CN116281975A - Method for preparing nano material by alternating current combined plasma - Google Patents
Method for preparing nano material by alternating current combined plasma Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/068—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with silicon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/485—Preparation involving the use of a plasma or of an electric arc
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05H—PLASMA TECHNIQUE; PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS
- H05H1/00—Generating plasma; Handling plasma
- H05H1/24—Generating plasma
- H05H1/26—Plasma torches
- H05H1/32—Plasma torches using an arc
- H05H1/34—Details, e.g. electrodes, nozzles
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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Abstract
The invention relates to a method for preparing nano materials by alternating current combined plasmas, which comprises the steps of preliminarily ionizing buffer gas through a high-frequency alternating current rotary sliding arc under a negative pressure condition, further exciting single-phase or three-phase power frequency discharge, generating stable high-power arc, introducing raw material gas, then generating cracking reaction, and nucleating and growing in a downlink fluidized bed to obtain the nano materials. The invention has reasonable design, prepares carbon black particles, graphene sheets, nitrogen-doped graphene sheets and silicon nitride particles by alternating current combined plasmas under the negative pressure condition, has convenient and fast product separation and recovery, simple process flow, no need of a catalyst and a substrate, low cost, environmental protection and suitability for continuous large-scale preparation of nano materials.
Description
Technical field:
the invention belongs to the technical field of nano material preparation, and particularly relates to a method for preparing a nano material by alternating-current combined plasmas.
The background technology is as follows:
in recent years, research on nano materials is quite active, and the two-dimensional nano materials taking graphene as a typical material have the characteristics of high electron mobility, good thermal conductivity, large specific surface area, strong mechanical strength and the like due to the structural specificity of the two-dimensional nano materials. With the continuous development of plasma technology, the method has unique advantages in the fields of nanomaterial science and technology, in particular in the aspects of preparation, modification and application of nanomaterials.
Chinese patent publication No. CN111453719a discloses a high quality graphene and a preparation method thereof, and the invention adds an oxidizer solution into graphite powder for micro-expansion, and then performs microwave plasma treatment to obtain graphene. According to the method, a microwave plasma technology is introduced into the process of preparing graphene, and the graphene is prepared by taking graphite powder and the like as raw materials through a specific process method, so that the problems of long reaction time, multiple defects of the graphene, and environmental pollution caused by waste liquid are solved, but the operations of washing, purifying, drying and the like are needed in the preparation process, the steps are complex, the operation is complicated, and the equipment price is high.
Chinese patent publication No. CN109534328A discloses a two-dimensional nitrogen doped graphene and a preparation method thereof, the copper sheet is annealed at high temperature, ammonia gas and methane are cracked under the action of a plasma generator, and deposited on the surface of a copper substrate under the catalysis of copper, and the nitrogen doped graphene material is obtained by assembly. The preparation temperature of the nitrogen-doped graphene is reduced to 400 ℃, the reaction time is also greatly shortened, the operation is simple, and the repeatability is good. However, the preparation process requires a substrate, and the yield is low, which is not suitable for mass production.
Chinese patent publication No. CN113200528A discloses a method and apparatus for preparing high purity alpha phase silicon nitride powder, which uses high purity nitrogen plasma to react rapidly with high purity silicon powder by plasma arc under the action of catalyst to obtain amorphous silicon nitride powder, and finally calcining in tube furnace to obtain alpha phase silicon nitride. The product obtained by the method has uniform particle size distribution and higher purity. However, the preparation method still comprises the steps of reacting gas with solid, and high-purity silicon powder is more deposited in a plasma area to prevent the reaction from continuously proceeding.
Compared with other forms of plasmas, the high-frequency alternating current rotary sliding arc plasma has the advantages of simple equipment structure, low cost and convenient operation, and is not limited by pressure change. Sliding arc discharge is therefore widely used and studied in methane gas reforming, pollutant degradation, nanomaterial preparation, modification, and other fields. Compared with high-frequency alternating current, the structure of the generator and the transformer of the single-phase or three-phase power frequency alternating current power supply is simpler, and the performance is excellent. The electric energy loss is less when the same power is output under the same condition, and the energy can be effectively saved. The two alternating current arc plasmas are combined, so that a discharge area can be enlarged, long-time stable discharge can be maintained, and the method is suitable for large-scale preparation of nano materials.
