CN111632558B - Device and method for continuously preparing nano material or preparing modified nano material - Google Patents

Device and method for continuously preparing nano material or preparing modified nano material Download PDF

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CN111632558B
CN111632558B CN202010451942.7A CN202010451942A CN111632558B CN 111632558 B CN111632558 B CN 111632558B CN 202010451942 A CN202010451942 A CN 202010451942A CN 111632558 B CN111632558 B CN 111632558B
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gas
fluidized bed
bed reactor
jet mill
recovery chamber
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CN111632558A (en
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靳玉广
杨裕生
彭江
周春梅
戴翼虎
杨艳辉
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Nanjing Bank Innovation Materials Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/24Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005Separating solid material from the gas/liquid stream
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1836Heating and cooling the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • B02C19/0012Devices for disintegrating materials by collision of these materials against a breaking surface or breaking body and/or by friction between the material particles (also for grain)
    • B02C19/0043Devices for disintegrating materials by collision of these materials against a breaking surface or breaking body and/or by friction between the material particles (also for grain) the materials to be pulverised being projected against a breaking surface or breaking body by a pressurised fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/16Preparation
    • C01B32/162Preparation characterised by catalysts
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/184Preparation
    • C01B32/186Preparation by chemical vapour deposition [CVD]
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof

Abstract

The invention discloses a device for continuously preparing nano materials or modified nano materials, which comprises a fluidized bed reactor and a jet mill, wherein a catalyst or the nano materials to be modified are fed into the fluidized bed reactor through the jet mill. The invention also discloses a method for continuously preparing the nano material or preparing the modified nano material by using the device. The device of the invention inputs the catalyst or the nano material to be modified into the fluidized bed reactor through the jet mill, effectively enhances the dispersibility of the catalyst or the nano material to be modified, thereby solving the problem that the fine granular catalyst and the nano material to be modified in the reactor are easy to agglomerate in the reaction process.

