热丝，并且加热单元能够通过所述加热室炉体上设置的开口连接至外部，并且电连接设置完成之后，对上述开口进行密封。In one embodiment, the heating chamber has a conical structure, the skeleton is welded by heat-resistant stainless steel and section steel, and carbon fiber felt is arranged inside as a thermal insulation layer, and the heating body of the heating unit can use special graphite; In an alternative solution, the heating unit can also use an electric heating wire, and the heating unit can be connected to the outside through an opening provided on the furnace body of the heating chamber, and after the electrical connection is set, the above opening is sealed.
在一种实施方式中，进一步地，所述加热单元电连接至所述控制***，由所述控制***提供电力，使所述加热单元对所述加热室进行加热。In one embodiment, further, the heating unit is electrically connected to the control system, and the control system provides power to enable the heating unit to heat the heating chamber.
在一种实施方式中，所述冷却室能够采用与所述第一炉体同样构造的炉体。In one embodiment, the cooling chamber can adopt a furnace body with the same structure as the first furnace body.
本发明还提供一种用于碳纳米管提纯的方法，所述方法采用本发明的提纯装置，所述方法具体包括如下步骤：The present invention also provides a method for the purification of carbon nanotubes, the method adopts the purification device of the present invention, and the method specifically includes the following steps:
步骤一：将进料储罐中的碳纳米管通过物料输送管道导入第一炉体中，并关闭物料输送管道，打开所述第一炉体的真空排气口和置换气体入口，由充放气***向所述第一炉体中通入氮气或氩气，并由真空***将所述第一炉体中的气体抽出，从而在第一炉体中进行氧气置换，使其中含氧量低于50ppm；Step 1: Import the carbon nanotubes in the feed storage tank into the first furnace body through the material delivery pipeline, close the material delivery pipeline, open the vacuum exhaust port and the replacement gas inlet of the first furnace body, and charge and discharge The gas system feeds nitrogen or argon into the first furnace body, and the gas in the first furnace body is pumped out by the vacuum system, so as to perform oxygen replacement in the first furnace body, so that the oxygen content in it is low at 50ppm;
步骤二：所述第一炉体进行氧气置换完成之后，由空压***打开所述第一炉体下端出料口的真空阀门，将物料通入第一加热室，并在物料全部落入所述第一加热室后关闭真空阀门；所述第一加热室为负压加热室，将物料加热至500℃、同时抽真空至1000Pa；Step 2: After the oxygen replacement of the first furnace body is completed, the vacuum valve of the discharge port at the lower end of the first furnace body is opened by the air pressure system, and the materials are passed into the first heating chamber, and when all the materials fall into the After the first heating chamber is described, the vacuum valve is closed; the first heating chamber is a negative pressure heating chamber, and the material is heated to 500 ° C and vacuumed to 1000 Pa at the same time;
步骤三：控制***检测到所述第一加热室达到500℃，并且所述真空***检测到所述第一加热室的压力到达1000Pa后，由所述空压***控制所述第一加热室的真空阀门打开，使所述第一加热室中的物料落入所述第二加热室，所述第二加热室为真空加热提纯室，将物料加热至2000℃、同时抽真空至3Pa，保温120min；Step 3: After the control system detects that the first heating chamber reaches 500°C, and the vacuum system detects that the pressure of the first heating chamber reaches 1000Pa, the air pressure system controls the temperature of the first heating chamber Open the vacuum valve so that the material in the first heating chamber falls into the second heating chamber, the second heating chamber is a vacuum heating purification chamber, heat the material to 2000 ° C, and at the same time evacuate to 3Pa, and keep it warm for 120min ;
步骤四：所述步骤三完成后，由所述空压***控制所述第二加热室的真空阀门打开，使所述第二加热室中的物料落入所述第一冷却室，所述第一冷却室为降温下料室，并且所述第一冷却室通过风冷降温，使物料降温至500℃；Step 4: After Step 3 is completed, the vacuum valve of the second heating chamber is controlled by the air pressure system to open, so that the materials in the second heating chamber fall into the first cooling chamber, and the second heating chamber The first cooling chamber is a cooling and feeding chamber, and the first cooling chamber is cooled by air to cool the material to 500°C;
步骤五，所述步骤四完成后，由所述空压***控制所述第一冷却室的真空阀门打开，使所述第一冷却室中的物料落入第二冷却室，并在物料完全下落后关闭真空阀门，将所述第二冷却室的置换气体入口打开，通过所述置换气体入口补充冷氮气或氩气，使所述第二冷却室内的炉膛压力恢复至大气压，同时使碳纳米管冷却至400℃以下。Step five, after the step four is completed, the vacuum valve of the first cooling chamber is controlled by the air pressure system to open, so that the materials in the first cooling chamber fall into the second cooling chamber, and when the materials are completely Close the vacuum valve behind, open the replacement gas inlet of the second cooling chamber, supplement cold nitrogen or argon through the replacement gas inlet, and restore the furnace pressure in the second cooling chamber to atmospheric pressure, and simultaneously make the carbon nanotubes Cool to below 400°C.
