CN107311146A - A kind of serialization prepares the device and method of nano-carbon material - Google Patents
A kind of serialization prepares the device and method of nano-carbon material Download PDFInfo
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- 229910021392 nanocarbon Inorganic materials 0.000 title claims abstract description 61
- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000003860 storage Methods 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 238000010924 continuous production Methods 0.000 claims abstract description 6
- 230000035484 reaction time Effects 0.000 claims abstract 3
- 239000007789 gas Substances 0.000 claims description 75
- 239000000463 material Substances 0.000 claims description 25
- 239000003054 catalyst Substances 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 229910052799 carbon Inorganic materials 0.000 claims description 15
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 13
- 239000003245 coal Substances 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 239000011261 inert gas Substances 0.000 claims description 8
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 229910003271 Ni-Fe Inorganic materials 0.000 claims description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
- 239000003345 natural gas Substances 0.000 claims description 3
- 229910017060 Fe Cr Inorganic materials 0.000 claims description 2
- 229910002544 Fe-Cr Inorganic materials 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910002221 La2NiO4 Inorganic materials 0.000 claims description 2
- 229910017950 MgOz Inorganic materials 0.000 claims description 2
- UPHIPHFJVNKLMR-UHFFFAOYSA-N chromium iron Chemical compound [Cr].[Fe] UPHIPHFJVNKLMR-UHFFFAOYSA-N 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229910021382 natural graphite Inorganic materials 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 239000006104 solid solution Substances 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
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- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
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- 238000007664 blowing Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 abstract 1
- 241000234282 Allium Species 0.000 description 6
- 235000002732 Allium cepa var. cepa Nutrition 0.000 description 6
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 4
- 229910003472 fullerene Inorganic materials 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
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- 239000002134 carbon nanofiber Substances 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
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- 238000001816 cooling Methods 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses the device and method that a kind of serialization prepares nano-carbon material, belong to nano-carbon material preparing technical field.Serialization prepares the device of nano-carbon material, including tubular reactor, auger conveyor, heating furnace, storage bin, screw feeder, feed pipe, air inlet pipe, blast pipe, drainage conduit, loading head；Raw material enters on tubular reactor inside spin conveyer via screw feeder, heating furnace is heated to reacting required temperature, the required reaction time is controlled by adjusting the rotating speed of auger conveyor, the product nano carbon material after the completion of reaction continues to be carried to the discharge mouth of pipe under the rotation of feeding screw and entered in loading head.The invention further relates to the method that serialization prepares nano-carbon material, the serialization for realizing nano-carbon material is prepared and produced, it is to avoid intermittent reaction blowing out operation, so as to improve the production efficiency of nano-carbon material；Suitable for nano-carbon material and with it is similar preparation production technology nano material continuous production.
Description
Technical Field
The invention relates to the technical field of nano carbon material preparation, in particular to a device and a method for continuously preparing a nano carbon material.
Background
Carbon is one of the most abundant elements in the world and also a basic element constituting a living body. Under the continuous exploration and research of researchers, the structures, properties and application values of various allotropes of carbon are gradually enriched, such as carbon nanotubes, graphene, carbon onions, and the like, so the research and development of carbon nanomaterials are valued by many researchers. Highly graphitized carbon materials such as nano onion carbon, nano carbon tubes, nano carbon spheres, etc., have good mechanical and electronic properties, chemical inertness and biocompatibility, and are widely applied to the fields of engineering, electronics, chemical engineering, biology, etc. The nano onion carbon, also called onion-like fullerene, is an allotrope of carbon with the most stable energy, has small volume, large specific surface area and good conductivity, and has wide application prospect in the fields of super capacitors, lithium ion batteries, solid lubricants and the like.
The preparation method of the nano carbon material generally comprises an arc discharge method, an electron beam radiation method, a pyrolysis method, a chemical vapor deposition method and the like. At present, equipment for industrially producing the nano carbon material by adopting a chemical vapor deposition method has great advantages in the aspect of realizing on-line preparation of the nano carbon material and achieving the aim of production, but most of the equipment adopts an intermittent reactor, so that the on-line carbon extraction is difficult in the preparation process of the nano carbon material, and the continuous production cannot be realized.
