RU212492U1 - Device for the production of fullerene-containing soot - Google Patents

Abstract

The proposed utility model relates to the field of production of fullerene-containing soot containing fullerenes (C60, C70 and higher fullerenes), based on electric arc evaporation of graphite in an inert gas atmosphere.

Description

This utility model relates to devices for the production of fullerene-containing soot containing fullerenes C60, C70 and higher fullerenes. The utility model can be used in chemistry, physics, technology, metallurgy, energy, electronics, biology, medicine, pharmaceuticals and other areas of human activity.

Currently, the method based on the evaporation of graphite in an electric arc is the most effective for the synthesis of fullerenes, mainly C60 and C70, which are part of the main product of carbon vapor condensation - fullerene-containing soot. The electric arc method remains the most popular method for obtaining fullerenes in quantities sufficient for practical needs [1, 2].

The stability of the electric arc process for the synthesis of fullerenes and fullerene-containing soot is affected by many factors: voltage, current, pressure in the system, properties and flow rate of the inert gas, the nature and purity of the electrode material, etc. [3, 4].

The raw material for obtaining fullerene-containing soot is electrodes made of spectrally pure graphite. As is known, the purity of the feedstock affects the content of fullerenes in fullerene-containing soot: the cleaner the graphite electrode and the less impurities it contains, the higher the percentage of fullerenes in fullerene-containing soot. Cleaning graphite rods in a vacuum oven just prior to use is not suitable for a multiple charge machine with automatic electrode feed. A buffer chamber is used to clean the electrodes.

A device for producing fullerene-containing soot [5] is known, which includes a horizontal sealed cylindrical discharge chamber, two graphite electrodes placed on the axis of the chamber, an inert gas circulation system with a means for trapping fullerene-containing soot, a chamber for degassing a movable graphite electrode by a glow electric discharge (Patent RU No. 2341451 C1, IPC С01В 31/00, published 12/20/2008). The disadvantages of the known device are the inability to optimize the temperature field in the reactor, regardless of the arc current, which prevents the achievement of the maximum yield of fullerenes and a significant part of the graphite evaporated in the arc (up to 25-30%) goes to waste.

A device for producing fullerene-containing soot [6], including a cylindrical plasma reactor with a horizontal sealed cylindrical discharge chamber, two graphite electrodes placed along the axis of the chamber, an inert gas circulation system with a means of trapping fullerene-containing soot (Patent RU No. 102606 U1, IPC S01V 31/00 , published 03/10/2011). The disadvantages of the known device is the high cost of the material of the hollow cylinder and end caps, which inevitably leads to an increase in the cost of the process of obtaining fullerene-containing soot and the cost of the fullerene itself.

A device for producing fullerene-containing soot [7] is known, including a plasma reactor in the form of a sealed cylindrical chamber with two graphite rod electrodes placed along the axis of the chamber, a means for supplying an inert gas and swirling the flow along the axis of the electrodes, a container for collecting slags (Patent RU 39129 U1, IPC C01B 31/00, published 20.07.2004). The disadvantages of the device are the unreasonable complication of the design by various effects on the arc and the reaction volume, the impossibility of removing the resulting cathode deposit without stopping the process, which leads to a decrease in the percentage of fullerenes in soot.

A device for the production of fullerene-containing soot [8] is known (see US patent 6358375, IPC H05N 1/42, publ. 07/20/2004), including a plasma reactor and successively descending heated and cooled separators. The disadvantages of this device are the lack of degassing of the electrodes, the deposition of a cathode deposit on the fixed electrode, the deposition of a large amount of soot in the reactor, the need to stop the device to replace burnt electrodes and remove fragments of electrodes from the reaction volume, the cause of which is usually considered to be the inhomogeneity of the electrodes and a high voltage drop in the plasma. .

A device for the continuous production of carbon nanotubes and fullerenes [9] (US 2005/0019245 A1, IPC D01F 9/12, publ. 27.01.2005), including a sealed water-cooled chamber, two graphite electrodes, a replaceable sealed cartridge containing a catalyst in the form of metal wire or fine metal powder, heat exchanger, filter, storage hopper with automatic outlet valve and recirculation pump. The disadvantages of the device are the lack of degassing of the electrodes and the inability to remove the cathode deposit.

A device for obtaining fullerene-containing soot [10], including a horizontal sealed discharge chamber with two graphite rod electrodes placed along the axis of the chamber, an inert gas circulation system with a means of trapping fullerene-containing soot, a glow discharge degassing chamber (Patent RU 2343111 C1, IPC S01V 31/00 , published 01/10/2009). The disadvantages of the device are the complexity of the design, the consumption of inert gas to maintain the glow discharge and the glow discharge does not provide a high vacuum for efficient degassing of the entire volume of the electrode.

The closest to the claimed device for obtaining fullerene-containing soot is a device [11], including a plasma reactor in the form of a sealed cylindrical chamber with an inert gas circulation system with a means of trapping fullerene-containing soot, with two graphite rod electrodes placed along the axis of the chamber, with a chamber for degassing a movable graphite electrode glowing electric discharge (Patent RU 2234457 C2, IPC C01B 31/02, publ. 20.08.2004). The disadvantage of this technical device is the deposition of a significant amount of the deposit on the cathode, which causes the destruction of the material when the polarity changes, a relatively low performance on soot and fullerenes. The disadvantage of the device is the relatively low percentage of fullerenes in the soot, insufficiently complete removal of fullerene-containing soot from the reactor volume during the process.

