Method of continuous production of graphenes

FIELD: chemistry.

SUBSTANCE: invention relates to field of nanotechnologies and can be used for obtaining composite materials with high electric and heat conductivity, additives to concretes and ceramics, sorbents, catalysts. Carbon-containing material is evaporated in volume thermal plasma and condensed on target surface 9 and internal surface of collector 7. Plasma generator 3, which includes coaxially located electrodes: rod cathode 4 and nozzle-shaped output anode 5, are used. Gaseous carbon-containing material 6 is supplied with plasma-forming gas through vortex chamber with channels 2 and selected from the group, consisting of methane, propane, and butane. Bottom of collector is made with hole 8 for gas flow to pass.

EFFECT: invention makes it possible to reduce energy consumption of the process, extend types of applied hydrocarbon raw material, simplify device construction and provide continuity of the process and its high productivity.

2 dwg, 3 ex


The invention relates to the field of nanotechnology and can be used to produce carbon nanostructures, in particular graphene. Synthesized by this method, the carbon materials may be used as the basis of composite materials with high electrical and thermal conductivity, as an additive in concrete and ceramics, can act as a sorbent and carrier of catalysts.

A method of producing fullerenes (application for invention RU №2005141129 "Method of producing fullerenes", IPC C01B 31/02, publ. 10.06.2006), in which a hydrocarbon gas and oxygen-containing gas discharged from the discharge section, placed in the fullerene reactor, in the fullerene reactor and burned.

The disadvantages of this method is the low rate of conversion of hydrocarbons to fullerenes, the high content of oxygen in fullerene products, and environmentally unfriendly process, due to the large amount of waste and emissions of combustion products into the atmosphere.

The known method (application for invention EN 97115694 "Method and device for producing fullerenes", IPC C01B 31/02, publ. 10.07.1999), in which the fullerenes are produced by exposure to a hydrocarbon by an electric arc, and as a carbon-containing material is used in liquid hydrocarbons.

The disadvantages of this spacebased high intensity of the process, associated with the use of the electric arc, and low manufacturability of the process, due to the fact that liquid hydrocarbon fills the casing above the level of the electrodes, which complicates the introduction of hydrocarbons to the discharge chamber and collecting the finished product.

A method of producing carbon nanotubes (patent RU 2414418 "Method of producing hydrogen and carbon nanotubes from hydrocarbon gas", IPC C01B 3/26, C01B 31/02, B82B 3/00, publ. 20.03.2011), which previously inert gas is carried out spraying of the catalyst nano-particles by evaporation of the anode graphite electrode, inside of which a wire of metal, which is used as a catalyst, with a diameter of 0.5 mm or less. Then the inert gas is pumped, ignite the arc AC method of touch electrodes with a consequent increase in the interelectrode distance to 0.3÷0.5 mm and in the plasma electric discharge is carried out high-temperature pyrolysis of hydrocarbon gas at a pressure in the reactor of 0.5÷2 ATM hydrogen and carbon nanostructures. The growth of carbon nanostructures, which is mainly single and multilayered nanotubes without admixtures of other carbon structures carbon, is synthesized on the catalyst particles. As the inert gas used�isout helium. As the hydrocarbon gas using methane, associated gas, acetylene, propane, butane, natural gas. As the catalyst, palladium, iron, Nickel, cobalt.

The disadvantage of this method is the high energy consumption associated with the use of electric arc alternating current, high costs on the behavior of the method, due to the need for expensive catalysts (cobalt, Nickel, etc.).