Description

Device and method for continuously preparing nano material or preparing modified nano material
Technical Field
The invention relates to a device for continuously preparing a nano material or a modified nano material and a method for continuously preparing the nano material or the modified nano material by using the device, belonging to the technical field of preparation of the nano material.
Background
The nano material is considered as one of the most important novel materials in the present and future, when the particle size is as small as nanometer, the nano material has special effects such as surface and interface effect, quantum size effect, small size effect and macroscopic quantum tunneling effect, and the special effects enable the nano material to present new characteristics in the aspects of sound, light, electricity, magnetism, thermal property and the like. With the continuous development of nanotechnology, more and more nanomaterials are gradually prepared in batches and are practically applied.
The chemical vapor phase method is a method for realizing the batch preparation of nano materials at present, and is widely applied to the aspects of substance purification, new crystal development, thin film material preparation, material modification and the like. The method has the advantages of simple device, mild reaction condition, easy regulation and control, low cost, easy scale production realization and the like, and the main reactor forms comprise a fixed bed reactor, a fluidized bed reactor and a rotary kiln reactor. The catalyst is usually used when the nano material is prepared by using a chemical vapor deposition method, the used catalyst is usually a micron-sized or nano-sized material, the material has a large specific surface area due to the small particle size, so that catalyst particles are easy to agglomerate, mass transfer and heat transfer inside a reactor are easy to be uneven due to the agglomeration of the catalyst particles, the reaction efficiency is reduced, the reaction is terminated, and the obtained final product has a local agglomeration phenomenon. Similarly, when the nano material is modified, the large specific surface area of the nano material itself is easy to cause particle agglomeration, so that the modification is not uniform, and finally, the product agglomeration phenomenon occurs.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a device for continuously preparing nano materials or preparing modified nano materials, which inputs catalysts or nano materials to be modified into a fluidized bed reactor through a jet mill, effectively enhances the dispersity of the catalysts or the nano materials to be modified, and thereby improves the problem that fine granular catalysts and the nano materials to be modified in the reactor are easy to agglomerate in the chemical vapor deposition reaction process.
The technical problem to be solved by the invention is to provide a method for continuously preparing nano materials or preparing modified nano materials by using the device, and the method utilizes the airflow pulverization to enhance the dispersity of the catalyst or the nano materials to be modified, thereby effectively improving the mass transfer and heat transfer efficiency in the reactor and further improving the reaction efficiency of solid particles and reaction gas.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the device for continuously preparing the nano material or preparing the modified nano material comprises a fluidized bed reactor and a jet mill, wherein a catalyst or the nano material to be modified is fed into the fluidized bed reactor through the jet mill.
The device also comprises a feed hopper and a screw feeding device, wherein the feed hopper is arranged above the screw feeding device, a discharge hole of the screw feeding device is connected with the airflow crusher, and a power mechanism of the screw feeding device is a motor.
The device also comprises a recovery chamber and a degassing device communicated with the recovery chamber, wherein a gas-solid separator is arranged in the recovery chamber, a discharge port of the fluidized bed reactor is communicated with the recovery chamber through a pipeline, after a gas-solid mixture entering the recovery chamber passes through the gas-solid separator, the gas is discharged through a tail gas port at the top of the recovery chamber, and solid substances enter the degassing device from the bottom of the recovery chamber to be degassed and then are discharged from a discharge port at the bottom of the degassing device.
Wherein, the gas inlet of the fluidized bed reactor is arranged at the bottom of the fluidized bed reactor, and the reaction gas entering the fluidized bed reactor through the gas inlet enters the reaction zone of the fluidized bed reactor after passing through the gas distributor; the discharge port of the fluidized bed reactor is positioned at the top of the fluidized bed reactor.
Wherein, be equipped with heating device in the fluidized bed reactor, further preferred, heating device is for setting up the heat exchange tube in fluidized bed reactor's lateral wall.
The method for continuously preparing the nano material or preparing the modified nano material by utilizing the device comprises the following steps:
(1) Starting a heating device to enable the fluidized bed reactor to reach a reaction temperature;
(2) Continuously feeding the catalyst or the nano material to be modified into a jet mill through a screw feeding device;
(3) The materials are dispersed by a jet mill in a high shearing way and then are carried into the fluidized bed reactor by carrier gas;
(4) Introducing reaction gas into the fluidized bed reactor, wherein the reaction gas enters a reaction zone through a gas distributor and performs chemical vapor deposition reaction with highly dispersed materials; the reacted product enters a recovery chamber through a discharge hole at the top of the fluidized bed reactor;
(5) And after gas-solid separation is carried out on the product entering the recovery chamber, gas is discharged from a tail gas port at the top of the recovery chamber, and solid enters a degassing device from the recovery chamber, is degassed and then is discharged from a discharge port.
Wherein in the step (3), the gas-solid ratio in the jet mill is 0.05-5 g/L.
Wherein in the step (4), the reaction space velocity is 5-10000 h -1 The superficial gas velocity of the gas is 0.05-3 m/s.
The principle of inputting materials into the fluidized bed reactor by adopting the jet mill is as follows: the jet milling is to use compressed air or superheated steam to generate supersonic airflow through a nozzle with certain pressure as a carrier of material particles, so that the particles obtain huge kinetic energy, impact can be generated between two opposite moving particles, and the airflow can also generate impact shearing action on the material particles, thereby realizing the dispersion of the material and preventing the material with smaller particle size from agglomerating. The solid phase particles entering the reactor are in a highly dispersed state, and the gas phase can fully contact and react with the solid phase; in addition, the heat in the reactor can be transferred to the reactants not only through heat conduction and radiation transfer but also through convection, namely the high dispersion of solid-phase particles and the back mixing of airflow can promote the heat transfer among the reactant particles, so that the temperature in the reactor is uniform.
