WO2021023179A1 - Device and method for preparing fullerene using compressive arc - Google Patents

Device and method for preparing fullerene using compressive arc Download PDF

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Publication number
WO2021023179A1
WO2021023179A1 PCT/CN2020/106772 CN2020106772W WO2021023179A1 WO 2021023179 A1 WO2021023179 A1 WO 2021023179A1 CN 2020106772 W CN2020106772 W CN 2020106772W WO 2021023179 A1 WO2021023179 A1 WO 2021023179A1
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arc
electrode
reaction chamber
gas
inert gas
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PCT/CN2020/106772
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French (fr)
Chinese (zh)
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纪崇甲
王兴立
李东岳
高树国
徐峰
姚文辉
李前胜
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北京三弧创科技术有限公司
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Priority claimed from CN201921258513.7U external-priority patent/CN210505592U/en
Priority claimed from CN201910716764.3A external-priority patent/CN110294468A/en
Application filed by 北京三弧创科技术有限公司 filed Critical 北京三弧创科技术有限公司
Publication of WO2021023179A1 publication Critical patent/WO2021023179A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • 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
    • C01B32/152—Fullerenes
    • C01B32/154—Preparation

Definitions

  • the present disclosure relates to the technical field of carbon nanomaterial preparation, in particular to a device for preparing fullerenes using a compressed arc, and a method for preparing fullerenes using the device.
  • the free arc method is generally used to prepare carbon nanomaterials and fullerenes.
  • the working conditions of the free arc method include: the distance between two carbon rods is about 20mm, and the free arc is obtained under the action of slight negative pressure, helium atmosphere and gravitational field.
  • the voltage of the arc is about 40V, the power is about 4-10Kw, and the arc
  • the temperature is around 6000°C. Since the minimum vaporization temperature of graphite is about 5100°C, and the arc temperature just exceeds the minimum temperature condition required for vaporization of graphite, the cathode arc root and anode arc root produced are very unstable. Specifically, the arc root area of the anode is small, and the arc root always jumps on the end surface of the graphite electrode instantly.
  • the present disclosure relates to an apparatus for preparing fullerenes using a compressed arc.
  • the apparatus includes an arc reaction chamber for preparing fullerene-containing soot, and a cathode is provided inside the arc reaction chamber Electrode, anode electrode, power supply, electromagnet and water wall, among them,
  • the water-cooled wall is a cylindrical structure with a sandwich cavity, and the water-cooled wall is provided with a water inlet and a water outlet to communicate with the sandwich cavity, and the sandwich cavity is used to provide a cooling water circulation space for cooling water Absorb and take away the heat of reaction,
  • the cathode electrode and the anode electrode are arranged oppositely in the water-cooled wall with a certain distance between them,
  • the positive pole of the power source is connected to the anode electrode, and the negative pole of the power source is connected to the cathode electrode, and an arc can be generated between the cathode electrode and the anode electrode,
  • the electromagnet is an energized coil, and the energized coil is sleeved outside the water-cooled wall and located between the cathode electrode and the anode electrode, and is used to generate a magnetic field and the inert gas introduced to simultaneously compress the arc,
  • the arc reaction chamber is provided with an inert gas inlet, an inert gas outlet, and a collection port for generating a plasma arc.
  • the inert gas inlet and the inert gas outlet are used to introduce and export inert gas into and out of the arc reaction chamber, respectively.
  • the collection port is used to lead the reacted gas phase products from the arc reaction chamber.
  • the material of the cathode electrode is copper, which contains a tungsten-cerium electrode core.
  • the material of the anode electrode is graphite.
  • an insulating layer is provided outside the energized coil.
  • an electrode moving mechanism is also provided inside the arc reaction chamber for moving the anode electrode toward the cathode electrode.
  • the electrode moving mechanism may be a known spiral moving mechanism or Pneumatic moving mechanism.
  • the device further includes a cooling chamber, a filter chamber, and an exhaust gas processing unit connected to the arc reaction chamber in sequence, wherein:
  • the cooling bin is connected to the collection port of the arc reaction chamber, and is used to cool the gas phase products output from the arc reaction chamber, and input the cooled gas phase products into the filter bin,
  • the filter bin is used to filter out the solids in the gas-phase products, and input the gas-phase products without solids into the tail gas processing unit,
  • the tail gas processing unit is used to collect and purify the gas phase products output from the filter bin, and can be recycled.
  • the present disclosure relates to a method for preparing fullerenes, wherein the method uses the device of the present disclosure, and the method includes: passing an inert gas into the arc reaction chamber, and passing cooling into the water wall. The water discharges the cathode electrode and the anode electrode to generate a compression arc, and obtains fullerene-containing soot.
  • an organic solvent is added for thorough mixing, and the insoluble matter therein is removed to obtain a carbon nanomaterial containing fullerene.
  • the inert gas is a single helium gas, a single argon gas, or a mixed gas of helium and argon.
  • the power source used between the cathode electrode and the anode electrode is a direct current power source, the power source current is 100-500 amps, and the voltage is 10-400 volts.
  • the arc temperature generated during the discharge is 5000-20000°C, and the diameter of the arc column is 5-20 mm.
  • the present disclosure provides an apparatus for preparing fullerenes using a compressed arc, which compresses the arc by using an electromagnet and an inert gas passed in, so that the arc column is concentrated and controllable. Therefore, the gasification speed of the anode carbon rod is fast, which solves the shortcomings of the slow gasification speed of the current traditional method.
  • the present disclosure reduces the temperature of the sandwich cavity by using multiple air inlets for swirling air intake, so there is no need to use high-purity helium for heat exchange, which solves that traditional methods can only use high-purity helium.
  • helium, argon, or a mixture of two inert gases can be used in the present disclosure to produce fullerene-containing soot.
  • the generated soot particles can flow with the gas and deliver the product to the cooling chamber, which is more conducive to product collection.
  • the gas in the reaction chamber is static, so products can only be collected in the reaction chamber. Therefore, the present disclosure solves the problem that fullerene-containing soot can only be obtained by gasifying carbon rods in a static environment.
  • Figure 1 is a schematic diagram of a device for preparing fullerenes using a compressed arc.
  • Fig. 2 is a cross-sectional view of the main body of the arc generator.
  • Figure 3 is a cross-sectional view of the arc generating device (power supply).
  • Fig. 4 is a sectional view taken along the line A in Fig. 2.
  • Figure 5 is a schematic diagram of using an electromagnet to compress an arc.
  • Figure 6 is a chromatogram of the organic solvent in which the product is dissolved.
  • certain embodiments of the present disclosure relate to an apparatus for preparing fullerenes using a compressed arc.
  • the device includes an arc reaction chamber 1, and the function of the arc reaction chamber 1 is to prepare fullerene-containing soot.
  • a cathode electrode 11, an anode electrode 12, a power source 18, an electromagnet 13 and a water wall 14 are provided inside the arc reaction chamber.
  • the water wall 14 is a cylindrical structure with a sandwich cavity, and the water wall 14 is provided with water inlets and water outlets (not shown in the figure) to communicate with the sandwich cavity, and the number of water inlets and water outlets can be Greater than one.
  • the sandwich cavity is used to provide cooling water circulation space so that the cooling water absorbs and takes away the reaction heat and maintains the stable operation of the device.
  • the cathode electrode 11 and the anode electrode 12 are arranged oppositely in the water-cooled wall 14 with a certain distance between the two, which may be 10-45 mm.
  • the power supply 18 can be arranged inside or outside the arc reaction chamber.
  • the positive electrode of the power supply 18 is connected to the anode electrode 12 through a wire
  • the negative electrode of the power supply 18 is connected to the cathode electrode 11 through a wire, in the channel between the cathode electrode 11 and the anode electrode 12.
  • the high temperature zone generated by the arc 19 forms a large number of fullerene cages.
  • the fullerene cages formed in the high temperature zone can quickly leave the reaction zone and enter the subsequent cooling chamber 2, which is similar to the prior art Compared with the use of non-flowing inert gas in the medium arc reaction chamber, the yield and output of fullerene can be improved.
  • the electromagnet 13 is an energizing coil, and the energizing coil is sheathed outside the water wall 14 and located between the cathode electrode 11 and the anode electrode 12, and is used to generate a magnetic field to compress the arc 19.
  • Figure 5 is a schematic diagram of the use of electromagnets to compress the arc, that is, the Ampere’s rule in the energized solenoid (Ampere’s rule two): Hold the energized solenoid with your right hand and let the four fingers point in the direction of the current. The end pointed to is the N pole of the energized solenoid.
  • applying current to the energized coil generates a magnetic field, which can guide and compress the arc, and further control the shape and path of the arc 19 so that the arc 19 is located in the center of the channel.
  • the arc 19 is a plasma arc
  • the power of the arc 19 will not change after compression, but the shape of the arc 19 will change. Specifically, the arc column becomes thinner, and the energy per unit area is increased after being thinned.
  • the arc reaction chamber 1 is provided with an inert gas inlet 15, an inert gas outlet 16 and a collection port 17.
  • the inert gas inlet 15 and the inert gas outlet 16 are used to introduce and export inert gas into and out of the arc reaction chamber 1 to provide an inert atmosphere for the reaction.
  • the collection port 17 is used to lead the reacted gas phase product out of the arc reaction chamber 1, and the gas phase product needs to be cooled and collected later.
  • the material of the cathode electrode 11 is red copper, which contains a tungsten-cerium electrode core. Since copper has better thermal conductivity than other metals, using copper as the cathode electrode 11 can reduce the temperature of the cathode and has better electrical conductivity.