Disclosure of Invention
The invention provides a device and a method for continuously preparing a nano carbon material, which aim to solve the problems that in the prior art, production equipment of the nano carbon material is difficult to take carbon on line in the preparation process, and continuous production cannot be realized.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
an apparatus for continuously preparing a nano carbon material, comprising: the starting end of the tubular reactor is provided with an air inlet pipe and a feeding pipe, and the tail end of the tubular reactor is provided with an exhaust pipe and a discharge pipe; the air inlet pipe, the exhaust pipe and the discharge pipe are provided with stop valves; the spiral conveyor is arranged at the position of the central shaft of the reactor; the first motor is used for driving the screw conveyor to rotate and is electrically connected with the screw conveyor; the heating furnace is used for heating the reactor and is arranged at the position of the reaction zone of the reactor; the storage bin is connected with the feeding pipe; the spiral feeder is arranged in the storage bin, and the feeding pipe is hermetically connected with the spiral feeder; the second motor is used for driving the screw feeder to rotate and is electrically connected with the screw feeder; the material collector is connected with the material discharging pipe.
The invention also relates to a method for preparing the nano carbon material by using the device for continuously preparing the nano carbon material, which comprises the following steps: step 1, according to the atmosphere required by the production preparation process, introducing inert gas into a reactor through a gas inlet pipe, opening a gas outlet pipe, and discharging air in a reaction system; starting a heating furnace to heat to 600-1000 ℃, starting a screw feeder in a storage bin and a screw conveyor in a reactor, and enabling the raw materials to fall onto the screw conveyor through the screw feeder; step 2, changing inert gas into reducing gas, introducing the reducing gas into the reactor through the gas inlet pipe, enabling the generated nano carbon material to fall down after reaching the tail end of the screw conveyor along with the rotation of the screw conveyor, and enabling the nano carbon material to enter a material collector through a discharge pipe; tail gas generated by the reaction is discharged through an exhaust pipe; and 3, after the material collector is full, closing a stop valve of the material discharge pipe, and replacing a new material collector to continuously collect the generated nano carbon material.
The invention has the beneficial effects that:
the invention solves the problem of on-line collection of the nano carbon material in the preparation process, realizes the continuous production of the nano carbon material, avoids the independent collection process of the nano carbon material, improves the working efficiency of the reactor, reduces the repetition rate of cooling and heating of the reactor, reduces the energy consumption, prolongs the service life of the reactor, and reduces the production cost and the time cost; the device is simple in arrangement, convenient to use and maintain, safe and reliable; is suitable for the continuous production of the nano-carbon material and the nano-material with the similar preparation and production process.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for continuously preparing a nanocarbon material according to an embodiment;
FIG. 2 is an SEM photograph of nano onion like fullerenes of example 1;
fig. 3 is an SEM image of the nanocarbon material prepared in example 2.
In the figure: 1. a tubular reactor; 2. a screw conveyor; 3. heating furnace; 4. a storage bin; 5. a screw feeder; 6. a feed pipe; 7. a first intake pipe; 8. a second intake pipe; 9. a first shut-off valve; 10. a second stop valve; 11. a first motor; 12. a second motor; 13. an exhaust pipe; 14. a discharge pipe; 15. a third stop valve; 16. a material collector.
Detailed Description
The invention is further described with reference to the following figures and specific examples.