The closest to the claimed method is presented in the patent RU 2489350 C2 "Method of producing carbon nanomaterials and device for its implementation", IPC C01B 31/02, B82B 3/00, B82Y 40/00, publ. 10.08.2013. Bulletin No. 22. By this method the carbon-containing material vapor in the bulk thermal plasma and condensed on the outer surface of the anode and the inner cathode surface. Using glow discharge plasma. This glow discharge is set by applying an electrical voltage sufficient to breakdown of the interelectrode gap in the field formed by the anode, disposed in the cavity of the hollow cathode coaxially, and the walls of the hollow cathode. The anode is located in the cavity of the hollow cathode is movable along the axis in order to establish the distance required for the occurrence of breakdown, as well as to establish a desired distribution of electric�about potential field, current density and charge in the discharge gap, and the hollow cathode has a shape with a permeable bottom, ensuring that the flow through it of carbonaceous materials. Used carbonaceous materials may be in gaseous or liquid state, as hydrocarbons can serve as gaseous (methane, propane, butane, etc.) and liquid (oil, fuel oil, gasoil, etc.) hydrocarbons. The surface, which accumulates the produced carbon nanomaterial, represents the outer surface of the anode and the inner surface of the cathode cavity. The disadvantages of this invention are:

- the design complexity associated with the location of the anode to the cathode, and applying an additional device for moving it along the axis;

- the need for recirculation of unreacted gases to increase the degree of their transformation, which complicates the practical implementation of this method, since the inlet opening is in the bottom of the cathode;

as a plasma source applied glow discharge with significant thermal nonequilibrium. This leads to difficulties in ensuring the reproducibility of the properties of carbon nanomaterials;

- method of obtaining is not continuous and productive, since the formation of the product occurs in the volume� cathode with a diameter of 60 mm and a height of 100 mm and graphite anode with a diameter of 5 mm.

The objective of the claimed invention is to provide a method for the continuous production of graphene, which allows to achieve the technical result consists in reducing the energy intensity of the process, the expansion of the types of carbonaceous materials, simplifying the design of the device and ensure the continuity of the process and its high performance.

The task is achieved by the decomposition of gaseous carbon-containing material from the group consisting of methane, propane, butane in plasma, and its condensation on the surface, the method is characterized in that the plasma used bulk thermal plasma generated by the plasma torch with a coaxially arranged electrodes, wherein the hollow output electrode - anode has the shape of a nozzle, the cathode is in the form of a rod, a carbonaceous material is fed to a plasma-forming gas into the reaction zone through a vortex chamber to stabilize the arc gas flow, and the surface use the inner surface of the collector, the bottom of which is made with a hole for passage of gas flow, and the target surface is mounted perpendicular to this flow. The cathode, anode and the collector is cooled by water. As the plasma gas used is one of the gases: helium, argon, nitrogen or a mixture thereof. When using this method:

- the consumption of coal�roasteries materials the plasma gas and the power of plasma torch are regulated independent of each other;

can operate in the pressure range from 200 to 760 Torr;

- changing the pressure and speed of the plasma jet, it is possible within wide limits to vary the cooling rate of the resulting condensate;

- continuous synthesis is limited by the resource of the cathode of the plasma torch that can reach up to 50 hours for used designs of copper cathode with a tungsten insert.

In Fig. 1 is a diagram of a method for the continuous production of graphene.

A method of producing graphene can be implemented as follows: turn on the cooling water 1 and the working gas flowing in the channel of the vortex chamber 2 to enter the working gas. Next, a voltage is applied to the plasma torch 3 between the cathode 4 and anode 5 and one of the known methods arc is ignited between them. The distance between the electrodes continuously and is 6 mm. After stabilization of temperature in water cooling systems introduces a swirling flow of plasma gas with a carbonaceous material 6.

Consumption of carbon black with catalyst is 0.2-1 g/min plasma gas is helium or argon at pressures 350-710 Torr and with variation of flow rate from 0.5 to 1 g/ sec. In fact, the time of synthesis is determined by the capacity of the cylinder gases. �Raheny collect on the inner surface of the manifold 7 with a hole 8 and the surface of the metal target 9 after cooling the reactor to room temperature.

Analysis of the synthesized graphene obtained at a metal target, was carried out using simultaneous thermal analysis and electron microscopy.

Example 1. After temperature stabilization in the reactor tangentially injected with helium propane butane helium at a pressure of 710 Torr and a flow rate of 0.5 g/h, the arc current 400A, voltage of 70 V. the Flow rate of the mixture gas was 30 g/min. the machine is running 20 minutes On the surface of a collector formed soot with a low content of graphene. On target - graphenes in the form of defective roses. Output - 8 wt.%.