本发明有益效果是：The beneficial effects of the present invention are:
通过多级锥形真空炉连续下料，对碳纳米管进行加热和抽真空处理，解决了卧式真空炉不同位置纯度有明显差异、处理效率低、能耗高(技术问题，针对于背景技术中现有技术的缺点)，达到了单位设备的处理量提升50％、用电能耗降低20％、品质稳定性也得到改善。The carbon nanotubes are heated and evacuated through continuous feeding in a multi-stage conical vacuum furnace, which solves the obvious differences in purity at different positions of the horizontal vacuum furnace, low processing efficiency, and high energy consumption (technical problems, for the background technology The disadvantages of the existing technology in the present invention), the processing capacity of the unit equipment has been increased by 50%, the power consumption has been reduced by 20%, and the quality stability has also been improved.
附图说明Description of drawings
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings that need to be used in the description of the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For those skilled in the art, other drawings can also be obtained based on these drawings without creative effort.
图1为根据本发明的装置的总体结构示意图；Fig. 1 is the overall structure schematic diagram of device according to the present invention;
图2为根据本发明的提纯方法的具体流程示意图；Fig. 2 is the specific schematic flow sheet of purification method according to the present invention;
其中，1.第一炉体；2.第一加热室；3.第二加热室；4.第一冷却室；5.第二冷却室；6.真空***；7.冷凝过滤***；8.充放气***；9.真空***；10.控制***。Among them, 1. The first furnace body; 2. The first heating chamber; 3. The second heating chamber; 4. The first cooling chamber; 5. The second cooling chamber; 6. Vacuum system; 7. Condensation filtration system; 8. Inflatable and deflated system; 9. Vacuum system; 10. Control system.
具体实施方式Detailed ways
为使本发明的目的、技术方案和优点更加清楚，下面将结合附图对本发明实施方式作进一步地详细描述。In order to make the purpose, technical solution and advantages of the present invention clearer, the following will further describe in detail the embodiments of the present invention in conjunction with the accompanying drawings.
实施例一：Embodiment one:
本实施例提供一种用于碳纳米管提纯的装置，参见图1，所述装置包括：根据本发明提供的一种用于碳纳米管提纯的装置，包括：第一炉体1、加热室、冷却室、真空***6、充放气***8、空压***9以及控制***10；其中，第一炉体1用于临时存储物料，所述第一炉体1与所述加热室、所述冷却室依次通过管道连接，并且在所述第一炉体1与所述加热室、所述冷却室的物料出口分别设置有真空阀门；所述真空***分别连接至所述第一炉体与所述加热室，用于为所述第一炉体和所述加热室抽真空；所述充放气***分别连接至所述第一炉体和所述冷却室的置换气体入口，用于为所述第一炉体与所述冷却室提供置换气体；所述空压***用于为所述真空阀门提供动力，所述控制***与其他***电性连接，用于对所述装置进行控制。This embodiment provides a device for purifying carbon nanotubes, referring to Fig. 1, the device includes: a device for purifying carbon nanotubes according to the present invention, including: a first furnace body 1, a heating chamber , cooling chamber, vacuum system 6, inflation and deflation system 8, air pressure system 9 and control system 10; wherein, the first furnace body 1 is used for temporary storage of materials, the first furnace body 1 is connected with the heating chamber, the The cooling chambers are sequentially connected by pipelines, and vacuum valves are respectively provided at the material outlets of the first furnace body 1 and the heating chamber and the cooling chamber; the vacuum system is respectively connected to the first furnace body and the first furnace body. The heating chamber is used to evacuate the first furnace body and the heating chamber; the inflation and deflation system is respectively connected to the replacement gas inlets of the first furnace body and the cooling chamber, and is used for The first furnace body and the cooling chamber provide replacement gas; the air pressure system is used to provide power for the vacuum valve, and the control system is electrically connected to other systems for controlling the device.
在一种实施方式中，所述加热室和所述冷却室能够设置为多个，每个加热室均连接至所述真空***，并且每个加热室中分别设置有加热单元。In one embodiment, multiple heating chambers and cooling chambers can be provided, each heating chamber is connected to the vacuum system, and each heating chamber is respectively provided with a heating unit.
在一种实施方式中，所述第一炉体上设置有物料入口，并通过管道连接至进料储罐。In one embodiment, the first furnace body is provided with a material inlet, and is connected to a feed storage tank through a pipeline.