As shown in fig. 1, an apparatus for continuously preparing a nanocarbon material includes: the device comprises a tubular reactor 1, a screw conveyor 2, a first motor 11 for driving the screw conveyor 2 to rotate, a heating furnace 3 for heating the reactor 1, a storage bin 4, a screw feeder 5, a second motor 12 for driving the screw feeder 5 to rotate and a material collector 16; wherein,
the starting end 100 of the reactor 1 is provided with an air inlet pipe and a feeding pipe 6, and the tail end 200 of the reactor is provided with an exhaust pipe 13 and a discharge pipe 14; stop valves are arranged on the air inlet pipe, the exhaust pipe 13 and the discharge pipe 14; the screw conveyor 2 is arranged at the central shaft position of the reactor 1; the first motor 11 is electrically connected with the screw conveyor 2; the heating furnace 3 is arranged at the position of the reaction zone of the reactor 1; the storage bin 4 is connected with a feeding pipe 6; the spiral feeder 5 is arranged in the storage bin 4, and the feeding pipe 6 is connected with the spiral feeder 5 in a sealing way; the second motor 12 is electrically connected with the screw feeder 5; the collector 16 is connected to the discharge pipe 14.
In the embodiment, both ends of the reactor 1 need to be subjected to airtight treatment; the sealing between the feeding pipe 6 and the screw feeder 5 adopts the prior art, namely the prior art of sealing screw feeding, such as intermittent feeding, and the feeding pipe 6 is provided with a sealing valve; preferably, the heating furnace 3 is of an open type, which is heated by electric heating or by a combustible off-gas.
In the preparation process of the nano carbon material, two different gases need to be introduced into the reaction system in the front and back stages, preferably, the gas inlet pipe in the embodiment comprises a first gas inlet pipe 7 and a second gas inlet pipe 8, and a first stop valve 9 and a second stop valve 10 are respectively and correspondingly arranged and are respectively communicated with the reactor 1. A third shut-off valve 15 is arranged on the discharge pipe 14.
Preferably, the apparatus for continuously preparing a nano carbon material in the embodiment further comprises: a tail gas collecting device connected with the gas outlet of the exhaust pipe 13, and a gas storage tank connected with the gas inlet of the gas inlet pipe, wherein the gas storage tank provides required gas for reaction.
Preferably, the apparatus for continuously preparing a nano carbon material in the embodiment further comprises: and the pressure swing adsorption device is connected with the tail gas collecting device to realize gas recovery.
Preferably, the reactor 1 in the embodiment is made of stainless steel or quartz, and is provided with a thermocouple.
Preferably, in the embodiment, the reactor 1 is arranged in a fixed manner in a horizontal manner, the storage silo 4 is located above the beginning of the reactor 1, and the collector 16 is located below the end of the reactor 1, which is flanged to the discharge pipe 14.
In the embodiment, when the device for continuously preparing the nano carbon material works, equipment is connected firstly, according to the atmosphere required by the production and preparation process, an inert gas tank is connected with a first gas inlet pipe 7 (or a second gas inlet pipe 8), a reduction gas tank is connected with the second gas inlet pipe 8 (or the first gas inlet pipe 7), and a tail gas collecting device is connected with an exhaust pipe 13; closing the second stop valve 10 (or the first stop valve 9), the feeding pipe 6 and the third stop valve 15 in sequence, opening the exhaust pipe 13, then opening the first stop valve 9 (or the second stop valve 10), introducing inert gases such as nitrogen or argon into the reactor 1 through the first gas inlet pipe 7 (or the second gas inlet pipe 8), and discharging air in the reaction system; after emptying, carrying out leak detection on the reactor 1, and closing the first stop valve 9 (or the second stop valve 10) after confirming that no gas leakage part exists; then starting the heating furnace 3 to heat to the required temperature, opening the feeding pipe 6, starting the screw feeder 5 and the screw conveyor 2, and enabling the raw materials to fall onto the screw conveyor 2 through the action of the screw feeder 5; opening a second stop valve 10 (or a first stop valve 9), introducing a required auxiliary atmosphere (reducing gas) into the reactor 1 through a second gas inlet pipe 8 (or a first gas inlet pipe 7) to ensure the quality of the nanocarbon materials (such as nano onion carbon, a carbon nanotube, carbon nanofiber and the like), wherein the generated nanocarbon materials fall down after reaching the spiral end of the conveyor 2 along with the rotation of the spiral conveyor 2, and are discharged into a material collector 16 through a discharge pipe 14; if tail gas is generated in the reaction, the tail gas is discharged from an exhaust pipe 13 above the tail end of the reactor 1; after the collector 16 is full, the third stop valve 15 is closed, and the collector 16 is replaced with a new one to continuously collect the generated nano carbon material.