Example 2. Evaporation of the mixture of propane / butane at a flow rate of 30 g/min, at a pressure of argon of 500 Torr, the flow rate of 3.5 g/h, the current arc 350A and voltage 23 To gives the formation of layered graphene on target and the collector. On target advanced forms of amorphous carbon. Output - 50 wt.%

Example 3. By reducing the pressure to TIR, a current of 400 A, the voltage of 35 V and the flow rate of the mixture of propane, butane 25 g/min graphenes synthesized on the target and collector. Output - 95 wt.% (Fig. 2).

Example 4. The reduction of methane feed rate and pressure Not to 13.2 g/min and 300 Torr increased the yield of graphene up to 600 nm with a constant geometry to 90 wt.%.

Thus, it is possible to work continuously with high productivity in a wide range of pressures the inventive method has the advantages�society.

A method for the continuous production of graphene, including the decomposition of gaseous carbon-containing material from the group consisting of methane, propane, butane in plasma, and its condensation on the surface, characterized in that the plasma used bulk thermal plasma generated by the plasma torch with a coaxially arranged electrodes, wherein the hollow output electrode - anode has the shape of a nozzle, the cathode is in the form of a rod, a carbonaceous material is fed to a plasma-forming gas into the reaction zone through the vortex chamber, and the surface use the inner surface of the manifold, the bottom of which is made with a hole for passage of gas flow, and the target surface is mounted perpendicular to this flow.


Same patents:

FIELD: nanotechnologies.

SUBSTANCE: inventions relate to nanotechnology and may be used to manufacture catalysts and sorbents. Graphene pumice contains graphenes arranged in parallel at distances of more than 0.335 nm, and amorphous carbon as a binder at their edges, with the graphene-binder ratio from 1:0.1 to 1:1 by mass. The specific area of the surface is more than 1000 m2/g. The absolute hardness is 1 unit by the Mohs scale and less, specific density is 0.008-0.3 g/cm3 for solids, loose specific density of 0.005-0.25 g/cm3 for granules. The composition is produced by burning of a homogeneous powder mix of graphite oxide, unstable organic material and organic and inorganic metal salts with the moisture of all components of 10-15% in a heat-resistant open or tight mould. The source material for the binder is represented by chemical compounds capable of being in a liquid state up to 180°C, not soaking the graphite/graphene surface and damaged at a temperature of not more than 800°C. Graphene pumice is activated by restoration in hydrogen at 400-450°C and pressure of 0.05-0.11 MPa for 10-30 min or in methane at 800-950°C for at least 1 hour at atmospheric pressure with subsequent cooling.

EFFECT: produced sorbents make it possible to multiply increase the capacity of reservoirs for the storage and transportation of natural gas.

15 cl, 8 dwg, 2 tbl, 4 ex

FIELD: chemistry.

SUBSTANCE: graphite-containing component is mixed with a kaolin-based filling agent, dry mixing with simultaneous dispersion successively in a drum and centrifugal mixers is carried out. After that, a magnetised water solution of an alumoborophosphate concentrate, containing a surface-active substance, is introduced, and a wet batch in a screw mixer is carried out. After that, the obtained mass is processed in a tribochemical disperser under conditions of vacuuming and all-around compression to a pressure of 5-20 MPa. The tribochemical disperser includes a hermetic hollow cylindrical case 40, which has flanges 41 and 42 on butt ends, a permeable piston 44 with a rod 45, a drive 46 of reciprocating movement, means for the cavity vacuuming 43, two vacuum gate valves 471 and 472. The piston 44 represents a packet of adjoining each other pairs of metal nets which have the different cell size, located between two protective grids 445. The products are moulded from processed mass with their further thermal processing.

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20 cl, 4 dwg, 2 ex

FIELD: chemistry.

SUBSTANCE: first, particles of thermally expanded graphite are obtained by heating particles of hydrolysed graphite nitrate with specific melt energy equal or higher than 4.7 kJ/g in the atmosphere of products of combustion of liquid or gaseous fuel in air with the coefficient of air excess counted per fuel λ=0.8-1.1. Obtained thermally expanded graphite is compacted to the seeming density from 0.03 to 0.1 g/cm3 by rolling or uniaxial pressing. After that, the material is cut into measured blanks. At least, two measured blanks are subjected to joint compression with obtaining a monolith material. The finished low-density material is made in the form of long-measuring product up to 1500 mm wide.