  • the material of the anode electrode 12 is graphite.
  • a carbon rod can be used as the anode electrode 12, which is vaporized to generate fullerene and other carbon nanomaterials during the arc reaction.
  • an insulating layer 131 is provided outside the energized coil to prevent the energy of the arc 19 from dispersing, resulting in double arcs or series arcs.
  • a loop is formed between the cathode electrode 11 and the anode electrode 12, and the flowing inert gas can form a gaseous insulating layer between the cathode electrode 11 and the anode electrode 12. Since the insulating layer formed by the inert gas is occasionally destroyed, double arcs or string arcs will occur during destruction.
  • the insulating layer 131 outside the energized coil is an insulating layer to prevent cold air, that is, when the aforementioned gaseous insulating layer is destroyed, the current flows from the cathode electrode 11 to the auxiliary anode 121 and then to the anode electrode 12 to form a current path. Adding an insulating layer 131 outside the energized coil can effectively prevent such situations from occurring.
  • the specific structure of the arc generating device is shown in Figure 2 and Figure 3.
  • the device is located inside the arc reaction chamber 1 and includes a cathode electrode 11, an auxiliary anode 121, an anode electrode 12 and a power source 18.
  • a water-cooled wall 14 is provided on the outer periphery of the cathode electrode 11, and there is a certain gap between the water-cooled wall 14 and the cathode electrode 11 to form an inert gas circulation space.
  • the water wall 14 is provided with a water inlet and a water outlet, and the water wall 14 has a cooling water circulation space inside.
  • a cathode cooling water inlet 141 and a cathode cooling water outlet 142 are provided outside the cathode electrode 11, and an auxiliary anode cooling water inlet 143 and an auxiliary anode cooling water outlet 144 are provided outside the auxiliary anode 121.
  • the inert gas inlet 15 can adopt the method shown in Fig.
  • each inert gas inlet 15 is a tangential inlet hole, which can make the inert gas swirl into the water cooling wall. In the gap between the wall 14 and the cathode electrode 11, the reaction heat is quickly taken away.
  • an electromagnet 13 is provided between the cathode electrode 11 and the anode electrode 12.
  • the auxiliary anode 121 is located in the gap between the water-cooled wall 14 and the cathode electrode 11 and extends toward the position of the electromagnet 13 until it enters the inner ring of the electromagnet 13.
  • An insulating layer 131 is provided on the side of the electromagnet 13 close to the anode electrode 12.
  • the negative electrode of the power source 18 is connected to the cathode electrode 11, and the positive electrode of the power source 18 is connected to the anode electrode 12 and the auxiliary anode 121, respectively.
  • An anode control switch K1 is provided on the connecting wire between the positive electrode of the power source 18 and the anode electrode 12, and an auxiliary anode control switch K2 is provided on the connecting wire between the anode of the power source 18 and the auxiliary anode 121.
  • the auxiliary anode control switch K2 When the arc generator needs to be started, the auxiliary anode control switch K2 is first closed, and the inert gas is introduced into the inert gas inlet 15 to form an inert gas protective gas film on the surface of the cathode electrode 11. The electrons emitted from the cathode electrode 11 fall on the auxiliary anode 121 to form an auxiliary arc.
  • the anode control switch K1 is closed, and the anode arc root is transferred to the anode electrode 12, forming a main arc between the cathode electrode 11 and the anode electrode 12.
  • the auxiliary anode control switch K2 is opened. The auxiliary arc is automatically extinguished.
  • the auxiliary arc is formed first, and then the arc is turned to form the main arc.
  • the arc 19 is turned from the cathode electrode 11 to the auxiliary anode 121 at the shortest distance, and then the arc is sent to the anode electrode 12 by the flowing inert gas, and then the auxiliary anode 121 is disconnected from the power supply to allow the cathode electrode 11 to reach the anode electrode.
  • a loop is formed between 12 and a main arc 19 is formed.
  • the flowing inert gas can form an insulating layer between the cathode electrode 11 and the anode electrode 12.
  • the insulating layer formed by the inert gas is occasionally destroyed, double arcs or series arcs will occur when destroyed, and the arc energy is dispersed and the power is reduced. Therefore, it is necessary to provide an insulating layer 131 outside the energized coil.
  • the present disclosure prevents double arcs from appearing in the following ways: (1) Provide an insulating layer 131 outside the energized coil; (2) Reduce the temperature of the auxiliary anode 121 cooling water to make the temperature of the inert gas as low as possible; (3) Increase the flow rate of the inert gas; (4) Set up multiple inert gas inlets 15 to allow the inert gas to swirl in.
  • an electrode moving mechanism (not shown in the figure) is also provided inside the arc reaction chamber 1.
  • the anode electrode 12 usually a carbon rod
  • the anode electrode 12 can be moved toward the cathode electrode 11 by operating the electrode moving mechanism, so that the cathode electrode 11 and the anode electrode 12 are maintained at an appropriate distance.
  • the electrode moving mechanism may be a well-known screw moving mechanism or a pneumatic moving mechanism, for example, an air cylinder is used to move the anode electrode 12 back and forth.
  • the device further includes a cooling bin 2, a filtering bin 3, and an exhaust gas processing unit 4 connected to the arc reaction chamber 1 in sequence.
  • the cooling bin 2 is connected to the collection port 17 of the arc reaction chamber 1, and is used to cool the gas phase products output from the arc reaction chamber 1 and input the cooled gas phase products into the filter bin 3; The solids are filtered out, and the gas phase products that do not contain solids are input to the tail gas processing unit 4; the tail gas treatment unit 4 is used to collect and purify the gas phase products output from the filter bin 3, and can be recycled.
  • the arc reaction chamber 1, the cooling chamber 2 and the filter chamber 3 all work under vacuum conditions. Specifically, since a filter bag is used to filter and collect fullerene-containing carbon nanoparticles, it is necessary to cool the gas phase product output from the arc reaction chamber 1 to a temperature acceptable to the filter bag.
  • the filtered soot is stored at the bottom of the filter bin 3, and a vacuum valve is installed at the bottom of the filter bin 3. When collecting, connect the collection container to the valve and open the valve directly to prevent the soot from coming into contact with the air and water vapor in the air.
  • the gas phase products that do not contain solids enter the tail gas processing unit 4 for collection and purification, and can be compressed for secondary use when the purity reaches 99.99% or 99.999%.
  • certain embodiments of the present disclosure also relate to a method for preparing fullerenes using the device, which includes: passing an inert gas into the arc reaction chamber 1 and passing cooling water into the water wall 12 to make the cathode electrode The discharge of 11 and the anode electrode 12 generates a compressed arc 19 to obtain fullerene-containing soot.
  • the soot is collected after cooling and filtering, and an organic solvent is added to the collection to mix thoroughly, and the insoluble matter is removed from the collection to obtain a carbon nanomaterial containing fullerene.
  • the organic solvent added can be toluene or o-xylene. If the product contains fullerenes, the organic solvent changes from colorless and transparent to wine red to black.
  • the inert gas is a single helium gas, a single argon gas, or a mixed gas of helium and argon. Since helium has a small molecular weight and can quickly enter the fullerene cage for cooling, the prior art usually uses a single helium gas. But helium is usually extracted from natural gas with a higher content. Although there are many natural gas fields, the number of gas fields that can produce helium does not tend to increase significantly. Since helium is difficult to be replaced by other gases, and the supply of helium has been in a limited state, if consumption continues at the current rate, helium will be exhausted after 25 years.
  • the swirling air intake can be used to enhance the cooling effect through gas flow. Therefore, a mixed inert gas can be used, and the ratio of helium to argon in the mixed gas introduced is not required, and only a small amount of helium is required. .
  • the power source 18 used between the cathode electrode 11 and the anode electrode 12 in the present disclosure is a direct current power source.
  • the DC power supply is a constant current power supply, which can provide current to generate an arc between the cathode electrode 11 and the anode electrode 12. Because it is a constant current power supply, the current is the set value, the voltage is the change value, and the voltage change changes with the change of the distance between the cathode electrode 11 and the anode electrode 12 and the change of the gas flow.
  • the power source 18 has a current of 100-500 amps and a voltage of 10-400 volts.
  • the reaction time of the carbon rod as the anode electrode 12 is determined by the current setting value and the gas flow value. The higher the current, the faster the gasification speed, the greater the gas flow, and the faster the gasification speed. However, it cannot blindly increase the reaction speed, and needs to be adjusted according to specific experimental conditions.
  • the arc temperature generated during the discharge is 5000-20000°C
  • the arc column diameter is 5-20 mm.
  • the arc column diameter is 8-9 mm.
  • the diameter of the arc column generated in the prior art is 2-3 mm, and the arc temperature is below 6000°C.
  • the arc column generated by the device provided by the present disclosure is thicker and controllable in size, and the temperature is also increased.
  • a graphite rod with a length of 300 mm and a diameter of 8 mm was consumed in about 40-60 minutes. With the device of the present disclosure, carbon rods of the same size can be consumed within 5-15 minutes, so the fullerene production can be significantly increased.
  • the cathode electrode 11 in the arc reaction chamber 1 is a copper electrode containing a tungsten-cerium core
  • the anode electrode 12 is a carbon rod, which is passed into the water wall 14 under an inert gas atmosphere (the volume ratio of helium and argon is 1:5) Cooling water is introduced to discharge the cathode electrode 11 and the anode electrode 12 to generate a compressed arc.