在一种实施方式中，所述第一炉体还设置有置换气体入口，以及真空排气口，所述置换气体入口通过管道连接至所述充放气***，所述真空排气口通过管道连接至所述真空***6，能够进行氧气置换；并且所述第一炉体1的下部的物料出口处设置有真空阀门，并通过管道连接至加热室。In one embodiment, the first furnace body is also provided with a replacement gas inlet and a vacuum exhaust port, the replacement gas inlet is connected to the inflation and deflation system through a pipeline, and the vacuum exhaust port is connected to the gas filling and deflation system through a pipeline Connected to the vacuum system 6, capable of oxygen replacement; and a vacuum valve is provided at the material outlet of the lower part of the first furnace body 1, and is connected to the heating chamber through a pipeline.
在一种实施方式中，将进料储罐中的碳纳米管通过管道导入第一炉体1中，并打开所述第一炉体的真空排气口和置换气体入口，在第一炉体中进行氧气置换，使其中含氧量低于50ppm。In one embodiment, the carbon nanotubes in the feed storage tank are introduced into the first furnace body 1 through pipelines, and the vacuum exhaust port and the replacement gas inlet of the first furnace body are opened. Oxygen replacement is carried out in the middle, so that the oxygen content in it is lower than 50ppm.
在一种实施方式中，所述加热室包括第一加热室2和第二加热室3，所述第一加热室2和所述第二加热室3均设置有真空排气口，所述真空排气口通过管道连接至真空***6，用于在所述第一加热室2和所述第二加热室3进行加热的过程中抽真空，以防止物料氧化。In one embodiment, the heating chamber includes a first heating chamber 2 and a second heating chamber 3, and both the first heating chamber 2 and the second heating chamber 3 are provided with a vacuum exhaust port, and the vacuum The exhaust port is connected to the vacuum system 6 through a pipeline, and is used for evacuating during the heating process of the first heating chamber 2 and the second heating chamber 3, so as to prevent oxidation of materials.
在一种实施方式中，所述第一加热室2为负压加热室，用于将碳纳米管物料加热至500℃、同时抽真空至1000Pa。In one embodiment, the first heating chamber 2 is a negative pressure heating chamber, which is used to heat the carbon nanotube material to 500° C. while evacuating to 1000 Pa.
在一种实施方式中，所述第二加热室3为真空加热提纯室，用于将物料加热至2000℃、同时抽真空至3Pa，并保温120min。In one embodiment, the second heating chamber 3 is a vacuum heating purification chamber, which is used to heat the material to 2000° C. while evacuating to 3 Pa, and keep it warm for 120 minutes.
所述冷却室也能够设置为多个；具体包括第一冷却室4和第二冷却室5，所述第一冷却室4为降温下料室，所述第二冷却室5为降温出料室。The cooling chamber can also be set to a plurality; specifically, it includes a first cooling chamber 4 and a second cooling chamber 5, the first cooling chamber 4 is a lowering chamber, and the second cooling chamber 5 is a cooling chamber .
在一种实施方式中，所述第一冷却室4通过风冷降温，使物料降温至500℃；具体地，可采用外部风机对其冷却降温。In one embodiment, the temperature of the first cooling chamber 4 is reduced by air cooling to reduce the temperature of the material to 500°C; specifically, an external fan can be used to cool it down.
在一种实施方式中，所述第二冷却室5也设置有置换气体入口，并且所述置换气体入口连接至充放气***8，充放气***8通过所述置换气体入口补充冷氮气或氩气，使所述第二冷却室5内的炉膛压力恢复至大气压，同时使其中的碳纳米管冷却至400℃以下，并在冷却完成后打开所述第二冷却室5的物料出口的真空阀门，将提纯后的碳纳米管通过物料输处管道输送至出料储罐中。In one embodiment, the second cooling chamber 5 is also provided with a replacement gas inlet, and the replacement gas inlet is connected to the inflation and deflation system 8, and the inflation and deflation system 8 supplements cold nitrogen or gas through the replacement gas inlet. argon to restore the furnace pressure in the second cooling chamber 5 to atmospheric pressure, and at the same time cool the carbon nanotubes therein to below 400°C, and open the vacuum at the material outlet of the second cooling chamber 5 after the cooling is completed. The valve transports the purified carbon nanotubes to the discharge storage tank through the material delivery pipeline.
在一种实施方式中，所述真空***6由滑阀泵、罗茨泵及管路阀门构成，对泵采用冗余选择，以达到快速抽起真空目的，所述真空***还能够采用真空测量单元对炉体的真空进行测量；并且所述真空***连接至冷凝过滤***7。In one embodiment, the vacuum system 6 is composed of a slide valve pump, a Roots pump, and pipeline valves. Redundant selection is used for the pumps to achieve the purpose of quickly pumping up the vacuum. The vacuum system can also use vacuum measurement The unit measures the vacuum of the furnace; and the vacuum system is connected to a condensate filtration system 7 .