The invention comprises the following steps:
the invention aims at improving the problems existing in the prior art, namely the technical problem to be solved by the invention is to provide a method for preparing the nanomaterial by alternating-current combined plasmas, which has the advantages of simple and reasonable flow, no need of a catalyst and a substrate, low cost, environmental protection and suitability for continuous large-scale preparation of the nanomaterial.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the method for preparing the nano material by using the alternating current combined plasma comprises a gas flow control device, a high-frequency alternating current rotary sliding arc plasma generator, a single-phase or three-phase alternating current arc plasma generator, a fluidized bed and a separation dust removal device which are sequentially connected, wherein the gas outlet end of the separation dust removal device is connected with a tail gas treatment device through an induced air system, and the discharge end of the separation dust removal device is connected with a collecting device, and comprises the following steps:
(1) Opening an induced draft system to adjust the pressure of a plasma reaction area of the high-frequency alternating current rotary sliding arc plasma generator and the single-phase or three-phase alternating current arc plasma generator to form a negative pressure condition;
(2) Introducing buffer gas into a plasma reaction area of a high-frequency alternating current rotary sliding arc plasma generator, and cracking the buffer gas to form rotary sliding arc plasma after starting a high-frequency alternating current power supply; the buffer gas after preliminary ionization enters a plasma reaction area of a single-phase or three-phase alternating current arc plasma generator, a single-phase or three-phase alternating current power supply is started, and stable single-phase or three-phase alternating current arc plasma is formed by the buffer gas after preliminary ionization under the action of the single-phase or three-phase alternating current power supply;
(3) Raw material gas is introduced, the raw material gas sequentially passes through a plasma reaction area of a high-frequency alternating current rotary sliding arc plasma generator and a single-phase or three-phase alternating current arc plasma generator, the raw material gas enters a fluidized bed after being cracked, and free radicals continue to grow into nano powder materials through nucleation and growth;
(4) The nano material product treated in the step (3) enters a separation dust removal device, and the separated nano material product enters a collecting device and is cooled to obtain a nano material; and the tail gas separated and output is sent into a tail gas treatment device through an induced air system.
Further, the gas flow control device is a connected rotor flowmeter and a mass flowmeter; the induced air system is an induced draft fan or a vacuum pump; the separating and dedusting device is a cyclone separator and a cloth bag dust remover which are connected.
Further, the high-frequency alternating current rotary sliding arc plasma generator is connected with an electrode air cooling device; the single-phase or three-phase alternating-current arc plasma generator is provided with a leakage protection device.
Further, the nanomaterial is carbon black particles, graphene sheets, nitrogen-doped graphene sheets or silicon nitride particles.
Further, the fluidized bed adopts a structure of a descending fluidized bed, and the gas pressure is kept at a negative pressure condition of 20-90 kPa.
Further, in the step (2), the power of the high-frequency alternating current rotary sliding arc plasma generator is 1-200kW, and the frequency is 30kHz-300 kHz; the power of the single-phase or three-phase alternating-current arc plasma generator is 5 kW-2000 kW, and the frequency is 50Hz.
Further, in the step (2), the buffer gas is one or more of argon, helium and neon, and the total gas flow is 4-100L/min; in the step (3), the raw material gas is one or more of methane, ethane, propane, nitrogen, ammonia, nitrogen, silane and hydrogen, which are respectively used as a carbon source, a nitrogen source, a silicon source and an additive, and the total gas flow is 0.5-20L/min.
Further, the flow ratio of the buffer gas to the raw material gas is between 1:1 and 20:1; the residence time of the buffer gas, the raw material gas and the solid product in the fluidized bed is 0.5 to 10s.
Further, in the step (2), the electrode of the single-phase or three-phase alternating-current arc plasma generator consists of two or three graphite rods, when the single-phase alternating-current arc plasma generator is adopted, the electrode of the single-phase alternating-current arc plasma generator consists of two graphite rods, the electrode and the feed gas are in the same horizontal plane, and the included angle between the two graphite rods is 0-180 degrees; when the three-phase alternating-current arc plasma generator is adopted, when the electrodes of the three-phase alternating-current arc plasma generator consist of three graphite rods, the three graphite rods are arranged in the same horizontal plane according to phase difference or in parallel, and the phase difference arrangement included angle is 120 degrees.