  • a DC power source 18 is used to supply power to the cathode electrode 11 and the anode electrode 12, the current of the power source 18 is 200 amps, and the voltage is 50-200 volts.
  • the cooling water temperature is 18-20°C.
  • the temperature of the arc 19 generated during the discharge is 5000-20000°C, and the diameter of the arc column is 8-9mm.
  • the gaseous product of the reaction is output from the arc reaction chamber 1, and is cooled by the cooling chamber 2 and collected by the filtering chamber 3 to obtain fullerene-containing soot.
  • Method fullerene means that the C82 ball cage contains a metal atom, such as Gd@C82.
  • the cathode electrode was replaced with a carbon rod, the current value was 400A, and the voltage value was 100V, and the others were the same as in Example 1.
  • the current value is 400A
  • the voltage value is increased to 170V (this is the voltage change caused by changing the inert gas, not actively changing the voltage), and the others are the same as in Embodiment 1.
  • the inert gas was replaced with a single argon gas, the current value was 400A, and the voltage value was 100V, and the others were the same as in Example 1.
  • Example 1 Example 2
  • Example 3 Example 4
  • Example 5 C60 yield (%) 8.35 7.46 8.21 8.30 6.15

Abstract

Disclosed a device for preparing fullerene using a compressive arc, wherein the device can increase the temperature and power of the arc by using an electromagnet (13) in an arc reaction chamber (1), and a fullerene carbon cluster may be obtained by the reaction. Disclosed also is a method for preparing fullerene by using the device, comprising vaporizing a carbon rod by using a plasma generator in the arc reaction chamber (1) to obtain a fullerene-containing soot, which is cooled, filtered and then collected. The device and the method address the problem of low fullerene yield and realize automatic collection in a vacuum environment to avoid contamination of air environment and damage to operator's health.

Description

使用压缩电弧制备富勒烯的装置及方法Apparatus and method for preparing fullerene using compressed arc
相关申请的引用References to related applications
本公开要求于20219年8月5日向中华人民共和国国家知识产权局提交的申请号为201910716764.3、发明名称为“使用压缩电弧制备富勒烯的装置及方法”的发明专利申请，以及于20219年8月5日向中华人民共和国国家知识产权局提交的申请号为201921258513.7、发明名称为“使用压缩电弧制备富勒烯的装置”的实用新型专利申请的全部权益，并通过引用的方式将其全部内容并入本文。This disclosure requires an invention patent application filed with the State Intellectual Property Office of the People’s Republic of China on August 5, 20219 with an application number of 201910716764.3 and an invention title of "Apparatus and method for preparing fullerene using compressed arc", and on August 5, 20219 All rights and interests of the utility model patent application filed with the State Intellectual Property Office of the People’s Republic of China with the application number 201921258513.7 and the invention title "Apparatus for preparing fullerenes using compressed arc" on the 5th, and incorporated the entire contents by reference Into this article.
领域field
本公开涉及碳纳米材料制备技术领域，具体涉及使用压缩电弧制备富勒烯的装置，以及使用该装置制备富勒烯的方法。The present disclosure relates to the technical field of carbon nanomaterial preparation, in particular to a device for preparing fullerenes using a compressed arc, and a method for preparing fullerenes using the device.
背景background
目前，人们已通过不同的方法获取能量，来制备包括富勒烯的碳纳米材料。这些方法包括：煤燃烧法、苯燃烧法、激光蒸发法、光束轰击法、离子注入法、化学通道法、电弧放电法、高温高压法以及核反应法。由于电弧放电法的操作简单，成本较低，目前人们普遍选用该方法。但是由于电弧放电法的功率较低，严重限制了富勒烯的产量。Currently, people have obtained energy through different methods to prepare carbon nanomaterials including fullerenes. These methods include: coal combustion method, benzene combustion method, laser evaporation method, beam bombardment method, ion implantation method, chemical channel method, arc discharge method, high temperature and high pressure method, and nuclear reaction method. Because of the simple operation and low cost of the arc discharge method, this method is currently widely used. However, the low power of the arc discharge method severely limits the production of fullerenes.
两个平行放置的石墨电极建立电弧通道以后，产生的电弧未受外界压缩，弧柱截面随着功率的增加而增加，弧柱中电流密度近乎常数，这种方式产生的电弧为自由电弧。目前通常采用自由电弧法制备碳纳米材料及富勒烯。After two parallel graphite electrodes establish an arc channel, the arc generated is not compressed by the outside, the arc column section increases with the increase of power, and the current density in the arc column is almost constant. The arc generated in this way is a free arc. Currently, the free arc method is generally used to prepare carbon nanomaterials and fullerenes.
自由电弧法工作条件包括：两个碳棒之间的距离为20mm左右，在微负压、氦气氛和重力场作用下得到自由电弧，电弧的电压为40V左右，功率在4-10Kw左右，电弧温度为6000℃左右。由于石墨的最低气化温度为5100℃左右，电弧温度刚超过气化石墨所需的最低温度条件，因此产生的阴极弧根和阳极弧根均很不稳定。具体表现在阳极 弧根区较小，弧根总是瞬间跳跃在石墨电极端面。由于气化碳棒过程总是选择电弧电阻最小的路径，因此反应过程中总是刻蚀离阴极和阳极最近的一点，石墨的气化率与石墨电极直径大小几乎无关，因此即使增加石墨电极的体积，也无法高效率地制备碳纳米材料及富勒烯。The working conditions of the free arc method include: the distance between two carbon rods is about 20mm, and the free arc is obtained under the action of slight negative pressure, helium atmosphere and gravitational field. The voltage of the arc is about 40V, the power is about 4-10Kw, and the arc The temperature is around 6000°C. Since the minimum vaporization temperature of graphite is about 5100°C, and the arc temperature just exceeds the minimum temperature condition required for vaporization of graphite, the cathode arc root and anode arc root produced are very unstable. Specifically, the arc root area of the anode is small, and the arc root always jumps on the end surface of the graphite electrode instantly. Since the carbon rod gasification process always chooses the path with the smallest arc resistance, the point closest to the cathode and anode is always etched during the reaction process. The gasification rate of graphite is almost independent of the diameter of the graphite electrode, so even if the graphite electrode is increased Because of its volume, carbon nanomaterials and fullerenes cannot be produced efficiently.
概述Overview
一方面，本公开涉及使用压缩电弧制备富勒烯的装置，所述装置包括电弧反应室，所述电弧反应室用于制备含有富勒烯的烟炱，在所述电弧反应室内部设有阴极电极、阳极电极、电源、电磁铁和水冷壁，其中，In one aspect, the present disclosure relates to an apparatus for preparing fullerenes using a compressed arc. The apparatus includes an arc reaction chamber for preparing fullerene-containing soot, and a cathode is provided inside the arc reaction chamber Electrode, anode electrode, power supply, electromagnet and water wall, among them,
所述水冷壁为一个具有夹层腔体的圆柱状结构，所述水冷壁上设有进水口和出水口与该夹层腔体相连通，所述夹层腔体用于提供冷却水循环空间以使冷却水吸收并带走反应热，The water-cooled wall is a cylindrical structure with a sandwich cavity, and the water-cooled wall is provided with a water inlet and a water outlet to communicate with the sandwich cavity, and the sandwich cavity is used to provide a cooling water circulation space for cooling water Absorb and take away the heat of reaction,
所述阴极电极和阳极电极相对设置于所述水冷壁内，两者之间具有一定距离，The cathode electrode and the anode electrode are arranged oppositely in the water-cooled wall with a certain distance between them,
所述电源的正极与阳极电极连接，所述电源的负极与阴极电极连接，在所述阴极电极和阳极电极之间可产生电弧，The positive pole of the power source is connected to the anode electrode, and the negative pole of the power source is connected to the cathode electrode, and an arc can be generated between the cathode electrode and the anode electrode,
所述电磁铁为通电线圈，所述通电线圈套于所述水冷壁外，并位于所述阴极电极和阳极电极之间，用于产生磁场与通入的惰性气体同时对电弧进行压缩，The electromagnet is an energized coil, and the energized coil is sleeved outside the water-cooled wall and located between the cathode electrode and the anode electrode, and is used to generate a magnetic field and the inert gas introduced to simultaneously compress the arc,
所述电弧反应室设有用于产生等离子体电弧的惰性气体进口、惰性气体出口和收集口，所述惰性气体进口和惰性气体出口分别用于向所述电弧反应室内导入和导出惰性气体，所述收集口用于将反应后的气相产物从所述电弧反应室中导出。The arc reaction chamber is provided with an inert gas inlet, an inert gas outlet, and a collection port for generating a plasma arc. The inert gas inlet and the inert gas outlet are used to introduce and export inert gas into and out of the arc reaction chamber, respectively. The collection port is used to lead the reacted gas phase products from the arc reaction chamber.
在某些实施方案中，所述阴极电极的材质为紫铜，其内部含有钨铈电极芯。In some embodiments, the material of the cathode electrode is copper, which contains a tungsten-cerium electrode core.
在某些实施方案中，所述阳极电极的材质为石墨。In some embodiments, the material of the anode electrode is graphite.
在某些实施方案中，在所述通电线圈外设有绝缘层。In some embodiments, an insulating layer is provided outside the energized coil.