In the preparation process of the nano carbon material in the embodiment, if the raw material in the step 1 only contains catalyst powder, the raw material does not contain C, and the reducing gas in the step 2 is C-containing gas, such as natural gas, coal bed gas, methane or alkane gas; if the feedstock in step 1 contains C, such as a coal-based carbon feedstock, or a mixture of catalyst fines and coal-based carbon feedstock, the reducing gas in step 2 may be a C-containing gas or a C-free gas, such as hydrogen; the catalyst powder is Mox-Ni (Fe, Co) Y-MgOz solid solution catalyst, Ni/Y-type zeolite structure catalyst, La2NiO4 catalyst, Ni/MCM-41 catalyst, Fe-Cr alloy catalyst, LaNi0.9Co0.1O3 catalyst or Ni-Fe alloy catalyst with different Mo, Ni (Fe, Co) and Mg contents; the coal-based carbon raw material is natural graphite or flake graphite and the like.
The apparatus for continuously preparing the nano-carbon material in the embodiment can prepare different nano-carbon materials according to the difference of raw materials, heating temperature, the rotation speed of the screw feeder 5 and the screw conveyor 2, and other parameters.
Example 1
The preparation method of the nano onion-shaped fullerene by mixing graphite powder and a catalyst comprises the following steps:
step 1, connecting equipment, connecting a nitrogen tank with a first air inlet pipe 7, connecting a reduction gas tank with a second air inlet pipe 8, and connecting a tail gas collecting device with an exhaust pipe 13; closing the second stop valve 10, the feed pipe 6 and the third stop valve 15 in sequence, opening the exhaust pipe 13, then opening the first stop valve 9, introducing nitrogen to evacuate the reactor 1, wherein the nitrogen flow is 50-200sccm, the evacuation time is 15-45 min, after evacuation, performing leak detection on the reactor 1, and after confirming that no gas leakage part exists, closing the first stop valve 9; then heating the heating furnace 3 to 600-1000 ℃, opening the feeding pipe 6, adding the mixture of the pretreated graphite powder and the Ni-Fe alloy catalyst (the pretreatment is the prior art) into the storage bin 4, starting the screw feeder 5 and the screw conveyor 2, and enabling the raw materials to fall onto the screw conveyor 2 in the reactor 1 in a rotating manner under the action of the screw feeder 5;
step 2, opening a second stop valve 10, opening a valve of an exhaust pipe 13 connected with a tail gas collecting device, introducing reducing gas (H2 or alkane gas) through a second gas inlet pipe 8, setting the rotating speed of a screw feeder 5 to be 1-10r/min, setting the rotating speed of a screw conveyor 2 to be 2-20r/min, reacting for 15-30min, allowing the generated nano carbon material to enter a discharge pipe 14 along with the rotation of the screw conveyor 2 to the tail end of a reactor 1, opening a third stop valve 15, and discharging the generated nano carbon material into a collector 16 through the discharge pipe 14;
and 3, after the material collector 16 is full, closing the third stop valve 15, and replacing a new material collector 16 to continuously collect the generated nano carbon material.
SEM pictures of nano onion like fullerenes collected in the examples are shown in fig. 2.