Furthermore, the electrode distance of the single-phase or three-phase alternating current arc plasma generator can be automatically adjusted after the graphite electrode is stripped, and the electrode distance of normal discharge of the single-phase or three-phase alternating current arc after arc striking of the alternating current sliding arc is enlarged from 1-10mm to 1-40mm; the temperature in the plasma region is 500K-10000K.
Compared with the prior art, the invention has the following effects: the invention has reasonable design, the buffer gas is primarily ionized by the high-frequency alternating current rotary sliding arc under the negative pressure condition, thereby exciting single-phase or three-phase power frequency discharge, generating stable high-power arc, generating cracking reaction after the raw material gas is introduced, nucleating and growing in the descending fluidized bed to obtain the nano material, the whole method adopts gas phase raw material, the product separation and recovery are convenient, the process flow is simple, a catalyst and a substrate are not needed, the cost is low, and the method is green and environment-friendly, and is suitable for continuously preparing the nano material on a large scale.
Description of the drawings:
FIG. 1 is a flow chart of an embodiment of the present invention;
FIG. 2 is an SEM image of carbon black particles of example 1 of the present invention;
fig. 3 is an SEM image of graphene prepared in example 2 of the present invention;
FIG. 4 is an SEM image of nitrogen-doped graphene prepared in example 3 of the present invention;
fig. 5 is an SEM image of nitrogen-doped graphene prepared in comparative example 2 in the present invention.
The specific embodiment is as follows:
the invention will be described in further detail with reference to the drawings and the detailed description.
In the description of the present invention, it should be understood that the terms "longitudinal," "transverse," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the present invention, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
As shown in figure 1, the device adopted in the method for preparing the nano material by using the alternating current combined plasma comprises a gas flow control device, a high-frequency alternating current rotary sliding arc plasma generator, a single-phase or three-phase alternating current arc plasma generator, a fluidized bed and a separation dust removal device which are sequentially connected, wherein the gas outlet end of the separation dust removal device is connected with a tail gas treatment device through an induced air system, and the discharge end of the separation dust removal device is connected with a collecting device. Under the negative pressure condition, buffer gas is primarily ionized through a high-frequency alternating current rotary sliding arc, single-phase or three-phase power frequency discharge is excited, stable high-power arc is generated, raw material gas is introduced and then subjected to cracking reaction, and the nano material is obtained through nucleation and growth in a downlink fluidized bed. The method for preparing the nano material specifically comprises the following steps:
(1) Opening an induced draft system to adjust the pressure of a plasma reaction area of a high-frequency alternating current rotary sliding arc plasma generator and a single-phase or three-phase alternating current arc plasma generator, and forming a negative pressure condition in the plasma reaction area;
(2) Introducing buffer gas into a plasma reaction area of a high-frequency alternating current rotary sliding arc plasma generator, and cracking the buffer gas to form rotary sliding arc plasma after starting a high-frequency alternating current power supply; the buffer gas after preliminary ionization enters a plasma reaction area of a single-phase or three-phase alternating current arc plasma generator, a single-phase or three-phase alternating current power supply is started, and stable single-phase or three-phase alternating current arc plasma is formed by the buffer gas after preliminary ionization under the action of the single-phase or three-phase alternating current power supply;
(3) Raw material gas is introduced, the raw material gas sequentially passes through a plasma reaction area of a high-frequency alternating current rotary sliding arc plasma generator and a single-phase or three-phase alternating current arc plasma generator, the raw material gas enters a fluidized bed after being cracked, and free radicals continue to grow into nano powder materials through nucleation and growth;
(4) The nano material product treated in the step (3) enters a separation dust removal device, and the separated nano material product enters a collecting device and is cooled to obtain a nano material; and the tail gas separated and output is sent into a tail gas treatment device through an induced air system.
In this embodiment, the gas flow control device is a connected rotameter and a mass flowmeter, and the gas flow is adjusted by the rotameter and the mass flowmeter. Preferably, the flow range of the mass flowmeter is 0-200L/min, and preferably 50-150L/min.
In this embodiment, the induced air system is an induced draft fan or a vacuum pump.
In this embodiment, the separation dust collector is a cyclone separator and a bag-type dust collector which are connected, and the nanomaterial obtained in the step (4) is separated from the gas product by the cyclone separator and the bag-type dust collector, and the gas is exhausted or recycled. Wherein the height of the cyclone separator is 200-600cm, and the diameter of the cyclone separator is 40-60cm.