在某些实施方案中，所述电弧反应室内部还设有电极移动机构，用于使所述阳极电极向所述阴极电极方向移动。当观察到所述阳极电 极由于气化而变短时，可通过操纵所述电极移动机构使所述阴极电极和所述阳极电极维持于一合适距离，电极移动机构可以为公知的螺旋移动机构或气动移动机构。In some embodiments, an electrode moving mechanism is also provided inside the arc reaction chamber for moving the anode electrode toward the cathode electrode. When it is observed that the anode electrode becomes shorter due to vaporization, the cathode electrode and the anode electrode can be maintained at an appropriate distance by manipulating the electrode moving mechanism. The electrode moving mechanism may be a known spiral moving mechanism or Pneumatic moving mechanism.
在某些实施方案中，所述装置还包括与电弧反应室依次连接的冷却仓、过滤仓和尾气处理单元，其中，In some embodiments, the device further includes a cooling chamber, a filter chamber, and an exhaust gas processing unit connected to the arc reaction chamber in sequence, wherein:
所述冷却仓与电弧反应室的收集口连接，用于冷却从所述电弧反应室输出的气相产物，并将冷却后的气相产物输入过滤仓，The cooling bin is connected to the collection port of the arc reaction chamber, and is used to cool the gas phase products output from the arc reaction chamber, and input the cooled gas phase products into the filter bin,
所述过滤仓用于将气相产物中的固体物过滤掉，并将不含有固体物的气相产物输入尾气处理单元，The filter bin is used to filter out the solids in the gas-phase products, and input the gas-phase products without solids into the tail gas processing unit,
所述尾气处理单元用于对从过滤仓输出的气相产物进行收集和纯化处理，可以进行循环使用。The tail gas processing unit is used to collect and purify the gas phase products output from the filter bin, and can be recycled.
另一方面，本公开涉及置制备富勒烯的方法，其中所述方法使用本公开的装置，所述方法包括：向所述电弧反应室内通入惰性气体，向所述水冷壁中通入冷却水，使阴极电极和阳极电极放电产生压缩电弧，得到含有富勒烯的烟炱。In another aspect, the present disclosure relates to a method for preparing fullerenes, wherein the method uses the device of the present disclosure, and the method includes: passing an inert gas into the arc reaction chamber, and passing cooling into the water wall. The water discharges the cathode electrode and the anode electrode to generate a compression arc, and obtains fullerene-containing soot.
在某些实施方案中，所述烟炱冷却后加入有机溶剂进行充分混合，除去其中的不溶物后，得到含有富勒烯的碳纳米材料。In some embodiments, after the soot is cooled, an organic solvent is added for thorough mixing, and the insoluble matter therein is removed to obtain a carbon nanomaterial containing fullerene.
在某些实施方案中，所述惰性气体为单一氦气、单一氩气，或者为氦气和氩气的混合气体。In some embodiments, the inert gas is a single helium gas, a single argon gas, or a mixed gas of helium and argon.
在某些实施方案中，在阴极电极和阳极电极之间使用的电源为直流电源，电源电流为100-500安，电压为10-400伏。In some embodiments, the power source used between the cathode electrode and the anode electrode is a direct current power source, the power source current is 100-500 amps, and the voltage is 10-400 volts.
在某些实施方案中，放电过程中产生的电弧温度为5000-20000℃，电弧柱直径为5-20mm。In some embodiments, the arc temperature generated during the discharge is 5000-20000°C, and the diameter of the arc column is 5-20 mm.
在某些实施方案中，本公开提供了使用压缩电弧制备富勒烯的装置，该装置通过使用电磁铁和通入的惰性气体对电弧进行压缩，使电弧柱集中且可控。因此气化阳极碳棒的速度快，解决了目前传统方法气化速度慢的缺点。In certain embodiments, the present disclosure provides an apparatus for preparing fullerenes using a compressed arc, which compresses the arc by using an electromagnet and an inert gas passed in, so that the arc column is concentrated and controllable. Therefore, the gasification speed of the anode carbon rod is fast, which solves the shortcomings of the slow gasification speed of the current traditional method.
在某些实施方案中，本公开通过使用多个进气口进行旋流进气，降低了夹层腔体的温度，因此无需使用高纯氦气换热，解决了传统方法只能使用高纯氦气才能制备出含有富勒烯的烟炱的问题。In some embodiments, the present disclosure reduces the temperature of the sandwich cavity by using multiple air inlets for swirling air intake, so there is no need to use high-purity helium for heat exchange, which solves that traditional methods can only use high-purity helium. The problem of producing soot containing fullerenes only by using gas.
在某些实施方案中，本公开中使用氦气、氩气或者两种惰性气体的混合都可制备出含有富勒烯的烟炱。In some embodiments, helium, argon, or a mixture of two inert gases can be used in the present disclosure to produce fullerene-containing soot.
在某些实施方案中，由于使用流动气体换热，可以使产生的烟炱颗粒随着气体流动，并将产物输送到冷却仓内，更有利于产物的收集。而现有技术中反应腔内的气体是静止的，所以只能在反应腔内收集产物。因此本公开解决了只能在静态环境下气化碳棒得到含有富勒烯的烟炱的问题。In some embodiments, due to the use of flowing gas for heat exchange, the generated soot particles can flow with the gas and deliver the product to the cooling chamber, which is more conducive to product collection. In the prior art, the gas in the reaction chamber is static, so products can only be collected in the reaction chamber. Therefore, the present disclosure solves the problem that fullerene-containing soot can only be obtained by gasifying carbon rods in a static environment.
附图简要说明Brief description of the drawings
图1为使用压缩电弧制备富勒烯装置的结构示意图。Figure 1 is a schematic diagram of a device for preparing fullerenes using a compressed arc.
图2为电弧发生装置主体的剖面图。Fig. 2 is a cross-sectional view of the main body of the arc generator.
图3为电弧发生装置(加电源)的剖面图。Figure 3 is a cross-sectional view of the arc generating device (power supply).
图4为图2的A向剖面图。Fig. 4 is a sectional view taken along the line A in Fig. 2.
图5为采用电磁铁压缩电弧的原理图。Figure 5 is a schematic diagram of using an electromagnet to compress an arc.
图6为溶解有产物的有机溶剂的色谱图。Figure 6 is a chromatogram of the organic solvent in which the product is dissolved.
其中，among them,
1-电弧反应室；1- Arc reaction chamber;
11-阴极电极；11- cathode electrode;
12-阳极电极；121-辅助阳极；12- anode electrode; 121- auxiliary anode;
13-电磁铁；131-绝缘层；13-Electromagnet; 131-Insulation layer;
14-水冷壁；141-阴极冷却水进水口；142-阴极冷却水出水口；143-辅助阳极冷却水进水口；144-辅助阳极冷却水出水口；14-Water wall; 141-Cathode cooling water inlet; 142-Cathode cooling water outlet; 143-Anode cooling water inlet; 144-Anode cooling water outlet;
15-惰性气体进口；15- Inert gas inlet;
16-惰性气体出口；16- Inert gas outlet;
17-收集口；17- Collection port;
18-电源；18-power supply;
19-电弧；19- Arc;
2-冷却仓；2- Cooling chamber;
3-过滤仓；3- filter chamber;
4-尾气处理单元。4- Exhaust gas treatment unit.
详述Detail
为使本公开的目的、技术方案和优点更加清楚，下面将对本公开的技术方案进行详细的描述。显然，所描述的实施例仅仅是本公开一部分实施例，而不是全部的实施例。基于本公开中的实施例，本领域普通技术人员在没有做出创造性劳动的前提下所得到的所有其它实施方式，都属于本公开所保护的范围。In order to make the objectives, technical solutions, and advantages of the present disclosure clearer, the technical solutions of the present disclosure will be described in detail below. Obviously, the described embodiments are only a part of the embodiments of the present disclosure, rather than all the embodiments. Based on the embodiments in the present disclosure, all other implementations obtained by those of ordinary skill in the art without creative work shall fall within the protection scope of the present disclosure.
[电弧反应室][Arc reaction chamber]
一方面，本公开的某些实施例涉及使用压缩电弧制备富勒烯的装置。如图1所示，该装置包括电弧反应室1，电弧反应室1的作用为制备含有富勒烯的烟炱。在电弧反应室内部设有阴极电极11、阳极电极12、电源18、电磁铁13和水冷壁14。In one aspect, certain embodiments of the present disclosure relate to an apparatus for preparing fullerenes using a compressed arc. As shown in Fig. 1, the device includes an arc reaction chamber 1, and the function of the arc reaction chamber 1 is to prepare fullerene-containing soot. A cathode electrode 11, an anode electrode 12, a power source 18, an electromagnet 13 and a water wall 14 are provided inside the arc reaction chamber.
其中，水冷壁14为一个具有夹层腔体的圆柱状结构，水冷壁14上设有进水口和出水口(图中未示出)与该夹层腔体相连通，进水口和出水口的数量可以大于一个。夹层腔体用于提供冷却水循环空间以使冷却水吸收并带走反应热，维持装置稳定运行。Wherein, the water wall 14 is a cylindrical structure with a sandwich cavity, and the water wall 14 is provided with water inlets and water outlets (not shown in the figure) to communicate with the sandwich cavity, and the number of water inlets and water outlets can be Greater than one. The sandwich cavity is used to provide cooling water circulation space so that the cooling water absorbs and takes away the reaction heat and maintains the stable operation of the device.