在一种实施方式中，所述冷凝过滤***7是一种积储集、过滤、粗净化、精净化等多种功能于一体的冷凝过滤器收积罐。滤除炉内胶类、金属蒸汽及粉尘，能够极大提高真空泵使用寿命，特别适用粉尘、粘结剂含量多的场合。In one embodiment, the condensate filter system 7 is a condensate filter collection tank that integrates multiple functions such as storage, filtration, rough purification, and fine purification. Filter out glue, metal vapor and dust in the furnace, which can greatly improve the service life of the vacuum pump, especially suitable for occasions with a lot of dust and binder.
在一种实施方式中，所述充放气***8配置有Ar、N 2两组气体充入装置，用以进行空气置换，以实现各个炉体中载气定向气流排杂、快速冷却等目的。 In one embodiment, the charging and discharging system 8 is equipped with two sets of Ar and N gas charging devices for air replacement, so as to achieve the purpose of directional air flow of carrier gas in each furnace, rapid cooling, etc. .
在一种实施方式中，所述空压***9为气动组件，包括气源处理三联件，即过滤器、减压阀、油雾器三个部件；并且所述空压***9还包括压力表、电磁换向阀、气动接头、气动管路等；用于可对第一炉体、加热室、冷却室的真空阀门进行控制；图1作为示例，只示出了空压***9与所述第二冷却室5的真空阀门的连接；虽然图1中未示出，应理解为，所述空压***9通过常规的连接方式与所述第一炉体1、所述第一加热室2、所述第二加热室3、所述第一冷却室4及所述第一冷却室5的真空阀门连接。In one embodiment, the air pressure system 9 is a pneumatic assembly, including three components for air source treatment, namely a filter, a pressure reducing valve, and a lubricator; and the air pressure system 9 also includes a pressure gauge , electromagnetic reversing valve, pneumatic joint, pneumatic pipeline, etc.; used to control the vacuum valves of the first furnace body, heating chamber, and cooling chamber; Fig. 1 is an example, only shows the air pressure system 9 and the The connection of the vacuum valve of the second cooling chamber 5; although it is not shown in Fig. 1, it should be understood that the air pressure system 9 is connected with the first furnace body 1 and the first heating chamber 2 through a conventional connection mode. , the vacuum valves of the second heating chamber 3 , the first cooling chamber 4 and the first cooling chamber 5 are connected.
在一种实施方式中，所述控制***10以智能化温控仪、可控硅电压调整器、低压变压器为核心，构成包括供电、控制、监视、报警保护功能在内的电控***。智能化温控仪包括温度测量和控制元件，并且温度执行元件采用连续非通断式可控硅调压器，其在控制时不是传统的电气通断式，而是根据温控要求连续自动调节加热功率；对温度控制精度高，无噪音，对内部电网无干扰。In one embodiment, the control system 10 takes an intelligent temperature controller, a thyristor voltage regulator, and a low-voltage transformer as the core to form an electric control system including power supply, control, monitoring, and alarm protection functions. The intelligent temperature controller includes temperature measurement and control elements, and the temperature actuator adopts a continuous non-on-off thyristor voltage regulator, which is not a traditional electrical on-off type in control, but is continuously and automatically adjusted according to temperature control requirements. Heating power; high precision temperature control, no noise, no interference to the internal power grid.
在一种实施方式中，温度控制元件采用日本岛电(SHIMADEN)品牌\英国欧陆品牌数显智能化温控仪，控制精度±0.1％，可根据用户要求设定的工艺曲线，并存储多条温度工艺曲线，多组PID参数，以及PID自整定功能，有效的防止温度过冲，并具有自动+手动控制功能，连续自动控制加热功率。In one embodiment, the temperature control element adopts the digital display intelligent temperature controller of Japan's Shimaden (SHIMADEN) brand\UK Continental brand, with a control accuracy of ±0.1%. The process curve can be set according to user requirements, and multiple records can be stored. Temperature process curve, multiple sets of PID parameters, and PID self-tuning function can effectively prevent temperature overshoot, and has automatic + manual control function, continuous automatic control of heating power.
在一种实施方式中，温度测量元件采用热电偶以及双色红外的方式对各个炉体进行实时温度测量。并且隔热屏外设置一支PT100(0～500℃)热电偶监测炉壳温度，确保运行安全。In one embodiment, the temperature measuring element uses thermocouples and two-color infrared to measure the temperature of each furnace body in real time. And a PT100 (0-500°C) thermocouple is set outside the heat shield to monitor the temperature of the furnace shell to ensure safe operation.
在一种实施方式中，所述真空***的真空测量单元采用二路数显电阻真空测量仪，其具有相当宽的测量范围(105～10-1Pa)，可对真空***实现全程连续真空测量和控制。In one embodiment, the vacuum measurement unit of the vacuum system adopts a two-way digital display resistance vacuum measuring instrument, which has a relatively wide measurement range (105 ~ 10-1Pa), and can realize the whole process of continuous vacuum measurement and measurement of the vacuum system. control.