Has the beneficial effects that:
1. the device of the invention applies jet milling to the preparation of nano materials by a chemical vapor deposition method, effectively improves the dispersibility of raw material powder, thereby solving the problem of easy agglomeration caused by huge specific surface area of the material;
2. the device effectively improves the mass transfer and heat transfer efficiency in the reactor, thereby effectively improving the reaction efficiency, namely, the dispersed solid-phase particles can more efficiently react with the gas phase in the reactor, so that the problems of local bonding and uneven local temperature of reactants are thoroughly eliminated in the reactor, and the uniform distribution of the concentration and temperature of the reactants is realized, thereby ensuring that the obtained product is uniform and has no caking problem;
3. the method realizes the continuous production of the nano material, avoids the difference of product quality caused by different batches in the intermittent production process, can be used for preparing or modifying various nano materials, and has wide application range.
Drawings
FIG. 1 is a system schematic of the apparatus of the present invention.
Detailed Description
The invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the description of the embodiments is only for illustrating the present invention and should not be taken as limiting the invention as detailed in the claims.
Example 1
As shown in FIG. 1, the apparatus for continuously preparing nano-materials or preparing modified nano-materials according to the present invention comprises a feed hopper 2, a screw feeding device 3, a jet mill 4, a fluidized bed reactor 9, a recovery chamber 14 and a degassing device 17; the feeding hopper 2 is arranged above the screw feeding device 3, a discharge port of the screw feeding device 3 is connected with the airflow crusher 4, a power mechanism of the screw feeding device 3 is a motor 1, the motor 1 rotates to drive a screw in the screw feeding device 3 to rotate, so that a catalyst or a nano material to be modified is fed into the airflow crusher 4, a carrier gas inlet 5 is arranged at the lower part of the airflow crusher 4, the discharge port of the airflow crusher 4 is connected with a feed port 7 of the fluidized bed reactor 9, an air inlet 6 is arranged at the bottom of the fluidized bed reactor 9, a reaction gas entering the fluidized bed reactor 9 through the air inlet 6 enters a reaction zone of the fluidized bed reactor 9 after passing through a gas distributor 8, and a heat exchange tube 10 is arranged in the side wall of the reaction zone; the top of the fluidized bed reactor 9 is provided with a discharge port 11, the discharge port 11 of the fluidized bed reactor 9 is communicated with a recovery chamber 14 through a pipeline, a gas-solid separator 13 is arranged in the recovery chamber 14, after a gas-solid mixture entering the recovery chamber 14 passes through the gas-solid separator 13, gas is discharged through an exhaust port 12 at the top of the recovery chamber 14, solid substances enter a degassing device 17 through a pipeline at the bottom of the recovery chamber for degassing, after degassing, the solid substances are discharged through a discharge port 18 at the bottom of the degassing device 17, and the upper part of the degassing device 17 is also provided with a purge gas inlet 15 and a purge gas outlet 16 respectively. Wherein, the carrier gas inlet 5, the air inlet 6 of the fluidized bed reactor 9, the bottom pipeline of the recovery chamber, the purge gas inlet 15, the purge gas outlet 16 and the discharge hole 18 of the degasser 17 are all provided with valves.
Example 2
The method for continuously preparing the array carbon nano tube by using the device comprises the following steps:
(1) Replacing air in the jet mill and the fluidized bed reactor by nitrogen in advance, and starting a heating device of the fluidized bed reactor under the nitrogen protection atmosphere to enable the temperature of the fluidized bed reactor to reach 650 ℃;
(2) Starting a jet mill and a carrier gas inlet at the lower part of the jet mill (nitrogen enters the jet mill through the carrier gas inlet), adding a FeMgAl hydrotalcite catalyst prepared by a urea method into a feed hopper, starting a motor to drive a screw feeding device to rotate, continuously bringing the catalyst into the jet mill by a rotating screw, adjusting the rotating speed of the motor and the nitrogen flow rate to ensure that the feeding speed of the catalyst is 0.1g/min, the gas-solid ratio in the jet mill is 0.05g/L, and carrying the catalyst into a fluidized bed reactor by nitrogen after high-shear dispersion by the jet mill;
(3) Introducing mixed gas of nitrogen, hydrogen and ethylene into the bottom of the fluidized bed reactor for reaction, wherein the mixed gas enters a reaction zone through a gas distributor, and the mixing volume ratio of the nitrogen, the hydrogen and the ethylene in the mixed gas is N 2 ∶H 2 ∶C 2 H 4 =2:1, reaction space velocity 10000h -1 The empty tower flow velocity of the gas is 0.5m/s, and the high-dispersion catalyst and ethylene are subjected to chemical vapor deposition reaction to generate the array carbon nano tube;
(4) The carbon nano tube enters the recovery chamber through a pipeline at the top of the reactor, after passing through the gas-solid separator, the gas is discharged through a tail gas port at the top of the recovery chamber, and the carbon nano tube enters the degassing device from a pipeline at the bottom of the recovery chamber for degassing and then is discharged from a discharge port.
The carbon nanotubes prepared in example 2 were in the form of loose powder without agglomeration, had a diameter of about 11nm and a specific surface of about 200m 2 (ii) in terms of/g. The growth amount of the carbon nanotubes is 95% or more.
Comparative example 1
The method for preparing the array carbon nano tube by adopting the fluidized bed reactor specifically comprises the following steps:
(1) Starting a heating device of the fluidized bed reactor under the nitrogen protection atmosphere to enable the temperature of the fluidized bed reactor to reach 650 ℃;
(2) Adding FeMgAl hydrotalcite catalyst prepared by a urea method into a fluidized bed reactor;
(3) Introducing mixed gas of nitrogen, hydrogen and ethylene into the bottom of the fluidized bed reactor for reaction, wherein the mixed gas enters a reaction zone through a gas distributor, and the mixing volume ratio of the nitrogen, the hydrogen and the ethylene in the mixed gas is N 2 ∶H 2 ∶C 2 H 4 =2:1, reaction space velocity 10000h -1 The empty tower flow velocity of the gas is 0.5m/s, and the catalyst and the ethylene are subjected to chemical vapor deposition reaction to generate the array carbon nano tube;
(4) After the reaction is finished, the heater is closed, the temperature is reduced to the room temperature under the protection of nitrogen, and the product is taken out.
The carbon nanotubes prepared in comparative example 1 partially had hard agglomerates, the diameter of the carbon nanotubes was about 11nm, and the specific surface area was about 200m 2 (ii) in terms of/g. The content of the carbon nano tube in the knot block is 40 to 50 percent.
Example 3