In the embodiment, the collecting device is divided into ceramic or corundum pipes with the height of 20-40cm and the diameter of 10-20cm, and stainless steel sedimentation pipes with the height of 50-100cm and the diameter of 20-40cm, and the collecting device can be replaced according to the replacement of the fluidized bed reactor.
In this embodiment, the high-frequency ac rotating and sliding arc plasma generator is connected with an electrode air cooling device for air cooling the electrode. The power of the high-frequency alternating current rotary sliding arc plasma generator is 1-200kW, the frequency is 30kHz-300kHz, the electrode of the high-frequency alternating current rotary sliding arc plasma generator consists of a conical stainless steel electrode and cylindrical high-purity graphite, the structure of the high-frequency alternating current rotary sliding arc plasma generator is the prior art, for example, refer to a sliding arc plasma device disclosed by CN216217684U, and the motor structure of the high-frequency alternating current rotary sliding arc plasma generator is not repeated.
In this embodiment, the single-phase or three-phase ac arc plasma generator is provided with a leakage protection device for leakage protection. The power of the single-phase or three-phase alternating-current arc plasma generator is 5 kW-2000 kW, and the frequency is 50Hz. The single-phase or three-phase alternating-current arc plasma generator is positioned above the alternating-current rotary sliding arc, the electrode of the single-phase or three-phase alternating-current arc plasma generator consists of two or three graphite rods, when the single-phase alternating-current arc plasma generator is adopted, the electrode of the single-phase alternating-current arc plasma generator consists of two graphite rods, the electrode and the feed gas are in the same horizontal plane, and the included angle of the two graphite rods is 0-180 degrees, namely, the two graphite rods are basically parallel or opposite. When the three-phase alternating current arc plasma generator is adopted, when the electrode of the three-phase alternating current arc plasma generator consists of three graphite rods, the three graphite rods are uniformly arranged or basically arranged in parallel according to the phase difference in the same horizontal plane, namely: the electrodes are uniformly arranged according to the phase difference arrangement included angle of 120 degrees, or the included angle of 0 degree of each electrode is used for realizing the basically parallel arrangement.
In this embodiment, the nanomaterial is a solid powdery nanomaterial such as carbon black particles, graphene sheets, nitrogen-doped graphene sheets, or silicon nitride. The invention utilizes the advantage of easy arcing of high-frequency alternating current rotating arc, and effectively expands the plasma reaction area by matching with the characteristic of high efficiency of single-phase or three-phase alternating current plasmas. Obtaining carbon black particles, graphene materials, nitrogen-doped graphene and silicon nitride by directly cracking a gas reactant, wherein the particle size of the obtained carbon black particles is 50-100nm; the size of the graphene sheet layer is 100-300nm, and the number of layers is 2-6; the size of the nitrogen-doped graphene sheet layer is 100-200nm, and the number of layers is 3-10; the particle size of the silicon nitride particles is 10-50 nm; the kind and grain size of the nanometer material can be regulated and controlled by the kind of the introduced buffer gas, the kind of the raw material gas and the technological conditions.
In the embodiment, the fluidized bed adopts a structure of a descending fluidized bed reactor, and the gas pressure is kept at a negative pressure condition of 20-90 kPa and is regulated by a vacuum pump. Further, the fluidized bed is connected with the single-phase or three-phase alternating-current arc plasma reactor through a flaring, the diameter of the fluidized bed is 3-8 times of the diameter of the single-phase or three-phase alternating-current arc plasma reactor, and the height of the fluidized bed is 3-10 times of the height of the single-phase or three-phase alternating-current arc plasma reactor. The residence time of the buffer gas, the raw material gas and the solid product in the fluidized bed is 0.5-10s.
In this embodiment, in the step (2), the buffer gas is one or more of argon, helium and neon that are easy to crack, the total gas flow is 4-100L/min, preferably 20-80L/min, and the gas flow is adjusted by a rotor flowmeter and a mass flowmeter.
In the embodiment, in the step (3), the raw material gas is one or more of methane, ethane, propane, nitrogen, ammonia, nitrogen, silane and hydrogen, which are respectively used as a carbon source, a nitrogen source, a silicon source and an additive, the total gas flow is 0.5-20L/min, preferably 2-15L/min, and the gas flow is adjusted by a rotor flowmeter and a mass flowmeter; the flow ratio of the buffer gas to the raw material gas is between 1:1 and 20:1, preferably between 5:1 and 10:1.