根据本发明的装置，还配置有一套包括进水分配管和开放式出水斗的水冷***。在所述装置工作之前，对第一炉体、加热室及冷却室的炉门、炉壳、电极、真空机组等进行通水冷却。According to the device of the present invention, a set of water cooling system including water inlet distribution pipe and open water outlet bucket is also configured. Before the device works, the first furnace body, furnace doors, furnace shells, electrodes, vacuum units, etc. of the heating chamber and cooling chamber are cooled by passing water.
在一种实施方式中，每路冷却水都有手动阀门，可以按需要调节流量大小；并且进水管上设有电接点压力表，当水压低于设定值时，控制***会声、光报警，同时电极水路还设有水温开关，超温或水压过低时都会自动切断加热器电源。所述水冷***还配置有备用水接口，用于紧急停电时打开备用水源。In one embodiment, each channel of cooling water has a manual valve, which can adjust the flow rate as required; and the water inlet pipe is equipped with an electric contact pressure gauge. When the water pressure is lower than the set value, the control system will give an audible and visual alarm. , At the same time, the electrode water circuit is also equipped with a water temperature switch, which will automatically cut off the power supply of the heater when the temperature is too high or the water pressure is too low. The water cooling system is also equipped with a backup water interface, which is used to open the backup water source in case of emergency power failure.
在一种实施方式中，所述第一炉体1为立式圆锥体结构，由双层钢板卷筒后焊接而成，夹层内设有冷却水导流隔板，能够确保冷却水均匀的冷却炉体各个部位，不会出现局部过热， 烧坏部件等现象；并且筒体两端与法兰焊接，炉体内壁为SUS304耐热不锈钢制造，外壁为Q235A碳素钢制造。In one embodiment, the first furnace body 1 is a vertical conical structure, which is welded by double-layer steel plate rolls, and a cooling water diversion plate is arranged in the interlayer to ensure uniform cooling of the cooling water. All parts of the furnace body will not be overheated or burned out; and both ends of the cylinder are welded with flanges. The inner wall of the furnace is made of SUS304 heat-resistant stainless steel, and the outer wall is made of Q235A carbon steel.
在一种实施方式中，所述第一加热室2和第二加热室3的炉体上还设置有电极引入装置，泄压防爆装置，并且开设有热电偶测温孔、设备吊卸环等；炉门采用双开门，炉门由内外封头和法兰焊成，内封头为SUS304耐热不锈钢，外封头为Q235A碳素钢，中间可通水冷却炉盖；炉门上还设有快冷风门；炉门开启采用齿圈锁紧快开门结构，锁紧炉门的齿圈由气缸驱动旋转，炉壳法兰上装有真空密封圈，关紧炉门即可抽真空。In one embodiment, the furnace bodies of the first heating chamber 2 and the second heating chamber 3 are also provided with electrode introduction devices, pressure relief and explosion-proof devices, and thermocouple temperature measuring holes, equipment lifting and unloading rings, etc. The furnace door adopts double doors, the furnace door is welded by inner and outer heads and flanges, the inner head is SUS304 heat-resistant stainless steel, the outer head is Q235A carbon steel, and water can be passed through the middle to cool the furnace cover; There is a quick cooling air door; the furnace door is opened with a ring gear locking quick door structure. The gear ring that locks the furnace door is driven by a cylinder to rotate. The flange of the furnace shell is equipped with a vacuum seal ring, and the furnace door can be vacuumed when the furnace door is closed tightly.
在一种实施方式中，所述加热室为锥形结构，骨架由耐热不锈钢和型钢组焊成，内部设置有碳纤维毡作为保温隔热层，加热单元的加热体可采用特种石墨；在一种替代方案中，所述加热单元还可采用电加热丝，并且加热单元能够通过所述加热室炉体上设置的开口连接至外部，并且电连接设置完成之后，对上述开口进行密封。In one embodiment, the heating chamber has a conical structure, the skeleton is welded by heat-resistant stainless steel and section steel, and carbon fiber felt is arranged inside as a thermal insulation layer, and the heating body of the heating unit can use special graphite; In an alternative solution, the heating unit can also use an electric heating wire, and the heating unit can be connected to the outside through an opening provided on the furnace body of the heating chamber, and after the electrical connection is set, the above opening is sealed.
在一种实施方式中，进一步地，所述加热单元电连接至所述控制***，由所述控制***提供电力，使所述加热单元对所述加热室进行加热。In one embodiment, further, the heating unit is electrically connected to the control system, and the control system provides power to enable the heating unit to heat the heating chamber.
在一种实施方式中，所述第一冷却室和所述第二冷却室能够采用与所述第一炉体同样构造的炉体。In one embodiment, the first cooling chamber and the second cooling chamber can adopt a furnace body with the same structure as the first furnace body.
