CN111686650B - Carbon nano tube preparation device and method - Google Patents
Carbon nano tube preparation device and method Download PDFInfo
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- CN111686650B CN111686650B CN202010547238.1A CN202010547238A CN111686650B CN 111686650 B CN111686650 B CN 111686650B CN 202010547238 A CN202010547238 A CN 202010547238A CN 111686650 B CN111686650 B CN 111686650B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1836—Heating and cooling the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
- B01J8/003—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor in a downward flow
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1872—Details of the fluidised bed reactor
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
Abstract
The invention provides a carbon nanotube preparation device and a method, wherein the device comprises a fluidized reactor, a detachable heating component is arranged on the outer side of the main body of the fluidized reactor, and the heating component and the main body of the fluidized reactor are arranged in parallel and move along the horizontal direction; an outlet at the upper part of the fluidized reactor is connected with a gas-solid separator, and an outlet at the lower part of the fluidized reactor is connected with a product discharging pipeline. The device disclosed by the invention has the advantages that through the improvement of heating and separation components of the fluidized reactor, the movement, the installation and the disassembly of the heating components are facilitated, the maintenance cost is greatly reduced, meanwhile, the products can be quickly separated, the device is not easy to block, and the production efficiency of the device is improved; the solid product discharging mode can effectively avoid the problem that powder is easy to be compacted to cause blockage when discharging under positive pressure; the heat exchange and cooling pipelines are arranged, so that the heat utilization rate is effectively improved, the energy consumption is reduced, the cooling period of the device is shortened, and the production stop time is reduced.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and relates to a carbon nano tube preparation device and a method.
Background
The carbon nano tube is a one-dimensional quantum material with a special structure, has the advantages of small volume density, large specific surface area, excellent mechanical property, good heat and electricity conductivity and the like, wherein the structure of the carbon nano tube is similar to that of a high polymer material, but the structural stability of the carbon nano tube is obviously superior to that of the high polymer material, so that the carbon nano tube is one of the materials with the highest specific strength at present, is always widely concerned by people, and has wide application prospect in the fields of structural composite materials, energy sources, catalysis, functional devices and the like.
At present, the methods for preparing carbon nanotubes mainly include arc discharge, laser ablation, chemical vapor deposition, solid phase pyrolysis, glow discharge, gas combustion, and polymerization synthesis, among which the more mature method is chemical vapor deposition. The chemical vapor deposition method, also called as a hydrocarbon gas pyrolysis method, is a method for obtaining the carbon nano tube by cracking the carbon-containing gas under the action of the catalyst, and has high yield, but the chemical vapor deposition method has low crystallization degree of the carbon nano tube due to low inherent reaction temperature, so that the defect content of the carbon nano tube prepared by the chemical vapor deposition method is high, and the performances such as conductivity and the like are greatly limited.
CN 110217777A discloses a carbon nanotube preparation device and method, the device is formed by connecting a catalyst evaporation cavity, a chemical vapor deposition cavity and a gas-solid separation cavity in series, the catalyst in the catalyst evaporation cavity is directly evaporated into superfine catalyst by using high temperature and impact generated by arc flame, the superfine catalyst enters the chemical vapor deposition cavity through a connecting channel, simultaneously carrier gas and carbon source gas are respectively introduced from the catalyst evaporation cavity and the chemical vapor deposition cavity, the catalyst reacts with an organic carbon source of high-temperature cracking to generate carbon nanotubes, and then the carbon nanotubes are separated and collected by the gas-solid separation device. The device needs higher reaction temperature, namely high reaction energy consumption, has higher requirement on the stability of the catalyst, and has smaller device scale.
The preparation of the carbon nano tube can often use a fluidized bed reactor, the carbon nano tube is easy to agglomerate due to the structural characteristics of the carbon nano tube, and when the fluidized bed reactor is used for producing the carbon nano tube, the carbon nano tube is easy to agglomerate to form accumulation on the inner wall along with the production of the carbon nano tube, and the carbon nano tube is difficult to be brought out along with air flow during discharging. CN 205761066U discloses a automatically cleaning fluidized bed reactor for carbon nanotube production, including the fluidized bed reactor body that has the reacting chamber and locate the rotary device in the reacting chamber, rotary device includes along the vertical rotation axis that sets up in reacting chamber center and the rotator of being connected with the rotation axis, the reacting chamber is equipped with inflow entrance and egress opening, rotation axis and inflow entrance intercommunication, be equipped with on the rotator just to the inner wall of reacting chamber and with a plurality of gas pockets that the rotation axis intercommunication supplied gas to flow out the device is mainly the corresponding improvement made to the wall problem is glued to the reacting chamber material, but to the putty that exists at present, the cooling is slow, dismantle difficult scheduling problem and do not relate to.
In view of the above, the design and improvement of the carbon nanotube production apparatus are required to improve the production efficiency, shorten the production period, adapt the structure for the reaction, reduce the energy consumption, and be suitable for large-scale application.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a carbon nanotube preparation device and a method, wherein the device is used for improving the heating, separating and other components of a fluidized reactor, so that the heating components are convenient to move, install and disassemble, meanwhile, the product can be quickly separated, the device is not easy to block, the furnace shutdown time can be effectively shortened, and the production efficiency is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a carbon nanotube preparation apparatus, which comprises a fluidized reactor, wherein a detachable heating assembly is arranged on the outer side of a main body of the fluidized reactor, and the heating assembly and the main body of the fluidized reactor are arranged in parallel and move along the horizontal direction;
an outlet at the upper part of the fluidized reactor is connected with a gas-solid separator, and an outlet at the lower part of the fluidized reactor is connected with a product discharging pipeline.