In the embodiment, the electrode distance of the single-phase or three-phase alternating current arc plasma generator can be automatically adjusted after the graphite electrode is stripped, and the electrode distance of normal discharge of the single-phase or three-phase alternating current arc after arc striking of the alternating current sliding arc is enlarged from 1-10mm to 1-40mm; the temperature in the plasma region is 500K-10000K.
In this embodiment, the high frequency ac arc is able to continuously break down the buffer gas between the electrodes, making it less prone to ionization. Compared with high-frequency alternating current, the structure of the generator and the transformer of the single-phase or three-phase power frequency alternating current power supply is simpler, and the performance is excellent. The single-phase or three-phase alternating current has less electric energy loss when outputting the same power under the same condition, and can effectively save energy. The two types of alternating current arc plasmas are combined, and the alternating current rotary sliding arc plasmas can run from bottom to top to form plasma groups, so that single-phase or three-phase alternating current arcs are easier to form arcs, the electrode distance can be prolonged, the loss of the electrode is reduced, and the plasma reaction area is increased. Meanwhile, the negative pressure condition can increase the gas flow rate, reduce the gas density and enable the gas difficult to ionize more easily. And the combination of the nano-material and the descending fluidized bed can enable the free radical nucleation and growth of the nano-material to be more sufficient, and the yield is increased. The method can maintain stable discharge for a long time, and is suitable for large-scale preparation of nano materials for a long time. After the two plasmas are combined, the synthesis efficiency of the carbon material is improved, and a stable plasma region can be formed and expanded to achieve the effect of long-time large-scale synthesis. Based on the method, the carbon black particles, the graphene, the nitrogen doped graphene and the silicon nitride particles are prepared by using alternating current combined plasmas and gas as raw materials. The process has the advantages of convenient separation and recovery of the product, simple process flow, no need of a catalyst and a substrate, low cost, environmental protection and suitability for continuous large-scale preparation of the nano material.
The specific implementation process comprises the following steps:
(1) Starting an induced draft fan or a vacuum pump to adjust the pressure of a plasma reaction area, and starting a plasma electrode air cooling device, a leakage protection device and a mass flowmeter;
(2) Introducing buffer gas into a plasma reaction area, starting a high-frequency alternating current power supply, and then cracking to form rotary sliding arc plasma, wherein the buffer gas subjected to preliminary ionization forms stable single-phase or three-phase alternating current arc plasma under the action of the single-phase or three-phase alternating current power supply;
(3) Introducing raw material gas into a plasma generator and a downlink fluidized bed, passing through a combined plasma region, cracking the raw material gas, entering the downlink fluidized bed, and continuing to grow into nano powder materials by nucleation and growth of free radicals;
(4) The nano material product treated in the step (3) is separated and enters a collecting device through a cyclone separator, a cloth bag collector and other collecting systems, and the nano material is obtained after cooling; the tail gas is treated and purified properly by an induced draft system and then is reused as raw material.
Example 1
The method for preparing the carbon black particles by using the alternating current combined plasma comprises the following specific steps:
(1) Starting a vacuum pump, adjusting the pressure of a plasma area to 80 kPa, starting a plasma electrode air cooling device, setting to 60L/min, starting a mass flowmeter, and starting a leakage protection device;
(2) Argon is introduced into a plasma reaction area, the flow rates are respectively adjusted to be 50L/min through a rotor flowmeter and a mass flowmeter, a high-frequency alternating current power supply is started and then cracked to form rotary sliding arc plasma, and the primarily ionized argon forms stable three-phase alternating current arc plasma under the action of the three-phase alternating current power supply;
(3) Introducing ethane into a plasma generator and a downlink fluidized bed, regulating the flow to be 10L/min respectively through a rotor flowmeter and a mass flowmeter, passing through a combined plasma region, and after ethane is cracked, introducing the ethane into the downlink fluidized bed, and continuing to nucleate and grow free radicals;
(4) The carbon black particles obtained after the reaction are separated along with argon gas and enter a collecting device through a cyclone separator, a cloth bag collector and other collecting systems, products are obtained after cooling, tail gas is treated and purified properly through an induced draft system and is reused as a raw material;
(5) The collected carbon black particles are black nano powder and are in spherical agglomeration shape, and the diameter is 50-100 nm. The morphology is shown in figure 2.