阴极电极11和阳极电极12相对设置于该水冷壁14内，两者之间具有一定距离，该距离可以为10-45毫米。电源18可设置于电弧反应室的内部或外部，电源18的正极通过导线与阳极电极12连接，电源18的负极通过导线与阴极电极11连接，在阴极电极11和阳极电极12之间的通道内可产生电弧19。由电弧19产生的高温区形成了大量的富勒烯球笼，在流动气体作用下，高温区形成的富勒烯球笼能快速离开反应区，进入后续的冷却仓2中，与现有技术中电弧反应室内使用非流动的惰性气体相比，可以提升富勒烯的产率和产量。The cathode electrode 11 and the anode electrode 12 are arranged oppositely in the water-cooled wall 14 with a certain distance between the two, which may be 10-45 mm. The power supply 18 can be arranged inside or outside the arc reaction chamber. The positive electrode of the power supply 18 is connected to the anode electrode 12 through a wire, and the negative electrode of the power supply 18 is connected to the cathode electrode 11 through a wire, in the channel between the cathode electrode 11 and the anode electrode 12. Can produce arc19. The high temperature zone generated by the arc 19 forms a large number of fullerene cages. Under the action of the flowing gas, the fullerene cages formed in the high temperature zone can quickly leave the reaction zone and enter the subsequent cooling chamber 2, which is similar to the prior art Compared with the use of non-flowing inert gas in the medium arc reaction chamber, the yield and output of fullerene can be improved.
电磁铁13为通电线圈，通电线圈套于水冷壁14外，并位于阴极电极11和阳极电极12之间，用于产生磁场对电弧19进行压缩。图5为采用电磁铁压缩电弧的原理图，即通电螺线管中的安培定则(安培定则二)：用右手握住通电螺线管，让四指指向电流的方向，那么大拇指所指的那一端为通电螺线管的N极。可见向通电线圈内通入电流产生 磁场，能够对电弧产生导向和压缩作用，进一步控制电弧19的形状和路径，使电弧19位于通道的中心。需要说明的是，由于发生电弧19为等离子弧，经过压缩后电弧19的功率不会变化，但是电弧19的形状会变化，具体表现为电弧柱变细，变细后增加了单位面积的能量。The electromagnet 13 is an energizing coil, and the energizing coil is sheathed outside the water wall 14 and located between the cathode electrode 11 and the anode electrode 12, and is used to generate a magnetic field to compress the arc 19. Figure 5 is a schematic diagram of the use of electromagnets to compress the arc, that is, the Ampere’s rule in the energized solenoid (Ampere’s rule two): Hold the energized solenoid with your right hand and let the four fingers point in the direction of the current. The end pointed to is the N pole of the energized solenoid. It can be seen that applying current to the energized coil generates a magnetic field, which can guide and compress the arc, and further control the shape and path of the arc 19 so that the arc 19 is located in the center of the channel. It should be noted that since the arc 19 is a plasma arc, the power of the arc 19 will not change after compression, but the shape of the arc 19 will change. Specifically, the arc column becomes thinner, and the energy per unit area is increased after being thinned.
电弧反应室1设有惰性气体进口15、惰性气体出口16和收集口17，惰性气体进口15和惰性气体出口16分别用于向电弧反应室1内导入和导出惰性气体，为反应提供惰性气氛。收集口17用于将反应后的气相产物从电弧反应室1中导出，后续还需对气相产物进行冷却收集等操作。The arc reaction chamber 1 is provided with an inert gas inlet 15, an inert gas outlet 16 and a collection port 17. The inert gas inlet 15 and the inert gas outlet 16 are used to introduce and export inert gas into and out of the arc reaction chamber 1 to provide an inert atmosphere for the reaction. The collection port 17 is used to lead the reacted gas phase product out of the arc reaction chamber 1, and the gas phase product needs to be cooled and collected later.
在本公开的某些实施例中，阴极电极11的材质为紫铜，其内部含有钨铈电极芯。由于紫铜的导热率优于其它金属，采用紫铜作为阴极电极11能降低阴极温度，且具有较好的导电性。In some embodiments of the present disclosure, the material of the cathode electrode 11 is red copper, which contains a tungsten-cerium electrode core. Since copper has better thermal conductivity than other metals, using copper as the cathode electrode 11 can reduce the temperature of the cathode and has better electrical conductivity.
在本公开的某些实施例中，阳极电极12的材质为石墨。进一步可采用碳棒作为阳极电极12，在电弧反应过程中气化生成富勒烯和其它碳纳米材料。In some embodiments of the present disclosure, the material of the anode electrode 12 is graphite. Further, a carbon rod can be used as the anode electrode 12, which is vaporized to generate fullerene and other carbon nanomaterials during the arc reaction.
在本公开的某些实施例中，在通电线圈外设有绝缘层131，作用为防止电弧19能量分散，产生双弧或串弧。具体地，电弧19发生过程中，阴极电极11到阳极电极12之间形成回路，流动的惰性气体能够在阴极电极11和阳极电极12之间形成一个气态的绝缘层。由于通过该惰性气体形成的绝缘层偶尔会被破坏，破坏时会出现双弧或者叫串弧。当出现双弧时，原先电弧19上的部分电流会分散到另外出现的电弧上，且此种电弧不会受到约束，因此电弧能量分散，功率降低。通电线圈外的绝缘层131是防止冷气的绝缘层，即前文提及的气态绝缘层被破坏时，电流从阴极电极11到辅助阳极121，再到阳极电极12形成电流通道。在通电线圈外增加绝缘层131后，可以有效的防止此类情况的发生。In some embodiments of the present disclosure, an insulating layer 131 is provided outside the energized coil to prevent the energy of the arc 19 from dispersing, resulting in double arcs or series arcs. Specifically, during the occurrence of the arc 19, a loop is formed between the cathode electrode 11 and the anode electrode 12, and the flowing inert gas can form a gaseous insulating layer between the cathode electrode 11 and the anode electrode 12. Since the insulating layer formed by the inert gas is occasionally destroyed, double arcs or string arcs will occur during destruction. When a double arc occurs, part of the current on the original arc 19 will be dispersed to another arc, and this arc will not be restricted, so the arc energy is dispersed and the power is reduced. The insulating layer 131 outside the energized coil is an insulating layer to prevent cold air, that is, when the aforementioned gaseous insulating layer is destroyed, the current flows from the cathode electrode 11 to the auxiliary anode 121 and then to the anode electrode 12 to form a current path. Adding an insulating layer 131 outside the energized coil can effectively prevent such situations from occurring.
[电弧发生装置][Arc Generator]
电弧发生装置的具体结构如图2和图3所示。该装置位于电弧反应室1内部，包括阴极电极11、辅助阳极121、阳极电极12和电源 18。The specific structure of the arc generating device is shown in Figure 2 and Figure 3. The device is located inside the arc reaction chamber 1 and includes a cathode electrode 11, an auxiliary anode 121, an anode electrode 12 and a power source 18.
在阴极电极11外周设有水冷壁14，水冷壁14和阴极电极11之间具有一定空隙，构成惰性气体循环空间。水冷壁14上设有进水口和出水口，水冷壁14内部具有冷却水循环空间。具体地，在阴极电极11外部设有阴极冷却水进水口141和阴极冷却水出水口142，在辅助阳极121外部设有辅助阳极冷却水进水口143和辅助阳极冷却水出水口144。惰性气体进口15可采用图4所示的方式，即水冷壁14上同时设有多个惰性气体进口15，每一惰性气体进口15均为切向进气孔，可以使惰性气体旋流进入水冷壁14和阴极电极11之间的空隙内，迅速带走反应热。A water-cooled wall 14 is provided on the outer periphery of the cathode electrode 11, and there is a certain gap between the water-cooled wall 14 and the cathode electrode 11 to form an inert gas circulation space. The water wall 14 is provided with a water inlet and a water outlet, and the water wall 14 has a cooling water circulation space inside. Specifically, a cathode cooling water inlet 141 and a cathode cooling water outlet 142 are provided outside the cathode electrode 11, and an auxiliary anode cooling water inlet 143 and an auxiliary anode cooling water outlet 144 are provided outside the auxiliary anode 121. The inert gas inlet 15 can adopt the method shown in Fig. 4, that is, multiple inert gas inlets 15 are provided on the water-cooled wall 14 at the same time, and each inert gas inlet 15 is a tangential inlet hole, which can make the inert gas swirl into the water cooling wall. In the gap between the wall 14 and the cathode electrode 11, the reaction heat is quickly taken away.
在水冷壁14外，阴极电极11和阳极电极12之间设有电磁铁13。辅助阳极121位于水冷壁14和阴极电极11之间的空隙内，并向电磁铁13所在位置延伸，直至进入电磁铁13的内环。电磁铁13靠近阳极电极12的一侧设有绝缘层131。Outside the water wall 14, an electromagnet 13 is provided between the cathode electrode 11 and the anode electrode 12. The auxiliary anode 121 is located in the gap between the water-cooled wall 14 and the cathode electrode 11 and extends toward the position of the electromagnet 13 until it enters the inner ring of the electromagnet 13. An insulating layer 131 is provided on the side of the electromagnet 13 close to the anode electrode 12.
电源18的负极与阴极电极11连接，电源18的正极分别与阳极电极12和辅助阳极121连接。在电源18正极与阳极电极12的连接导线上设有阳极控制开关K1，电源18正极与辅助阳极121的连接导线上设有辅助阳极控制开关K2。The negative electrode of the power source 18 is connected to the cathode electrode 11, and the positive electrode of the power source 18 is connected to the anode electrode 12 and the auxiliary anode 121, respectively. An anode control switch K1 is provided on the connecting wire between the positive electrode of the power source 18 and the anode electrode 12, and an auxiliary anode control switch K2 is provided on the connecting wire between the anode of the power source 18 and the auxiliary anode 121.