实施例二Embodiment two
本实施例提供一种用于碳纳米管提纯的方法，所述方法采用本发明实施例一的提纯装置，结合图1及图2所示，所述方法具体包括如下步骤：This embodiment provides a method for purifying carbon nanotubes. The method adopts the purification device of Embodiment 1 of the present invention, as shown in FIG. 1 and FIG. 2 , and the method specifically includes the following steps:
步骤一：将进料储罐中的碳纳米管通过物料输送管道导入第一炉体中，并关闭物料输送管道，打开所述第一炉体的真空排气口和置换气体入口，由充放气***向所述第一炉体中通入氮气或氩气，并由真空***将所述第一炉体中的气体抽出，从而在第一炉体中进行氧气置换，使其中含氧量低于50ppm；Step 1: Import the carbon nanotubes in the feed storage tank into the first furnace body through the material delivery pipeline, close the material delivery pipeline, open the vacuum exhaust port and the replacement gas inlet of the first furnace body, and charge and discharge The gas system feeds nitrogen or argon into the first furnace body, and the gas in the first furnace body is pumped out by the vacuum system, so as to perform oxygen replacement in the first furnace body, so that the oxygen content in it is low at 50ppm;
步骤二：所述第一炉体进行氧气置换完成之后，由空压***打开所述第一炉体下端出料口的真空阀门，将物料通入第一加热室，并在物料全部落入所述第一加热室后关闭真空阀门；所述第一加热室为负压加热室，将物料加热至500℃、同时抽真空至1000Pa；Step 2: After the oxygen replacement of the first furnace body is completed, the vacuum valve of the discharge port at the lower end of the first furnace body is opened by the air pressure system, and the materials are passed into the first heating chamber, and when all the materials fall into the After the first heating chamber is described, the vacuum valve is closed; the first heating chamber is a negative pressure heating chamber, and the material is heated to 500 ° C and vacuumed to 1000 Pa at the same time;
步骤三：控制***检测到所述第一加热室达到500℃，并且所述真空***检测到所述第一加热室的压力到达1000Pa后，由所述空压***控制所述第一加热室的真空阀门打开，使所述第一加热室中的物料落入所述第二加热室，所述第二加热室为真空加热提纯室，将物料加热至2000℃、同时抽真空至3Pa，保温120min；Step 3: After the control system detects that the first heating chamber reaches 500°C, and the vacuum system detects that the pressure of the first heating chamber reaches 1000Pa, the air pressure system controls the temperature of the first heating chamber Open the vacuum valve so that the material in the first heating chamber falls into the second heating chamber, the second heating chamber is a vacuum heating purification chamber, heat the material to 2000 ° C, and at the same time evacuate to 3Pa, and keep it warm for 120min ;
步骤四：所述步骤三完成后，由所述空压***控制所述第二加热室的真空阀门打开，使所述第二加热室中的物料落入所述第一冷却室，所述第一冷却室为降温下料室，并且所述第一冷却室通过风冷降温，使物料降温至500℃；Step 4: After Step 3 is completed, the vacuum valve of the second heating chamber is controlled by the air pressure system to open, so that the materials in the second heating chamber fall into the first cooling chamber, and the second heating chamber The first cooling chamber is a cooling and feeding chamber, and the first cooling chamber is cooled by air to cool the material to 500°C;
步骤五，所述步骤四完成后，由所述空压***控制所述第一冷却室的真空阀门打开，使所述第一冷却室中的物料落入第二冷却室，并在物料完全下落后关闭真空阀门，将所述第二冷却室的置换气体入口打开，通过所述置换气体入口补充冷氮气或氩气，使所述第二冷却室内的炉膛压力恢复至大气压，同时使碳纳米管冷却至400℃以下。Step five, after the step four is completed, the vacuum valve of the first cooling chamber is controlled by the air pressure system to open, so that the materials in the first cooling chamber fall into the second cooling chamber, and when the materials are completely Close the vacuum valve behind, open the replacement gas inlet of the second cooling chamber, supplement cold nitrogen or argon through the replacement gas inlet, and restore the furnace pressure in the second cooling chamber to atmospheric pressure, and simultaneously make the carbon nanotubes Cool to below 400°C.
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection of the present invention. within range.