Example 2
The method for preparing the graphene by utilizing the alternating current combined plasma comprises the following specific steps:
(1) Starting a vacuum pump, adjusting the pressure of a plasma area to 60 kPa, starting a plasma electrode air cooling device, setting the pressure to 60L/min, starting a mass flowmeter, and starting a leakage protection device;
(2) Argon and helium are introduced into a plasma reaction area, the flow rates are respectively adjusted to be 100L/min and 10L/min by a rotor flowmeter and a mass flowmeter, a high-frequency alternating current power supply is started and then cracked to form rotary sliding arc plasma, and the primarily ionized argon forms stable three-phase alternating current arc plasma under the action of the three-phase alternating current power supply;
(3) Methane and hydrogen are introduced into a plasma generator and a descending fluidized bed, the flow rates are adjusted to be 10L/min and 2L/min respectively through a rotor flowmeter and a mass flowmeter, and the methane and the hydrogen pass through a combined plasma region to be cracked and then enter the descending fluidized bed, so that free radicals continue to nucleate and grow;
(4) The graphene sheets obtained after the reaction are separated along with argon and helium gas through a cyclone separator, a cloth bag collector and other collecting systems, and enter a collecting device, products are obtained after cooling, and tail gas is reused as raw materials after being properly treated and purified through an induced draft system;
(5) The collected graphene is black nano powder, and is in a flake shape, and the diameter is 100-300 nm. The morphology is shown in figure 3.
Example 3
The method for preparing the nitrogen-doped graphene by utilizing the alternating-current combined plasma comprises the following specific steps of:
(1) Starting a vacuum pump, adjusting the pressure of a plasma area to be 50 kPa, starting a plasma electrode air cooling device, setting the pressure to be 60L/min, starting a mass flowmeter, and starting a leakage protection device;
(2) Argon and neon are introduced into a plasma reaction area, the flow rates are respectively adjusted to 80L/min and 20L/min by a rotor flowmeter and a mass flowmeter, a high-frequency alternating current power supply is started and then cracked to form rotary sliding arc plasma, and the primarily ionized argon and neon form stable three-phase alternating current arc plasma under the action of the three-phase alternating current power supply;
(3) Methane and nitrogen are introduced into a plasma generator and a descending fluidized bed, the flow rates are adjusted to be 5L/min and 15L/min respectively through a rotor flowmeter and a mass flowmeter, and after the methane and the nitrogen are cracked through a combined plasma area, the methane and the nitrogen enter the descending fluidized bed, and free radicals continue to nucleate and grow;
(4) The nitrogen doped graphene sheets obtained after the reaction are separated along with argon and neon through a multi-stage cyclone separator, a cloth bag collector and other collecting systems, and enter a collecting device, products are obtained after cooling, and tail gas is reused as raw materials after being properly treated and purified through an induced draft system;
(5) The collected nitrogen doped graphene is black nano powder, and is in a flake shape, and the diameter is 100-200 nm. The morphology is shown in figure 4.
Comparative example 1
The method for preparing the nitrogen-doped graphene by utilizing the alternating-current combined plasma comprises the following specific steps of:
(1) Starting an induced draft fan, wherein the pressure of a plasma area is normal pressure, starting a plasma electrode air cooling device, setting the pressure to be 60L/min, starting a mass flowmeter, and starting a leakage protection device;
(2) Argon and neon are introduced into a plasma reaction area, the flow rates are respectively adjusted to 80L/min and 20L/min by a rotor flowmeter and a mass flowmeter, a high-frequency alternating current power supply is started and then cracked to form rotary sliding arc plasma, and the primarily ionized argon and neon form three-phase alternating current arc plasma under the action of the three-phase alternating current power supply;
(3) Methane and nitrogen are introduced into the plasma generator and the descending fluidized bed, the flow rates are adjusted to be 5L/min and 15L/min respectively through a rotor flowmeter and a mass flowmeter, and the arc is extinguished and the ignition fails after passing through the combined plasma region.