Example 2
The method for continuously preparing the nano carbon material by catalytic cracking of the coal bed gas comprises the following steps:
step 1, connecting equipment, connecting a nitrogen tank with a first air inlet pipe 7, connecting a reduction gas tank with a second air inlet pipe 8, and connecting a tail gas collecting device with an exhaust pipe 13; closing the second stop valve 10, the feed pipe 6 and the third stop valve 15 in sequence, opening the exhaust pipe 13, then opening the first stop valve 9, introducing nitrogen to evacuate the reactor 1, wherein the nitrogen flow is 50-200sccm, the evacuation time is 15-45 min, after evacuation, performing leak detection on the reactor 1, and after confirming that no gas leakage part exists, closing the first stop valve 9; then heating the heating furnace 3 to 600-1000 ℃, opening the feeding pipe 6, adding the Ni/Y-type zeolite structure into the storage bin 4, starting the screw feeder 5 and the screw conveyor 2, and enabling the raw materials to fall onto the screw conveyor 2 in the reactor 1 under the action of the screw feeder 5;
step 2, opening a second stop valve 10, opening a valve of an exhaust pipe 13 connected with a tail gas collecting device, introducing coal bed gas through a second air inlet pipe 8, setting the rotating speed of a screw feeder 5 to be 1-10r/min, setting the rotating speed of a screw conveyor 2 to be 1-5r/min, reacting for 30-90min, allowing the generated nano carbon material to rotate to the tail end of a reactor 1 along with the rotation of the screw conveyor 2 to enter a discharge pipe 14, opening a third stop valve 15, and discharging the generated nano carbon material into a collector 16 through the discharge pipe 14;
and 3, after the material collector 16 is full, closing the third stop valve 15, and replacing a new material collector 16 to continuously collect the generated nano carbon material.
SEM pictures of the nanocarbon materials collected in the examples are shown in fig. 3.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art, and the scope of the present invention should be construed as being limited thereto.
Claims (10)
1. An apparatus for continuously preparing a nano carbon material, comprising:
the device comprises a tubular reactor (1), wherein a starting end (100) of the tubular reactor is provided with an air inlet pipe and a feeding pipe (6), and a tail end (200) of the tubular reactor is provided with an exhaust pipe (13) and a discharge pipe (14); stop valves are arranged on the air inlet pipe, the exhaust pipe (13) and the discharge pipe (14);
a screw conveyor (2) provided at the central axis position of the reactor (1);
a first motor (11) for driving the screw conveyor (2) to rotate, electrically connected with the screw conveyor (2);
the heating furnace (3) is used for heating the reactor (1) and is arranged at the position of the reaction zone of the reactor (1);
the storage bin (4) is connected with the feeding pipe (6);
the spiral feeder (5) is arranged in the storage bin (4), and the feeding pipe (6) is hermetically connected with the spiral feeder (5);
the second motor (12) is used for driving the screw feeder (5) to rotate and is electrically connected with the screw feeder (5);
a collector (16) connected to the discharge pipe (14).
2. The continuous production device for nano carbon material according to claim 1, wherein the gas inlet pipe comprises a first gas inlet pipe (7) and a second gas inlet pipe (8), and a first stop valve (9) and a second stop valve (10) are correspondingly arranged and respectively communicated with the reactor (1).
3. The apparatus for continuously preparing a nano carbon material according to claim 1, further comprising:
the tail gas collecting device is connected with the gas outlet of the exhaust pipe (13);
and the gas storage tank is connected with the gas inlet of the gas inlet pipe.
4. The apparatus for continuously preparing a nano carbon material according to claim 1, further comprising: and the pressure swing adsorption device is connected with the tail gas collecting device.
5. The apparatus for continuously preparing nano carbon material according to claim 1, wherein the reactor (1) is made of stainless steel or quartz and is equipped with a thermocouple.
6. The apparatus for continuously preparing nano carbon material according to claim 1, wherein both ends of the reactor (1) are hermetically sealed.