The proposed technical solution of the claimed utility model is aimed at improving the efficiency of the device for the production of fullerene-containing soot.

The problem is solved by the fact that the device for obtaining fullerene-containing soot includes a horizontal sealed cylindrical discharge chamber with two graphite electrodes placed along the axis, an inert gas circulation system with a means for trapping fullerene-containing soot, a buffer chamber for degassing a movable consumable graphite anode. At the same time, the movable sacrificial graphite anode is resistively heated in the buffer chamber, which ensures maximum outgassing of the movable sacrificial graphite anode not only from the surface, but throughout the entire volume. The outgassing products are continuously pumped out by a vacuum pump. Tightness between the horizontal sealed cylindrical discharge chamber, the buffer chamber and the external environment is provided by Wilson seals. Heating of a movable sacrificial graphite anode is carried out due to internal resistance when current passes through it from an external current source. The first pole from an external current source is connected via a conductor to a movable sacrificial graphite anode directly at the entrance to the buffer chamber using a copper brush contact. The second pole from an external current source is connected to the anode flange with a contact group via a conductor.

Brief description of the drawing

A device for producing fullerene-containing soot (Fig. 1) includes a horizontal cylindrical sealed discharge chamber (1), a cathode flange with a graphite electrode fixation unit (cathode) (2), an anode flange with a graphite electrode fixation unit (3) (anode) (4) , buffer chamber (5), arc gap position detector (6), graphite electrode feed mechanism (7) (4). Additionally, in the buffer chamber, the electrode (4) is heated by supplying voltage to it through the conductor (8) and (9) from the current source (10). The current conductor (8) is connected to the copper brush contact (11), and the current conductor (9) is connected to the anode contact group (3). The electrode heating is controlled by a thermocouple thermostat (12). The outgassing products are removed through the pipe (13) using a vacuum pump (not shown in the figure). The unburned deposit is collected in the deposit box (14).

Literature

1. Bogdanov A.A., Deininger D., Dyuzhev G.A. Prospects for the development of industrial methods for the production of fullerenes. ZhTF , 2000, Vol. 70, Issue. 5, pp. 1-7.

2. Gruzinskaya E.A., Keskinov V.A., Keskinova M.V., Semenov K.N., Charykov N.A. Fullerene soot of electric arc synthesis. Nanosystems: physics, chemistry, mathematics , 2012, vol. 3, no. 6, pp. 83-90.

3. Afanasiev D., Blinov I., Bogdanov A., Dyuzhev G., Karataev V., Kruglikov A. Formation of fullerenes in an arc discharge. ZhTF , 1994, V. 64, Issue. 10, pp. 76-88.

4. Afanasiev D.V., Bogdanov A.A., Dyuzhev G.A., Kruglikov A.A. Formation of fullerenes in an arc discharge. II. ZhTF , 1997, V. 67, Issue. 2, pp. 125-128.

5. Bolstren N.N., Bosargin I.V., Bogdanov A.A., Sedov A.I., Filipov B.M. A method for the production of fullerene-containing soot and a device for its implementation (Patent RU No. 2341451 C1, IPC C01B 31/00, publ. 20.12.2008).

6. Sedov A.I., Basargin I.V., Bogdanov A.A., Ponyaev S.A., Bobashev S.V., Zhukov B.G. A device for the production of fullerene-containing soot. (Patent RU No. 102606 U1, IPC С01В 31/00, published on March 10, 2011).

7. Abduguev R.M., Alekhin O.S., Gerasimov V.I., Losev G.M., Nekrasov K.V., Nikonov Yu.A., Charykov N.A. Installation for obtaining fullerene-containing soot (options). (Patent RU 39129 U1, IPC С01В 31/00, published on July 20, 2004).

8. Schwob Yvon (Cannes, FR) Method and device for producing fullerenes. (Patent US 6358375, IPC H05N 1/42, publ. 20.07.2004).

9. Koulikov D. Continuous production of carbon nanotubes and fullerenes (US 2005/0019245 A1, IPC D01F 9/12, publ. 27.01.2005).

10. Bolstren N.N., Oichenko V.M., Druzhinin G.N., Belov V.A. Installation for the production of fullerene-containing soot. (Patent RU 2343111 C1, IPC C01B 31/00, published on January 10, 2009).

11. Dyuzhev G.A., Basargin I.V., Filippov B.M., Alekseev N.I., Afanasiev D.V., Bogdanov A.A. A method for producing fullerene-containing soot and a device for its implementation. Patent RU 2234457 C2, IPC C01B 31/02, published 20.08.2004.

Claims (1)

A device for producing fullerene-containing soot, including a horizontal sealed cylindrical discharge chamber with two graphite electrodes placed along the axis - one fixed on the cathode flange with a graphite electrode fixation unit, and a movable consumable graphite anode, as well as a buffer chamber hermetically connected to it, designed for degassing of a movable sacrificial graphite anode, characterized in that the buffer chamber is configured to resistively heat the movable sacrificial graphite anode for its deep outgassing, while said movable sacrificial graphite anode is configured to be connected to one pole of an external current source through a current conductor using a copper brush contact directly at the inlet to the buffer chamber, and the anode flange with the contact group is made with the possibility of connecting to the second pole of an external current source through a conductor.

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