需要启动该电弧发生装置时，首先闭合辅助阳极控制开关K2，向惰性气体进口15内通入惰性气体，在阴极电极11的表面形成惰性气体保护气膜。由阴极电极11发射的电子落在辅助阳极121上，形成辅助电弧。当辅助电弧达到一定功率和长度后，闭合阳极控制开关K1，阳极弧根转移至阳极电极12上，形成阴极电极11到阳极电极12之间的主电弧，此时断开辅助阳极控制开关K2，辅助电弧自动熄灭。即先形成辅助电弧，再转弧形成主电弧。电弧19的转弧是从阴极电极11到辅助阳极121距离最短的位置，然后通过流动的惰性气体将电弧送到阳极电极12上，接着断开辅助阳极121的电源，让阴极电极11到阳极电极12之间形成回路，形成主电弧19。流动的惰性气体能够在阴极电极11和阳极电极12之间形成一个绝缘层。由于通过该惰性气体形成的绝缘层偶尔会被破坏，破坏时会出现双弧或者叫串弧，电弧 能量分散，功率降低，因此需要在通电线圈外设置绝缘层131。When the arc generator needs to be started, the auxiliary anode control switch K2 is first closed, and the inert gas is introduced into the inert gas inlet 15 to form an inert gas protective gas film on the surface of the cathode electrode 11. The electrons emitted from the cathode electrode 11 fall on the auxiliary anode 121 to form an auxiliary arc. When the auxiliary arc reaches a certain power and length, the anode control switch K1 is closed, and the anode arc root is transferred to the anode electrode 12, forming a main arc between the cathode electrode 11 and the anode electrode 12. At this time, the auxiliary anode control switch K2 is opened. The auxiliary arc is automatically extinguished. That is, the auxiliary arc is formed first, and then the arc is turned to form the main arc. The arc 19 is turned from the cathode electrode 11 to the auxiliary anode 121 at the shortest distance, and then the arc is sent to the anode electrode 12 by the flowing inert gas, and then the auxiliary anode 121 is disconnected from the power supply to allow the cathode electrode 11 to reach the anode electrode. A loop is formed between 12 and a main arc 19 is formed. The flowing inert gas can form an insulating layer between the cathode electrode 11 and the anode electrode 12. Since the insulating layer formed by the inert gas is occasionally destroyed, double arcs or series arcs will occur when destroyed, and the arc energy is dispersed and the power is reduced. Therefore, it is necessary to provide an insulating layer 131 outside the energized coil.
综上所述，本公开通过以下方式防止双弧出现：(1)在通电线圈外设置绝缘层131；(2)降低辅助阳极121冷却水的温度，使惰性气体的温度尽量低；(3)增加惰性气体的流动速度；(4)设置多个惰性气体进口15，使惰性气体旋流进入。In summary, the present disclosure prevents double arcs from appearing in the following ways: (1) Provide an insulating layer 131 outside the energized coil; (2) Reduce the temperature of the auxiliary anode 121 cooling water to make the temperature of the inert gas as low as possible; (3) Increase the flow rate of the inert gas; (4) Set up multiple inert gas inlets 15 to allow the inert gas to swirl in.
[其它装置结构][Other device structure]
在某些实施例中，电弧反应室1内部还设有电极移动机构(图中未示出)。当观察到阳极电极12(通常为碳棒)由于蒸发而变短时，可通过操纵电极移动机构使阳极电极12向阴极电极11方向移动，使阴极电极11和阳极电极12维持于一合适距离。电极移动机构可以为公知的螺旋移动机构或气动移动机构，例如使用气缸使阳极电极12往返移动。In some embodiments, an electrode moving mechanism (not shown in the figure) is also provided inside the arc reaction chamber 1. When it is observed that the anode electrode 12 (usually a carbon rod) becomes shorter due to evaporation, the anode electrode 12 can be moved toward the cathode electrode 11 by operating the electrode moving mechanism, so that the cathode electrode 11 and the anode electrode 12 are maintained at an appropriate distance. The electrode moving mechanism may be a well-known screw moving mechanism or a pneumatic moving mechanism, for example, an air cylinder is used to move the anode electrode 12 back and forth.
在某些实施例中，该装置还包括与电弧反应室1依次连接的冷却仓2、过滤仓3和尾气处理单元4。其中，冷却仓2与电弧反应室1的收集口17连接，用于冷却从电弧反应室1输出的气相产物，并将冷却后的气相产物输入过滤仓3；过滤仓3用于将气相产物中的固体物过滤掉，并将不含有固体物的气相产物输入尾气处理单元4；尾气处理单元4用于对从过滤仓3输出的气相产物进行收集和纯化处理，可以进行循环使用。In some embodiments, the device further includes a cooling bin 2, a filtering bin 3, and an exhaust gas processing unit 4 connected to the arc reaction chamber 1 in sequence. Wherein, the cooling bin 2 is connected to the collection port 17 of the arc reaction chamber 1, and is used to cool the gas phase products output from the arc reaction chamber 1 and input the cooled gas phase products into the filter bin 3; The solids are filtered out, and the gas phase products that do not contain solids are input to the tail gas processing unit 4; the tail gas treatment unit 4 is used to collect and purify the gas phase products output from the filter bin 3, and can be recycled.
需要说明的是，电弧反应室1、冷却仓2和过滤仓3都是在真空条件下工作的。具体地，由于使用滤袋对含有富勒烯的碳纳米颗粒进行过滤收集，因此需要将从电弧反应室1输出的气相产物先冷却到滤袋可以接受的温度。过滤出的烟炱存留在过滤仓3底部，在过滤仓3底部安装有真空阀门。收集时在阀门处连接收集容器，直接将该阀门打开即可，可以避免烟炱与空气和空气中的水蒸气接触。不含有固体物的气相产物进入尾气处理单元4进行收集和纯化，当纯度到达99.99％或99.999％时可以压缩进行二次使用。It should be noted that the arc reaction chamber 1, the cooling chamber 2 and the filter chamber 3 all work under vacuum conditions. Specifically, since a filter bag is used to filter and collect fullerene-containing carbon nanoparticles, it is necessary to cool the gas phase product output from the arc reaction chamber 1 to a temperature acceptable to the filter bag. The filtered soot is stored at the bottom of the filter bin 3, and a vacuum valve is installed at the bottom of the filter bin 3. When collecting, connect the collection container to the valve and open the valve directly to prevent the soot from coming into contact with the air and water vapor in the air. The gas phase products that do not contain solids enter the tail gas processing unit 4 for collection and purification, and can be compressed for secondary use when the purity reaches 99.99% or 99.999%.
[制备富勒烯的方法][Method of preparing fullerene]
另一方面，本公开的某些实施例还涉及使用该装置制备富勒烯的方法，其包括：向电弧反应室1内通入惰性气体，向水冷壁12中通入冷却水，使阴极电极11和阳极电极12放电产生压缩电弧19，得到含有富勒烯的烟炱。On the other hand, certain embodiments of the present disclosure also relate to a method for preparing fullerenes using the device, which includes: passing an inert gas into the arc reaction chamber 1 and passing cooling water into the water wall 12 to make the cathode electrode The discharge of 11 and the anode electrode 12 generates a compressed arc 19 to obtain fullerene-containing soot.
在本公开的某些实施例中，烟炱经冷却和过滤后收集得到，向收集物中加入有机溶剂进行充分混合，除去其中的不溶物后，得到含有富勒烯的碳纳米材料。加入的有机溶剂可以为甲苯或邻二甲苯。如果产物中含富勒烯，则有机溶剂由无色透明转变为酒红色至黑色。In some embodiments of the present disclosure, the soot is collected after cooling and filtering, and an organic solvent is added to the collection to mix thoroughly, and the insoluble matter is removed from the collection to obtain a carbon nanomaterial containing fullerene. The organic solvent added can be toluene or o-xylene. If the product contains fullerenes, the organic solvent changes from colorless and transparent to wine red to black.
在本公开的某些实施例中，惰性气体为单一氦气、单一氩气，或者为氦气和氩气的混合气体。由于氦气的分子量小，能快速进入富勒烯的球笼进行冷却，现有技术通常使用单一氦气。但氦气通常是从含量比例较高的天然气中提取。虽然天然气田为数众多，但能开采出氦气的气田没有大幅增加的倾向。由于氦气难以被其他气体替代，而氦气的供应却一直处于有限的状态，如果继续按照目前的速度消费，25年后氦气就会被消耗殆尽。而本公开中采用旋向进气，可通过气体流动增强冷却效果，因此可使用混合惰性气体，并且在通入的混合气体中，氦气和氩气的比例没有要求，含有微量氦气即可。In some embodiments of the present disclosure, the inert gas is a single helium gas, a single argon gas, or a mixed gas of helium and argon. Since helium has a small molecular weight and can quickly enter the fullerene cage for cooling, the prior art usually uses a single helium gas. But helium is usually extracted from natural gas with a higher content. Although there are many natural gas fields, the number of gas fields that can produce helium does not tend to increase significantly. Since helium is difficult to be replaced by other gases, and the supply of helium has been in a limited state, if consumption continues at the current rate, helium will be exhausted after 25 years. In the present disclosure, the swirling air intake can be used to enhance the cooling effect through gas flow. Therefore, a mixed inert gas can be used, and the ratio of helium to argon in the mixed gas introduced is not required, and only a small amount of helium is required. .