Claims (10)

  1. 一种用于碳纳米管提纯的装置，其特征在于，所述装置包括：第一炉体、加热室、冷却室、真空***、充放气***、空压***以及控制***；其中，所述第一炉体用于临时存储物料，所述第一炉体与所述加热室、所述冷却室依次通过管道连接，并且在所述第一炉体及所述加热室、所述冷却室的物料出口分别设置有真空阀门；所述真空***分别连接至所述第一炉体与所述加热室，用于为所述第一炉体和所述加热室抽真空；所述充放气***分别连接至所述第一炉体和所述冷却室的置换气体入口，用于为所述第一炉体与所述冷却室提供置换气体；所述空压***用于为所述真空阀门提供动力，所述控制***与其他***电性连接，用于对所述装置进行控制。A device for purifying carbon nanotubes, characterized in that the device includes: a first furnace body, a heating chamber, a cooling chamber, a vacuum system, a gas filling and deflation system, an air pressure system, and a control system; wherein, the The first furnace body is used for temporary storage of materials, the first furnace body is connected with the heating chamber and the cooling chamber through pipelines in turn, and between the first furnace body and the heating chamber and the cooling chamber The material outlets are respectively provided with vacuum valves; the vacuum system is respectively connected to the first furnace body and the heating chamber for vacuumizing the first furnace body and the heating chamber; the charging and deflation system The replacement gas inlets respectively connected to the first furnace body and the cooling chamber are used to provide replacement gas for the first furnace body and the cooling chamber; the air pressure system is used to provide the vacuum valve Power, the control system is electrically connected with other systems for controlling the device.
  2. 根据权利要求1所述的装置，其特征在于，所述加热室和所述冷却室能够设置为多个，并且每个加热室均通过管道连接至所述真空***，每个加热室中分别设置有加热单元。The device according to claim 1, characterized in that the heating chamber and the cooling chamber can be set in multiples, and each heating chamber is connected to the vacuum system through a pipeline, and each heating chamber is respectively set There is a heating unit.
  3. 根据权利要求1所述的装置，其特征在于，所述第一炉体上设置有物料入口，并通过管道连接至进料储罐，并且所述冷却室的物料出口通过管道连接至出料储罐。The device according to claim 1, wherein the first furnace body is provided with a material inlet, and is connected to the feed storage tank through a pipeline, and the material outlet of the cooling chamber is connected to the discharge storage tank through a pipeline. Can.
  4. 根据权利要求3所述的装置，其特征在于，所述第一炉体还设置有置换气体入口，以及真空排气口；所述置换气体入口通过管道连接至所述充放气***，所述真空排气口通过管道连接至所述真空***，能够对所述第一炉体进行氧气置换；当所述进料储罐中的碳纳米管通过管道导入所述第一炉体后，打开所述第一炉体的真空排气口和置换气体入口，在第一炉体中进行氧气置换，能够使其中含氧量低于50ppm。The device according to claim 3, wherein the first furnace body is also provided with a replacement gas inlet and a vacuum exhaust port; the replacement gas inlet is connected to the inflation and deflation system through a pipeline, and the The vacuum exhaust port is connected to the vacuum system through a pipeline, which can replace the first furnace body with oxygen; when the carbon nanotubes in the feed storage tank are introduced into the first furnace body through a pipeline, open the The vacuum exhaust port and the replacement gas inlet of the first furnace body are replaced by oxygen in the first furnace body, so that the oxygen content therein can be lower than 50ppm.
  5. 根据权利要求1所述的装置，其特征在于，所述加热室包括第一加热室和第二加热室，所述第一加热室和所述第二加热室均设置有真空排气口，所述真空排气口连接至真空***，用于在所述第一加热室和所述第二加热室进行加热的过程中抽真空，以防止物料氧化。The device according to claim 1, wherein the heating chamber comprises a first heating chamber and a second heating chamber, and both the first heating chamber and the second heating chamber are provided with a vacuum exhaust port, so The vacuum exhaust port is connected to a vacuum system for evacuating during the heating process of the first heating chamber and the second heating chamber to prevent oxidation of materials.
  6. 根据权利要求1所述的装置，其特征在于，所述第一加热室为负压加热室，用于将碳纳米管物料加热至500℃、同时抽真空至1000Pa；所述第二加热室为真空加热提纯室，用于将物料加热至2000℃、同时抽真空至3Pa，并保温120min。The device according to claim 1, wherein the first heating chamber is a negative pressure heating chamber for heating the carbon nanotube material to 500° C. while evacuating to 1000 Pa; the second heating chamber is The vacuum heating purification chamber is used to heat the material to 2000°C while evacuating to 3Pa and keeping it warm for 120min.
  7. 根据权利要求1所述的装置，其特征在于，所述冷却室也能够设置为多个；具体包括第一冷却室和第二冷却室，所述第一冷却室为降温下料室，所述第二冷却室为降温出料室。The device according to claim 1, characterized in that, the cooling chamber can also be set to a plurality; specifically comprising a first cooling chamber and a second cooling chamber, the first cooling chamber is a cooling chamber, the The second cooling chamber is the cooling discharge chamber.
  8. 根据权利要求1所述的装置，其特征在于，所述第一冷却室通过风冷降温，能够使物料降温至500℃。The device according to claim 1, characterized in that the temperature of the first cooling chamber can be reduced to 500° C. by air cooling.