The method for continuously preparing the carbon nano tube by using the device comprises the following steps:
(1) Replacing air in the jet mill and the fluidized bed reactor by nitrogen in advance, and starting a heating device of the fluidized bed reactor under the nitrogen protection atmosphere to enable the temperature of the fluidized bed reactor to reach 700 ℃;
(2) Starting a jet mill and a carrier gas inlet at the lower part of the jet mill (nitrogen enters the jet mill through the carrier gas inlet), adding a FeMoAl catalyst prepared by a coprecipitation method into a feed hopper, starting a motor to drive a screw feeding device to rotate, continuously bringing the catalyst into the jet mill by a rotating screw, adjusting the rotating speed of the motor and the nitrogen flow rate to ensure that the feeding speed of the catalyst is 1g/min, the gas-solid ratio in the jet mill is 0.2g/L, and carrying the catalyst into a fluidized bed reactor by the nitrogen after high-shear dispersion by the jet mill;
(3) Introducing mixed gas of nitrogen, hydrogen and propylene into the bottom of the fluidized bed reactor for reaction, wherein the mixed gas enters a reaction zone through a gas distributor, and the mixing volume ratio of the nitrogen, the hydrogen and the propylene in the mixed gas is N 2 ∶H 2 ∶C 3 H 6 = 3: 1, reaction space velocity 3000h -1 The empty tower flow velocity of the gas is 1m/s, and the high-dispersion catalyst and propylene are subjected to chemical vapor deposition reaction to generate the array carbon nano tube;
(4) The carbon nano tube enters the recovery chamber through a pipeline at the top of the reactor, after passing through the gas-solid separator, the gas is discharged through a tail gas port at the top of the recovery chamber, and the carbon nano tube enters the degassing device from a pipeline at the bottom of the recovery chamber for degassing and then is discharged from a discharge port.
The carbon nanotubes prepared in example 3 were in the form of loose powder without agglomeration, had a diameter of about 12nm and a specific surface of about 190m 2 /g。
Example 4
The method for continuously preparing the graphene nanosheets by using the device specifically comprises the following steps:
(1) Replacing air in the jet mill and the reactor with argon (or dry air) in advance, and starting a heating device to enable the temperature of the fluidized bed reactor to reach 900 ℃;
(2) Starting a jet mill and a carrier gas inlet at the lower part of the jet mill (argon or dry air enters the jet mill through the carrier gas inlet), adding MgO sheet materials into a feed hopper, starting a motor to drive a screw feeding device to rotate, continuously bringing the MgO sheet materials into the jet mill by a rotating screw, adjusting the rotating speed of the motor and the flow speed of the argon to ensure that the feeding speed of a catalyst is 5 g/min and the gas-solid ratio is 3g/L, and carrying the MgO sheet materials into a fluidized bed reactor through argon after the MgO sheet materials are subjected to high-shear dispersion by the jet mill;
(3) Introducing mixed gas of argon, hydrogen and methane into the bottom of the fluidized bed reactor for reaction, wherein the mixed gas enters a reaction zone through a gas distributor, and the mixed volume ratio of the argon, the hydrogen and the methane in the mixed gas is Ar: H 2 ∶CH 4 = 5: 1, reaction space velocity 5000h -1 The empty tower flow velocity of the gas is 3m/s, and the high-dispersion MgO lamellar material and methane are subjected to chemical vapor deposition reaction to generate graphene on the surface of the MgO lamellar material;
(4) The product enters the recovery chamber through a pipeline at the top of the reactor, after passing through the gas-solid separator, the gas is discharged through a tail gas port at the top of the recovery chamber, and the product enters a degassing device from a pipeline at the bottom of the recovery chamber to be degassed and then is discharged from a discharge port.
The product prepared in example 4 is in the form of loose powder without agglomeration, and the graphene powder obtained after purification has a thickness of about 1nm and a specific surface of about 900m 2 /g。
Example 5
The method for continuously preparing the modified white carbon black by using the device comprises the following steps:
(1) Replacing air in the jet mill and the reactor with nitrogen (or dry air) in advance, and starting a heating device to enable the temperature of the fluidized bed reactor to reach 200 ℃;
(2) Opening a jet mill and a carrier gas inlet at the lower part of the jet mill (nitrogen or dry air enters the jet mill through the carrier gas inlet), adding white carbon black powder into a feed hopper, opening a motor to drive a screw rod feeding device to rotate, continuously feeding the white carbon black into the jet mill by a rotating screw rod, adjusting the rotating speed of the motor and the nitrogen flow rate to ensure that the feeding speed of a catalyst is 20 g/min and the gas-solid ratio is 5g/L, and carrying the white carbon black into a fluidized bed reactor by nitrogen after the white carbon black is subjected to high-shear dispersion by the jet mill;
(3) Introducing nitrogen containing 15 percent (volume fraction) of hexamethyldisilazane into the bottom of the fluidized bed reactor, and introducing the fluid into a reaction zone through a gas distributor, wherein the reaction space velocity is 5h -1 The empty tower flow rate of the gas is 0.05m/s, and the high-dispersion white carbon black powder and hexamethyldisilazane react in a reactor to finish the white carbon blackModifying carbon black;
(4) The modified white carbon black enters the recovery chamber through a pipeline at the top of the reactor, after passing through the gas-solid separator, the gas is discharged through a tail gas port at the top of the recovery chamber, and the modified white carbon black enters the degassing device from a pipeline at the bottom of the recovery chamber for degassing and then is discharged from a discharge port.
The product of example 5 was in the form of a loose powder with no lumps in the product and a carbon content of about 3%.
Comparative example 2
The method for preparing the modified white carbon black by adopting the rotary kiln specifically comprises the following steps:
(1) Putting the white carbon black into a rotary kiln reactor, adjusting the rotating speed of the rotary kiln to 10 revolutions per minute, and heating to 200 ℃ under the protection of nitrogen;
(2) Introducing nitrogen containing 15% (volume fraction) of hexamethyldisilazane, and reacting the white carbon black and the hexamethyldisilazane in a reactor to complete the modification of the white carbon black;
(3) After the reaction is finished, the heating is closed, the temperature is reduced to room temperature under the protection of nitrogen, and the product is taken out.
The product prepared in comparative example 2 had a partial caking rate of 5 to 15% and a carbon content of about 2%.
When equal amounts of the product obtained in example 5 and the product obtained in comparative example 2 were placed in equal amounts of water, respectively, it was seen that the product obtained in comparative example 2 was partially submerged (the hydrophobic modification was incomplete), whereas the product obtained in example 5 (modified from hydrophilic to hydrophobic) was completely floated (the hydrophobic modification was complete).