在某些实施例中，本公开在阴极电极11和阳极电极12之间使用的电源18为直流电源。该直流电源为恒流电源，可以提供电流使阴极电极11和阳极电极12之间产生电弧。因为是恒流电源，所以电流是设定值，电压是变化值，电压的变化是随着阴极电极11和阳极电极12之间距离的变化，以及气体流量的变化而变化的。在某些实施例中，电源18电流为100-500安，电压为10-400伏。In some embodiments, the power source 18 used between the cathode electrode 11 and the anode electrode 12 in the present disclosure is a direct current power source. The DC power supply is a constant current power supply, which can provide current to generate an arc between the cathode electrode 11 and the anode electrode 12. Because it is a constant current power supply, the current is the set value, the voltage is the change value, and the voltage change changes with the change of the distance between the cathode electrode 11 and the anode electrode 12 and the change of the gas flow. In some embodiments, the power source 18 has a current of 100-500 amps and a voltage of 10-400 volts.
作为阳极电极12的碳棒的反应时间，是由电流设定值和气体流量值决定的。电流越大气化速度越快，气体流量越大，气化速度也越快。但并不能一味地提高反应速度，需要根据具体实验条件进行调整。The reaction time of the carbon rod as the anode electrode 12 is determined by the current setting value and the gas flow value. The higher the current, the faster the gasification speed, the greater the gas flow, and the faster the gasification speed. However, it cannot blindly increase the reaction speed, and needs to be adjusted according to specific experimental conditions.
在某些实施例中，放电过程中产生的电弧温度为5000-20000℃，电弧柱直径为5-20mm。在某些实施例中，电弧柱直径为8-9mm。现有技术中产生的电弧柱直径为2-3mm，电弧温度在6000℃以下。与现有技术相比，采用本公开提供的装置产生的电弧柱***且尺寸可控， 温度也有所升高。申请人发现，采用现有富勒烯制备装置，大约40-60分钟消耗一根长为300mm，直径为8mm的石墨棒。而采用本公开的装置，在5-15分钟之间可消耗同样尺寸的碳棒，因此可以显著提升富勒烯产量。In some embodiments, the arc temperature generated during the discharge is 5000-20000°C, and the arc column diameter is 5-20 mm. In some embodiments, the arc column diameter is 8-9 mm. The diameter of the arc column generated in the prior art is 2-3 mm, and the arc temperature is below 6000°C. Compared with the prior art, the arc column generated by the device provided by the present disclosure is thicker and controllable in size, and the temperature is also increased. The applicant found that using the existing fullerene preparation device, a graphite rod with a length of 300 mm and a diameter of 8 mm was consumed in about 40-60 minutes. With the device of the present disclosure, carbon rods of the same size can be consumed within 5-15 minutes, so the fullerene production can be significantly increased.
实施例1Example 1
电弧反应室1内的阴极电极11为含有钨铈芯的紫铜电极，阳极电极12为碳棒，在惰性气体气氛下(氦气和氩气的体积比为1:5)向水冷壁14中通入冷却水，使阴极电极11和阳极电极12放电产生压缩电弧。采用直流电源18为阴极电极11和阳极电极12供电，电源18电流为200安，电压为50-200伏。冷却水温度为18-20℃。The cathode electrode 11 in the arc reaction chamber 1 is a copper electrode containing a tungsten-cerium core, and the anode electrode 12 is a carbon rod, which is passed into the water wall 14 under an inert gas atmosphere (the volume ratio of helium and argon is 1:5) Cooling water is introduced to discharge the cathode electrode 11 and the anode electrode 12 to generate a compressed arc. A DC power source 18 is used to supply power to the cathode electrode 11 and the anode electrode 12, the current of the power source 18 is 200 amps, and the voltage is 50-200 volts. The cooling water temperature is 18-20°C.
放电过程中产生的电弧19温度为5000-20000℃，电弧柱直径为8-9mm。反应的气相产物从电弧反应室1中输出，经冷却仓2冷却和过滤仓3收集后，得到含有富勒烯的烟炱。The temperature of the arc 19 generated during the discharge is 5000-20000°C, and the diameter of the arc column is 8-9mm. The gaseous product of the reaction is output from the arc reaction chamber 1, and is cooled by the cooling chamber 2 and collected by the filtering chamber 3 to obtain fullerene-containing soot.
向烟炱中加入邻二甲苯溶解，离心分离出不溶物后得到红棕色的溶液，对其进行液相色谱检测，色谱图如图6所示，可以看出当保留时间为7.449秒时，出现的是C60的特征峰，11.954秒出现的是C70的特征峰，证明产物中含有富勒烯。Add o-xylene to the soot to dissolve it, centrifuge to separate the insoluble matter to obtain a reddish-brown solution, which is detected by liquid chromatography. The chromatogram is shown in Figure 6. It can be seen that when the retention time is 7.449 seconds, it appears The characteristic peak of C60 is the characteristic peak of C60, and the characteristic peak of C70 appears at 11.954 seconds, which proves that the product contains fullerene.
当电流为100A时，将电源电压从40V调至110V，富勒烯产率变化见表1。When the current is 100A, adjust the power supply voltage from 40V to 110V, and the fullerene yield changes are shown in Table 1.
表1Table 1
 To 40V40V 50V50V 60V60V 70V70V 80V80V 90V90V 100V100V 110V110V
C60产率(％)C60 yield (%) 0.310.31 0.580.58 0.820.82 2.312.31 2.762.76 2.432.43 2.112.11 1.851.85
C70产率(％)C70 yield (%) 0.080.08 0.090.09 0.2660.266 0.680.68 0.930.93 0.790.79 0.680.68 0.620.62
C80产率(％)C80 yield (%) 0.0010.001 0.0030.003 0.0030.003 0.0210.021 0.0270.027 0.020.02 0.0180.018 0.0060.006
金属富勒烯产率(％)Metal fullerene yield (%) 00 00 00 00 0.00060.0006 00 00 00
*金属富勒烯的含义为C82球笼内部含有一个金属原子，例如Gd@C82。*Metal fullerene means that the C82 ball cage contains a metal atom, such as Gd@C82.
当电流为200A时，同样改变电源电压，富勒烯产率变化见表2。When the current is 200A, the power supply voltage is also changed, the fullerene yield changes are shown in Table 2.
表2Table 2
 To 40V40V 50V50V 60V60V 70V70V 80V80V 90V90V 100V100V 110V110V
C60产率(％)C60 yield (%) 1.281.28 1.961.96 2.732.73 3.273.27 4.164.16 4.914.91 5.245.24 5.385.38
C70产率(％)C70 yield (%) 0.430.43 0.630.63 0.940.94 1.111.11 1.371.37 1.611.61 1.761.76 1.751.75
C80产率(％)C80 yield (%) 0.0410.041 0.0610.061 0.0910.091 0.1070.107 0.1340.134 0.1480.148 0.1520.152 0.1490.149
金属富勒烯产率(％)Metal fullerene yield (%) 00 0.0020.002 0.0030.003 0.00110.0011 0.0040.004 0.0050.005 0.00520.0052 0.00540.0054
当电流为300A时，改变电源电压，富勒烯产率变化见表3。When the current is 300A, changing the power supply voltage, the fullerene yield changes are shown in Table 3.
表3table 3
 To 40V40V 50V50V 60V60V 70V70V 80V80V 90V90V 100V100V 110V110V
C60产率(％)C60 yield (%) 2.532.53 3.263.26 5.195.19 6.446.44 7.887.88 8.438.43 7.637.63 7.257.25
C70产率(％)C70 yield (%) 0.850.85 1.071.07 1.731.73 2.112.11 2.632.63 2.812.81 2.442.44 2.392.39
C80产率(％)C80 yield (%) 0.0820.082 0.1080.108 0.1690.169 0.1990.199 0.2320.232 0.2590.259 0.2110.211 0.1130.113
金属富勒烯产率(％)Metal fullerene yield (%) 0.00220.0022 0.00310.0031 0.00490.0049 0.00570.0057 0.00810.0081 0.00840.0084 0.00690.0069 0.00680.0068
当电流为400A时，改变电源电压，富勒烯产率变化见表4。When the current is 400A, changing the power supply voltage, the fullerene yield changes are shown in Table 4.
表4Table 4
 To 40V40V 50V50V 60V60V 70V70V 80V80V 90V90V 100V100V 110V110V
C60产率(％)C60 yield (%) 2.852.85 3.713.71 5.315.31 6.766.76 8.258.25 8.428.42 8.358.35 8.338.33
C70产率(％)C70 yield (%) 0.920.92 1.221.22 1.781.78 2.242.24 2.392.39 2.792.79 2.872.87 2.792.79
C80产率(％)C80 yield (%) 0.0740.074 0.1150.115 0.1630.163 0.2120.212 0.2360.236 0.2580.258 0.2730.273 0.2680.268
金属富勒烯产率(％)Metal fullerene yield (%) 0.00270.0027 0.00360.0036 0.00510.0051 0.00590.0059 0.00780.0078 0.00750.0075 0.00790.0079 0.00840.0084
当电流为500A时，改变电源电压，富勒烯产率变化见表5。When the current is 500A, changing the power supply voltage, the fullerene yield changes are shown in Table 5.