  9. 根据权利要求1所述的装置，其特征在于，所述第二冷却室能够设置置换气体入口，并通过所述置换气体入口补充冷氮气或氩气，能够使所述第二冷却室内的炉膛压力恢复至大气压，同时使碳纳米管冷却至400℃以下，并在冷却完成后打开物料出口的阀门，将提纯后的碳纳米管输送至出料储罐中。The device according to claim 1, wherein the second cooling chamber can be provided with a replacement gas inlet, and cold nitrogen or argon can be supplemented through the replacement gas inlet to make the furnace pressure in the second cooling chamber Return to the atmospheric pressure, while cooling the carbon nanotubes to below 400°C, and open the valve of the material outlet after the cooling is completed, and transport the purified carbon nanotubes to the discharge storage tank.
  10. 一种用于碳纳米管提纯的方法，所述方法采用如权利要求1-9的任一项所述的一种用于碳纳米管提纯的装置，所述方法包括如下步骤：A method for purifying carbon nanotubes, said method adopts a device for purifying carbon nanotubes as described in any one of claims 1-9, said method comprising the steps of:
    步骤一：将进料储罐中的碳纳米管通过物料输送管道导入第一炉体中，并关闭物料输送管道，打开所述第一炉体的真空排气口和置换气体入口，由充放气***向所述第一炉体中通入氮气或氩气，并由真空***将所述第一炉体中的气体抽出，从而在第一炉体中进行氧气置换，使其中含氧量低于50ppm；Step 1: Import the carbon nanotubes in the feed storage tank into the first furnace body through the material delivery pipeline, close the material delivery pipeline, open the vacuum exhaust port and the replacement gas inlet of the first furnace body, and charge and discharge The gas system feeds nitrogen or argon into the first furnace body, and the gas in the first furnace body is pumped out by the vacuum system, so as to perform oxygen replacement in the first furnace body, so that the oxygen content in it is low at 50ppm;
    步骤二：所述第一炉体进行氧气置换完成之后，由空压***打开所述第一炉体下端出料口的真空阀门，将物料通入第一加热室，并在物料全部落入所述第一加热室后关闭真空阀门；所述第一加热室为负压加热室，将物料加热至500℃、同时抽真空至1000Pa；Step 2: After the oxygen replacement of the first furnace body is completed, the vacuum valve of the discharge port at the lower end of the first furnace body is opened by the air pressure system, and the materials are passed into the first heating chamber, and when all the materials fall into the After the first heating chamber is described, the vacuum valve is closed; the first heating chamber is a negative pressure heating chamber, and the material is heated to 500 ° C and vacuumed to 1000 Pa at the same time;
    步骤三：控制***检测到所述第一加热室达到500℃，并且所述真空***检测到所述第一加热室的压力到达1000Pa后，由所述空压***控制所述第一加热室的真空阀门打开，使所述第一加热室中的物料落入所述第二加热室，所述第二加热室为真空加热提纯室，将物料加热至2000℃、同时抽真空至3Pa，保温120min；Step 3: After the control system detects that the first heating chamber reaches 500°C, and the vacuum system detects that the pressure of the first heating chamber reaches 1000Pa, the air pressure system controls the temperature of the first heating chamber Open the vacuum valve so that the material in the first heating chamber falls into the second heating chamber, the second heating chamber is a vacuum heating purification chamber, heat the material to 2000 ° C, and at the same time evacuate to 3Pa, and keep it warm for 120min ;
    步骤四：所述步骤三完成后，由所述空压***控制所述第二加热室的真空阀门打开，使所述第二加热室中的物料落入所述第一冷却室，所述第一冷却室为降温下料室，并且所述第一冷却室通过风冷降温，使物料降温至500℃；Step 4: After Step 3 is completed, the vacuum valve of the second heating chamber is controlled by the air pressure system to open, so that the materials in the second heating chamber fall into the first cooling chamber, and the second heating chamber The first cooling chamber is a cooling and feeding chamber, and the first cooling chamber is cooled by air to cool the material to 500°C;
    步骤五，所述步骤四完成后，由所述空压***控制所述第一冷却室的真空阀门打开，使所述第一冷却室中的物料落入第二冷却室，并在物料完全下落后关闭真空阀门，将所述第二冷却室的置换气体入口打开，通过所述置换气体入口补充冷氮气或氩气，使所述第二冷却室内的炉膛压力恢复至大气压，同时使碳纳米管冷却至400℃以下。Step five, after the step four is completed, the vacuum valve of the first cooling chamber is controlled by the air pressure system to open, so that the materials in the first cooling chamber fall into the second cooling chamber, and when the materials are completely Close the vacuum valve behind, open the replacement gas inlet of the second cooling chamber, supplement cold nitrogen or argon through the replacement gas inlet, and restore the furnace pressure in the second cooling chamber to atmospheric pressure, and simultaneously make the carbon nanotubes Cool to below 400°C.
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