7. A method for producing a nanocarbon material using the apparatus for continuously producing a nanocarbon material according to claims 1 to 6, comprising the steps of:
step 1, according to the atmosphere required by the production preparation process, introducing inert gas into a reactor (1) through a gas inlet pipe, opening a gas outlet pipe (13), and discharging air in a reaction system; starting a heating furnace (3) to heat to 600-1000 ℃, starting a screw feeder (5) in a storage bin (4) and a screw conveyor (2) in a reactor (1), and enabling the raw materials to fall onto the screw conveyor (2) through the screw feeder (5);
step 2, changing inert gas into reducing gas, introducing the reducing gas into the reactor (1) through the gas inlet pipe, enabling the generated nano carbon material to reach the tail end of the screw conveyor (2) along with the rotation of the screw conveyor (2), then falling down, and entering a material collector (16) through a discharge pipe (14); tail gas generated by the reaction is discharged from an exhaust pipe (13);
and 3, after the material collector (16) is full, closing a stop valve of the material discharge pipe (14), and replacing a new material collector to continuously collect the generated nano carbon material.
8. The method of claim 7,
the raw material in the step 1 is catalyst powder, and the reducing gas in the step 2 is natural gas, coal bed gas, methane or alkane gas; or,
the raw material in the step 1 is coal-based carbon raw material or a mixture of catalyst powder and coal-based carbon raw material, and the reducing gas in the step 2 is natural gas, coal bed gas, methane, alkane gas or hydrogen;
the catalyst powder is Mox-Ni (Fe, Co) Y-MgOz solid solution catalyst, Ni/Y-type zeolite structure catalyst, La2NiO4 catalyst, Ni/MCM-41 catalyst, Fe-Cr alloy catalyst, LaNi0.9Co0.1O3 catalyst or Ni-Fe alloy catalyst with different Mo, Ni (Fe, Co) and Mg contents;
the coal-based carbon raw material is natural graphite or crystalline flake graphite.
9. The method as claimed in claim 8, wherein in the step 1, the inert gas is nitrogen, the nitrogen flow is 50-200sccm, the evacuation time is 15-45 min, and the raw material is a mixture of graphite powder and a Ni-Fe alloy catalyst; in the step 2, the rotating speed of the screw feeder (5) is 1-10r/min, the rotating speed of the screw conveyor (2) is 2-20r/min, and the reaction time is 15-30 min.
10. The method of claim 8, wherein in the step 1, the inert gas is nitrogen, the nitrogen flow rate is 50-200sccm, the evacuation time is 15-45 min, and the raw material is catalyst powder; in the step 2, the rotating speed of the screw feeder (5) is 1-10r/min, the rotating speed of the screw conveyor (2) is 1-5r/min, and the reaction time is 30-90 min.
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| CN110127664A (en) * | 2019-06-27 | 2019-08-16 | 深圳市中科纳米科技有限公司 | The device and method of carbon nanotube are automatically continuously produced using fixed bed |
| CN111921528A (en) * | 2020-06-28 | 2020-11-13 | 济南大学 | Method and system for preparing slurry bed Fischer-Tropsch synthesis catalyst slurry by pyrolyzing MOFs |
| CN112279289A (en) * | 2020-07-14 | 2021-01-29 | 济南大学 | Semi-continuous production method and system for preparing nano material by pyrolyzing MOFs |
| WO2021172077A1 (en) * | 2020-02-28 | 2021-09-02 | 日本ゼオン株式会社 | Manufacturing method for carbon nanotube aggregates |
| CN113736996A (en) * | 2021-09-03 | 2021-12-03 | 西安交通大学 | Method and device for intermittently and continuously smelting crystallized magnesium in Pidgeon reduction tank |
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| CN111921528A (en) * | 2020-06-28 | 2020-11-13 | 济南大学 | Method and system for preparing slurry bed Fischer-Tropsch synthesis catalyst slurry by pyrolyzing MOFs |
| CN112279289A (en) * | 2020-07-14 | 2021-01-29 | 济南大学 | Semi-continuous production method and system for preparing nano material by pyrolyzing MOFs |
| CN113736996A (en) * | 2021-09-03 | 2021-12-03 | 西安交通大学 | Method and device for intermittently and continuously smelting crystallized magnesium in Pidgeon reduction tank |
| CN113736996B (en) * | 2021-09-03 | 2022-10-25 | 西安交通大学 | Method and device for intermittently and continuously smelting crystallized magnesium in Pidgeon reduction tank |
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