Claims (5)

1. A method for continuously preparing nano-materials, which is characterized by comprising the following steps: the device adopted by the method comprises a fluidized bed reactor and a jet mill, and catalyst materials are fed into the fluidized bed reactor through the jet mill;
the method for continuously preparing the array carbon nano tube specifically comprises the following steps:
(1) Replacing air in the jet mill and the fluidized bed reactor by nitrogen in advance, and starting a heating device of the fluidized bed reactor under the nitrogen protection atmosphere to enable the temperature of the fluidized bed reactor to reach 650 ℃;
(2) Starting a jet mill and a carrier gas inlet at the lower part of the jet mill, introducing nitrogen into the jet mill through the carrier gas inlet, adding a FeMgAl hydrotalcite catalyst prepared by a urea method into a feed hopper, starting a motor to drive a screw feeding device to rotate, continuously introducing the catalyst into the jet mill by a rotating screw, adjusting the rotating speed of the motor and the nitrogen flow rate to ensure that the feeding speed of the catalyst is 0.1g/min, the gas-solid ratio in the jet mill is 0.05g/L, and introducing the catalyst into a fluidized bed reactor by nitrogen after high-shear dispersion by the jet mill;
(3) Introducing mixed gas of nitrogen, hydrogen and ethylene into the bottom of the fluidized bed reactor for reaction, and introducing the mixed gas into a reaction zone through a gas distributor, wherein the mixed volume ratio of the nitrogen, the hydrogen and the ethylene in the mixed gas is N 2 :H 2 :C 2 H 4 1, and the reaction space velocity is 10000h -1 The empty tower flow velocity of the gas is 0.5m/s, and the high-dispersion catalyst and ethylene are subjected to chemical vapor deposition reaction to generate the array carbon nano tube;
(4) The carbon nano tube enters the recovery chamber through a pipeline at the top of the reactor, after passing through the gas-solid separator, the gas is discharged through a tail gas port at the top of the recovery chamber, and the carbon nano tube enters the degassing device from a pipeline at the bottom of the recovery chamber for degassing and then is discharged from a discharge port.
2. The method for continuously preparing nano-materials according to claim 1, characterized in that: the device also comprises a feed hopper and a screw feeding device, wherein the feed hopper is arranged above the screw feeding device, a discharge hole of the screw feeding device is connected with the airflow crusher, and a power mechanism of the screw feeding device is a motor.
3. The method for continuously producing nanomaterials of claim 2, wherein: the device also comprises a recovery chamber and a degassing device communicated with the recovery chamber, wherein a gas-solid separator is arranged in the recovery chamber, a discharge port of the fluidized bed reactor is communicated with the recovery chamber through a pipeline, after a gas-solid mixture entering the recovery chamber passes through the gas-solid separator, the gas is discharged through a tail gas port at the top of the recovery chamber, and solid substances enter the degassing device from the bottom of the recovery chamber for degassing and are discharged from a discharge port at the bottom of the degassing device.
4. The method for continuously producing nanomaterials of claim 3, wherein: the gas inlet of the fluidized bed reactor is arranged at the bottom of the fluidized bed reactor, and the reaction gas entering the fluidized bed reactor through the gas inlet enters the reaction zone of the fluidized bed reactor after passing through the gas distributor; the discharge port of the fluidized bed reactor is positioned at the top of the fluidized bed reactor.
5. The method for continuously preparing nano-materials according to claim 4, characterized in that: and a heating device is arranged in the fluidized bed reactor.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101665248A (en) * 2009-09-11 2010-03-10 清华大学 Method for preparing single-walled and double-walled carbon nanotubes based on layered dihydroxy metal hydroxide
CN102295510A (en) * 2010-06-24 2011-12-28 中国石油化工股份有限公司 Method for catalytically converting naphtha into low-carbon olefin
CN106079001A (en) * 2016-06-20 2016-11-09 浙江旺林生物科技有限公司 A kind of nano bamboo powdered carbon production technology
CN107188157A (en) * 2016-03-15 2017-09-22 本田技研工业株式会社 Manufacture the system and method for combination product