表5table 5
 To 40V40V 50V50V 60V60V 70V70V 80V80V 90V90V 100V100V 110V110V
C60产率(％)C60 yield (%) 2.152.15 2.912.91 4.874.87 5.635.63 7.547.54 8.268.26 7.927.92 7.167.16
C70产率(％)C70 yield (%) 0.830.83 0.960.96 1.631.63 1.881.88 2.532.53 2.742.74 2.632.63 2.372.37
C80产率(％)C80 yield (%) 0.0770.077 0.0810.081 0.0990.099 0.1820.182 0.2490.249 0.2710.271 0.2580.258 0.2310.231
金属富勒烯产率(％)Metal fullerene yield (%) 0.00190.0019 0.00270.0027 0.00460.0046 0.00550.0055 0.00740.0074 0.00860.0086 0.00780.0078 0.00680.0068
结合表1-5数据可以看出，当电流值从100A增加至500A后，C60的产率呈现先增加后下降的趋势，在400A时达到最大值。Combining the data in Table 1-5, it can be seen that when the current value increases from 100A to 500A, the yield of C60 shows a trend of first increasing and then decreasing, reaching the maximum at 400A.
实施例2Example 2
将阴极电极替换为碳棒，电流值为400A，电压值为100V，其它同实施例1。The cathode electrode was replaced with a carbon rod, the current value was 400A, and the voltage value was 100V, and the others were the same as in Example 1.
实施例3Example 3
将惰性气体替换为单一氦气，电流值为400A，电压值增加至170V(这是改变惰性气体带来的电压变化，并非主动改变电压)，其它同实施例1。Replace the inert gas with a single helium gas, the current value is 400A, and the voltage value is increased to 170V (this is the voltage change caused by changing the inert gas, not actively changing the voltage), and the others are the same as in Embodiment 1.
实施例4Example 4
将惰性气体替换为单一氩气，电流值为400A，电压值为100V，其它同实施例1。The inert gas was replaced with a single argon gas, the current value was 400A, and the voltage value was 100V, and the others were the same as in Example 1.
实施例5Example 5
去掉电弧反应室内的电磁铁，电流值为400A，电压值为100V，其它同实施例1。Remove the electromagnet in the arc reaction chamber, the current value is 400A, the voltage value is 100V, and the others are the same as in Example 1.
实施例1-5的富勒烯(C60)产率见表6。The fullerene (C60) yields of Examples 1-5 are shown in Table 6.
表6Table 6
 To 实施例1Example 1 实施例2Example 2 实施例3Example 3 实施例4Example 4 实施例5Example 5
C60产率(％)C60 yield (%) 8.358.35 7.467.46 8.218.21 8.308.30 6.156.15
从表6数据可以看出，使用单一或混合惰性气体，对富勒烯产率影响不大。不使用电磁铁会使产率下降。It can be seen from the data in Table 6 that the use of single or mixed inert gases has little effect on the yield of fullerenes. Not using an electromagnet will reduce the yield.
以上所述，仅为本公开的具体实施方式，但本公开的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本公开揭露的技术范围内，可轻易想到变化或替换，都应涵盖在本公开的保护范围之内。因此，本公开的保护范围应以所述权利要求的保护范围为准。The above are only specific implementations of the present disclosure, but the protection scope of the present disclosure is not limited thereto. Any person skilled in the art can easily think of changes or substitutions within the technical scope disclosed in the present disclosure. It should be covered within the protection scope of the present disclosure. Therefore, the protection scope of the present disclosure should be subject to the protection scope of the claims.

Claims (10)

  1. 使用压缩电弧制备富勒烯的装置，所述装置包括电弧反应室，所述电弧反应室用于制备含有富勒烯的烟炱，在所述电弧反应室内部设有阴极电极、阳极电极、电源、电磁铁和水冷壁，其中，A device for preparing fullerenes using a compressed arc, the device comprising an arc reaction chamber for preparing fullerene-containing soot, and a cathode electrode, an anode electrode, and a power source are provided inside the arc reaction chamber , Electromagnet and water wall, among them,
    所述水冷壁为一个具有夹层腔体的圆柱状结构，所述水冷壁上设有进水口和出水口与该夹层腔体相连通，所述夹层腔体用于提供冷却水循环空间以使冷却水吸收并带走反应热，The water-cooled wall is a cylindrical structure with a sandwich cavity, and the water-cooled wall is provided with a water inlet and a water outlet to communicate with the sandwich cavity, and the sandwich cavity is used to provide a cooling water circulation space for cooling water Absorb and take away the heat of reaction,
    所述阴极电极和阳极电极相对设置于所述水冷壁内，两者之间具有一定距离，所述电源的正极与阳极电极连接，所述电源的负极与阴极电极连接，在所述阴极电极和阳极电极之间可产生电弧，The cathode electrode and the anode electrode are arranged oppositely in the water-cooled wall with a certain distance between the two. The positive electrode of the power source is connected to the anode electrode, the negative electrode of the power source is connected to the cathode electrode, and the cathode electrode and An arc can be generated between the anode electrodes,
    所述电磁铁为通电线圈，所述通电线圈套于所述水冷壁外，并位于所述阴极电极和阳极电极之间，用于产生磁场与通入的惰性气体同时对电弧进行压缩，The electromagnet is an energized coil, and the energized coil is sleeved outside the water-cooled wall and located between the cathode electrode and the anode electrode, and is used to generate a magnetic field and the inert gas introduced to simultaneously compress the arc,
    所述电弧反应室设有用于产生等离子体电弧的惰性气体进口、惰性气体出口和收集口，所述惰性气体进口和惰性气体出口分别用于向所述电弧反应室内导入和导出惰性气体，所述收集口用于将反应后的气相产物从所述电弧反应室中导出。The arc reaction chamber is provided with an inert gas inlet, an inert gas outlet, and a collection port for generating a plasma arc. The inert gas inlet and the inert gas outlet are used to introduce and export inert gas into and out of the arc reaction chamber, respectively. The collection port is used to lead the reacted gas phase products from the arc reaction chamber.
  2. 根据权利要求1所述的装置，其中，所述阴极电极的材质为紫铜，其内部含有钨铈电极芯。The device according to claim 1, wherein the material of the cathode electrode is red copper, which contains a tungsten-cerium electrode core.
  3. 根据权利要求1或2所述的装置，其中，所述阳极电极的材质为石墨。The device according to claim 1 or 2, wherein the material of the anode electrode is graphite.
  4. 根据权利要求1至3中任一权利要求所述的装置，其中，在所述通电线圈外设有绝缘层。The device according to any one of claims 1 to 3, wherein an insulating layer is provided outside the energized coil.
  5. 根据权利要求1至4中任一权利要求所述的装置，其中，所述电弧反应室内部还设有电极移动机构，用于使所述阳极电极向所述阴极电极方向移动。The device according to any one of claims 1 to 4, wherein an electrode moving mechanism is further provided inside the arc reaction chamber for moving the anode electrode toward the cathode electrode.
  6. 根据权利要求1至5任一权利要求所述的装置，其中，所述装置还包括与电弧反应室依次连接的冷却仓、过滤仓和尾气处理单元，其中，The device according to any one of claims 1 to 5, wherein the device further comprises a cooling bin, a filter bin and an exhaust gas processing unit connected to the arc reaction chamber in sequence, wherein:
    所述冷却仓与电弧反应室的收集口连接，用于冷却从所述电弧反应室输出的气相产物，并将冷却后的气相产物输入过滤仓，The cooling bin is connected to the collection port of the arc reaction chamber, and is used to cool the gas phase products output from the arc reaction chamber, and input the cooled gas phase products into the filter bin,
    所述过滤仓用于将气相产物中的固体物过滤掉，并将不含有固体物的气相产物输入尾气处理单元，The filter bin is used to filter out the solids in the gas-phase products, and input the gas-phase products without solids into the tail gas processing unit,
    所述尾气处理单元用于对从过滤仓输出的气相产物进行收集和纯化处理，可以进行循环使用The tail gas processing unit is used to collect and purify the gas phase products output from the filter bin, and can be recycled
  7. 制备富勒烯的方法，其中，所述方法使用权利要求1至6任一权利要求所述的装置，所述方法包括：向所述电弧反应室内通入惰性气体，向所述水冷壁中通入冷却水，使阴极电极和阳极电极放电产生电弧，得到含有富勒烯的烟炱。A method for preparing fullerenes, wherein the method uses the device according to any one of claims 1 to 6, and the method comprises: passing an inert gas into the arc reaction chamber, and passing into the water wall Into the cooling water, the cathode electrode and the anode electrode are discharged to generate an arc, and soot containing fullerene is obtained.
  8. 根据权利要求7所述的方法，其中，所述惰性气体为单一氦气、单一氩气，或者为氦气和氩气的混合气体。The method according to claim 7, wherein the inert gas is a single helium gas, a single argon gas, or a mixed gas of helium and argon.
  9. 根据权利要求7或8所述的方法，其中，在阴极电极和阳极电极之间使用的电源为直流电源，电源电流为100-500安，电压为10-400伏。The method according to claim 7 or 8, wherein the power source used between the cathode electrode and the anode electrode is a direct current power source, the power source current is 100-500 amps, and the voltage is 10-400 volts.
  10. 根据权利要求7至9中任一权利要求所述的方法，其中，放电过程中产生的电弧温度为5000-20000℃，电弧柱直径为5-20mm。The method according to any one of claims 7 to 9, wherein the temperature of the arc generated during the discharge is 5000-20000°C, and the diameter of the arc column is 5-20 mm.
PCT/CN2020/106772 2019-08-05 2020-08-04 Device and method for preparing fullerene using compressive arc WO2021023179A1 (en)

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