Comparative example 2
The method for preparing the nitrogen-doped graphene by utilizing the alternating-current combined plasma comprises the following specific steps of:
(1) Starting a vacuum pump, adjusting the pressure of a plasma area to be 50 kPa, starting a plasma electrode air cooling device, setting the pressure to be 60L/min, starting a mass flowmeter, and starting a leakage protection device;
(2) Argon and neon are introduced into a plasma reaction area, the flow rates are respectively adjusted to 80L/min and 20L/min by a rotor flowmeter and a mass flowmeter, a high-frequency alternating current power supply is started and then cracked to form rotary sliding arc plasma, and the primarily ionized argon and neon form three-phase alternating current arc plasma under the action of the three-phase alternating current power supply;
(3) Methane and nitrogen are introduced into a plasma generator and a downlink fluidized bed, the flow rates are adjusted to be 5L/min and 15L/min respectively through a rotor flowmeter and a mass flowmeter, the methane and the nitrogen pass through a combined plasma region, are directly introduced into a collecting device after being cracked, and are cooled to obtain a product, and finally, the gas and the nitrogen doped graphene sheet are separated;
(4) The yield of the product directly entering the collecting device is reduced by 50-70% compared with the yield of the product directly entering the collecting device after passing through the descending fluidized bed.
The invention has the advantages that:
(1) The invention can prepare the nano material with high value in the practical research field and industrial application, and can regulate and control the morphology structure; carbon black particles, graphene sheets, nitrogen-doped graphene sheets and silicon nitride particles are prepared by alternating current combined plasmas under the negative pressure condition, products are separated and recovered conveniently, the process flow is simple, a catalyst and a substrate are not needed, the cost is low, the environment is protected, and the method is suitable for continuously preparing nano materials on a large scale; negative pressure operation can be performed, so that the gas flow rate is increased, the throughput per unit time is increased, and the yield is increased;
(2) According to the invention, the conductive carbon black and the small-diameter graphene can be prepared and stacked into a grape-shaped structure, and the number of layers is 2-6; the conductive carbon black and graphene in the product form a one-dimensional and two-dimensional structure, so that the combined conductivity is enhanced, and nitrogen-doped graphene and silicon nitride can be directly synthesized in one step by utilizing nitrogen, ammonia and silane gas reactants without a solid catalyst;
(3) Compared with other plasma modes, the invention has higher efficiency and large treatment capacity, and reduces the electric energy consumption; the synthesis efficiency of the nano material is improved, the discharge gap is increased, carbon deposition between electrodes is reduced, and a stable plasma region can be formed and expanded to achieve the effect of long-time large-scale synthesis;
(4) The invention combines the alternating-current combined plasma with the descending fluidized bed, increases the reaction time, enables free radicals to fully nucleate and grow, and improves the yield of the nano material.
If the invention discloses or relates to components or structures fixedly connected with each other, then unless otherwise stated, the fixed connection is understood as: detachably fixed connection (e.g. using bolts or screws) can also be understood as: the non-detachable fixed connection (e.g. riveting, welding), of course, the mutual fixed connection may also be replaced by an integral structure (e.g. integrally formed using a casting process) (except for obviously being unable to use an integral forming process).
In addition, terms used in any of the above-described aspects of the present disclosure to express positional relationship or shape have meanings including a state or shape similar to, similar to or approaching thereto unless otherwise stated.
Any part provided by the invention can be assembled by a plurality of independent components, or can be manufactured by an integral forming process.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same; while the invention has been described in detail with reference to the preferred embodiments, those skilled in the art will appreciate that: modifications may be made to the specific embodiments of the present invention or equivalents may be substituted for part of the technical features thereof; without departing from the spirit of the invention, it is intended to cover the scope of the invention as claimed.
Claims (10)
1. A method for preparing a nano material by alternating current combined plasmas is characterized by comprising the following steps of: including gas flow control device, high frequency alternating current rotary sliding arc plasma generator, single-phase or three-phase alternating current arc plasma generator, fluidized bed and the separation dust collector who connects gradually, separation dust collector's end of giving vent to anger is connected with tail gas processing apparatus through induced air system, and separation dust collector's discharge end is connected with collection device, includes the following step:
(1) Opening an induced draft system to adjust the pressure of a plasma reaction area of the high-frequency alternating current rotary sliding arc plasma generator and the single-phase or three-phase alternating current arc plasma generator to form a negative pressure condition;
(2) Introducing buffer gas into a plasma reaction area of a high-frequency alternating current rotary sliding arc plasma generator, and cracking the buffer gas to form rotary sliding arc plasma after starting a high-frequency alternating current power supply; the buffer gas after preliminary ionization enters a plasma reaction area of a single-phase or three-phase alternating current arc plasma generator, a single-phase or three-phase alternating current power supply is started, and stable single-phase or three-phase alternating current arc plasma is formed by the buffer gas after preliminary ionization under the action of the single-phase or three-phase alternating current power supply;
(3) Raw material gas is introduced, the raw material gas sequentially passes through a plasma reaction area of a high-frequency alternating current rotary sliding arc plasma generator and a single-phase or three-phase alternating current arc plasma generator, the raw material gas enters a fluidized bed after being cracked, and free radicals continue to grow into nano powder materials through nucleation and growth;
(4) The nano material product treated in the step (3) enters a separation dust removal device, and the separated nano material product enters a collecting device and is cooled to obtain a nano material; and the tail gas separated and output is sent into a tail gas treatment device through an induced air system.