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10 cl, 3 ex

FIELD: chemistry.

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FIELD: nanotechnology.

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FIELD: electricity.

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FIELD: chemistry.

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14 cl, 2 dwg, 5 tbl

FIELD: chemistry.

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5 tbl

FIELD: process engineering.

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FIELD: chemistry.

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11 cl, 3 dwg, 11 ex

FIELD: chemistry.

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FIELD: medicine.

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2 dwg, 1 tbl, 1 ex

FIELD: physics, optics.

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3 cl, 2 dwg

FIELD: measurement equipment.

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FIELD: medicine.

SUBSTANCE: invention refers to medicine, namely to pharmaceutical engineering, and concerns a method for the quantitative estimation of chemically combined organic substances, first of all, biologically active and medical substances with a nanodiamond surface in its conjugate. The method is based on using the method for the qualitative IR-spectroscopy of the conjugate and model mixtures of the organic substance with the nanodiamond to be detected. IR-spectrum signal intensity/amount of the model mixture organic substance calibration curves are constructed to determine its content in the conjugate.

EFFECT: improving the method.

3 tbl, 5 dwg, 1 ex

FIELD: medicine, pharmaceutics.

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34 cl, 8 ex, 5 tbl, 9 dwg

FIELD: electricity.

SUBSTANCE: invention is related to electrochemical installation intended to shape nanosized coating and may be used in semiconductor and electronics industry. The installation contains a computer, a controller and manipulator 1 mounted at the rack 2 rotatable around vertical axis and equipped with holder 3 for a processed sample 4. Around the manipulator 1 rack there are electrochemical cells 5 with electrodes connected to one pole of current source. The sample 4 submerged to electrochemical cells is connected to the other pole of current source. Holder 3 is installed so that it can be moved in regard to manipulator 1, and at that sample 4 in downwardmost position of holder 3 is placed in one of electrochemical cells. One of electrochemical cells is made as measuring cell 7 to control parameters of the processed sample 4. The installation is equipped with tube-type furnace 8 intended for thermal processing of the sample.

EFFECT: potential determining and setting of the required parameters for obtained nanomaterial against absolute value and conditions of their change.

4 dwg

FIELD: physics.

SUBSTANCE: proposed shutter comprises locally smelting or evaporating mirror metal film located in focal area of the lens and secured by translucent substrate. On radiation side said substrate includes also the ply of translucent liquid of solid sol with nanoparticles in size smaller than radiation wavelength. Mirror film is arranged on said substrate on radiation side or opposite side.

EFFECT: lower threshold of shutter operation.

4 dwg

FIELD: chemistry.

SUBSTANCE: method includes treating the surface of crystalline silicon by electrochemical etching in hydrofluoric acid solution with concentration of 20-30% while supplying current with surface density of 750-1000 mA/cm2 for 5-30 s to obtain hydrophobic silicon or supplying current with surface density of not more than 650 mA/cm2 for 5-30 s to obtain hydrophilic silicon.

EFFECT: method enables to obtain a surface with multimodal nano- or microporosity in a single step.

4 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to synthesis of diamond nanoparticles, which can be used in various fields of technology. Claimed method of synthesis of ultradispersed diamonds includes generation of carbon plasma from carbon-containing substance and its condensation with cooling liquid under conditions of cavitation. As plasma-generating substance any hydrocarbon gas or organic carbon-containing liquid, including one which additionally contains substances, containing heteroatoms, as well as dispersions of carbon particles of non-diamond allotropic shape in organic fluids or water, can be used. Flow of liquid inside flow cavitation apparatus, providing additional cavitation impact on cooling liquid, is used as cooling liquid.

EFFECT: invention makes it possible to increase energy efficiency of realised synthesis of nanodiamonds and provides possibility of managing properties of synthesised nanodiamonds.

3 dwg, 1 tbl