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4886644A (en) * 1987-12-02 1989-12-12 Texaco Inc. Liquid degaser in an ebullated bed process
DE602006010558D1 (en) * 2005-07-11 2009-12-31 Akzo Nobel Coatings Int Bv METHOD FOR THE ELECTROSTATIC POWDER COATING IN THE SPHERICAL BED
JP5549941B2 (en) * 2011-05-10 2014-07-16 株式会社日本製鋼所 Nanocarbon production method and production apparatus
CN209138817U (en) * 2018-08-22 2019-07-23 丹阳市田园圣树生态园有限公司 A kind of supersonic jet mill device advantageously reducing the reunion of mulberry leaf fragment
CN208928340U (en) * 2018-10-11 2019-06-04 河南晟道科技有限公司 Moissanite sword material production high-temperature steam jet mill grinding system

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101665248A (en) * 2009-09-11 2010-03-10 清华大学 Method for preparing single-walled and double-walled carbon nanotubes based on layered dihydroxy metal hydroxide
CN102295510A (en) * 2010-06-24 2011-12-28 中国石油化工股份有限公司 Method for catalytically converting naphtha into low-carbon olefin
CN107188157A (en) * 2016-03-15 2017-09-22 本田技研工业株式会社 Manufacture the system and method for combination product
CN106079001A (en) * 2016-06-20 2016-11-09 浙江旺林生物科技有限公司 A kind of nano bamboo powdered carbon production technology

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