2. The method for preparing the nano material by using the alternating current combined plasma according to claim 1, wherein the method comprises the following steps of: the gas flow control device is a rotor flowmeter and a mass flowmeter which are connected; the induced air system is an induced draft fan or a vacuum pump; the separating and dedusting device is a cyclone separator and a cloth bag dust remover which are connected.
3. The method for preparing the nano material by using the alternating current combined plasma according to claim 1, wherein the method comprises the following steps of: the high-frequency alternating current rotary sliding arc plasma generator is connected with an electrode air cooling device; the single-phase or three-phase alternating-current arc plasma generator is provided with a leakage protection device.
4. The method for preparing the nano material by using the alternating current combined plasma according to claim 1, wherein the method comprises the following steps of: the nano material is carbon black particles, graphene sheets, nitrogen doped graphene sheets or silicon nitride particles.
5. The method for preparing the nano material by using the alternating current combined plasma according to claim 1, wherein the method comprises the following steps of: the fluidized bed adopts a structure of a descending fluidized bed, and the gas pressure is kept at a negative pressure condition of 20-90 kPa.
6. The method for preparing the nano material by using the alternating current combined plasma according to claim 1, wherein the method comprises the following steps of: in the step (2), the power of the high-frequency alternating current rotary sliding arc plasma generator is 1-200kW, and the frequency is 30kHz-300 kHz; the power of the single-phase or three-phase alternating-current arc plasma generator is 5 kW-2000 kW, and the frequency is 50Hz.
7. The method for preparing the nano material by using the alternating current combined plasma according to claim 1, wherein the method comprises the following steps of: in the step (2), the buffer gas is one or more of argon, helium and neon, and the total gas flow is 4-100L/min; in the step (3), the raw material gas is one or more of methane, ethane, propane, nitrogen, ammonia, nitrogen, silane and hydrogen, which are respectively used as a carbon source, a nitrogen source, a silicon source and an additive, and the total gas flow is 0.5-20L/min.
8. The method for preparing the nano material by using the alternating current combined plasma according to claim 1, wherein the method comprises the following steps of: the flow ratio of the buffer gas to the raw material gas is between 1:1 and 20:1; the residence time of the buffer gas, the raw material gas and the solid product in the fluidized bed is 0.5 to 10s.
9. The method for preparing the nano material by using the alternating current combined plasma according to claim 1, wherein the method comprises the following steps of: in the step (2), the electrode of the single-phase or three-phase alternating-current arc plasma generator consists of two or three graphite rods, and when the single-phase alternating-current arc plasma generator is adopted, the electrode of the single-phase alternating-current arc plasma generator consists of two graphite rods, the electrode and the feed gas are in the same horizontal plane, and the included angle between the two graphite rods is 0-180 degrees; when the three-phase alternating-current arc plasma generator is adopted, when the electrodes of the three-phase alternating-current arc plasma generator consist of three graphite rods, the three graphite rods are arranged in the same horizontal plane according to phase difference or in parallel, and the phase difference arrangement included angle is 120 degrees.
10. The method for preparing the nano material by using the alternating current combined plasma according to claim 9, wherein the method comprises the following steps: the electrode distance of the single-phase or three-phase alternating current arc plasma generator can be automatically adjusted after the graphite electrode is stripped, and the electrode distance of normal discharge of the single-phase or three-phase alternating current arc after arc striking of the alternating current sliding arc is enlarged from 1-10mm to 1-40mm; the temperature in the plasma region is 500K-10000K.
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