According to the invention, the main body of the device is the fluidized reactor, the heating assembly and the fluidized reactor are separately installed, and the movable design of the heating assembly is convenient for controlling reaction conditions, and meanwhile, the heating assembly can be independently disassembled, so that the cost is greatly reduced; the discharge pipeline is convenient for discharging solid products, so that the problem of easy blockage is avoided, the separation of gas products is convenient for recycling tail gas, and the energy consumption is reduced.
The following technical solutions are preferred technical solutions of the present invention, but not limited to the technical solutions provided by the present invention, and technical objects and advantageous effects of the present invention can be better achieved and achieved by the following technical solutions.
As a preferable technical scheme of the invention, the fluidized reactor comprises a reaction section and a stripping section, wherein the reaction section is positioned at the lower part, the stripping section is positioned at the upper part, and the outer side of the reaction section is provided with a detachable heating component. In the stripping section, the gas can be stripped initially and the powder fixed.
As the preferable technical scheme of the invention, the heating assembly is longitudinally arranged, the top and the bottom of the heating assembly are provided with the pulleys and the positioning rails, and the pulleys drive the heating assembly to move along the positioning rails.
In the invention, for the movement of the heating assembly, a positioning track is arranged outside the fluidized reactor, so that the heating assembly can move along the horizontal direction of the positioning track, and the distance between the heating assembly and the reactor is adjusted, thereby controlling the reaction condition.
Preferably, the heating assembly is provided with at least 2, for example, 2, 3, 4 or 5, and the selection of the specific number is determined by the size and reaction requirements of the fluidized reactor and the heating assembly, and the heating assembly are uniformly arranged along the peripheral side of the fluidized reactor, so that the materials in the reactor are heated and uniformly reacted, and the uniformity of the carbon nanotube product is ensured.
As a preferable technical scheme of the invention, at least 2 gas-solid separators are arranged, and the gas-solid separators are arranged in parallel.
In the invention, at least 2 gas-solid separators are arranged in parallel, a stop valve is arranged in front of each gas-solid separator so as to be used alternately, and in the cleaning process after one of the gas-solid separators is blocked, the other gas-solid separator can be used continuously, thereby ensuring the continuous production efficiency and prolonging the period of shutdown maintenance, wherein the stop valves can be used normally under the high-temperature condition.
Preferably, at least 1 respirator is provided in each gas-solid separator, such as 1, 2, 3, or 4, etc.
Preferably, the lower part of the gas-solid separator is connected with a material receiving device, and the upper part of the gas-solid separator is provided with a back blowing hole.
In the invention, small particles are attached to the respirator in the production process, when the blockage of the respirator is not serious, gas can be blown in through the back blowing holes for simple cleaning, and blown powder is collected and recycled by the material receiving device.
As a preferable technical scheme of the invention, the exhaust pipeline of the gas-solid separator and the air inlet pipeline of the fluidized reactor form a heat exchange pipeline.
In the invention, the temperature of the discharged gas after reaction is still high, about 400 ℃, the discharged gas is directly discharged to cause heat waste and possibly heat damage, and the reaction raw gas is preheated by exchanging heat with the reaction inlet gas, so that the temperature rise time after entering the reactor is shortened, and the reaction rate is improved.
Preferably, a cooler is further arranged on the gas exhaust pipeline of the gas-solid separator.
According to the invention, after the shutdown, the reactor can be rapidly cooled through gas circulation, and the condenser is arranged on the gas exhaust pipeline, so that heat carried by the heated gas can be taken away, the gas can be recycled, the cooling period is shortened, and the furnace shutdown time is shortened.
As the preferable technical scheme of the invention, the product discharging pipeline is internally provided with flowing carrier gas.
According to the invention, the pressure in the discharge pipeline is lower than that at the outlet of the reactor through the rapid flowing of the carrier gas, so that jet type negative pressure discharge of reaction products is realized, and the problem of material blockage caused by the fact that material powder is easily compacted at the outlet during positive pressure discharge is avoided. The carrier gas may be nitrogen or inert gas, which is not easy to react with the product.
In another aspect, the present invention provides a method for preparing carbon nanotubes using the above apparatus, the method comprising:
and (2) placing the catalyst in a fluidized reactor, heating to raise the temperature, then introducing organic carbon source gas and carrier gas to react, discharging the reacted gas after gas-solid separation, and discharging a solid product under negative pressure to obtain the carbon nano tube.
As a preferred embodiment of the present invention, the catalyst comprises a transition metal catalyst, preferably any one or a combination of at least two of nickel-based, cobalt-based, iron-based, copper-based or rare earth metal catalysts, and the combination is exemplified by, but not limited to: a combination of a nickel-based catalyst and a cobalt-based catalyst, a combination of a cobalt-based catalyst and an iron-based catalyst, a combination of a nickel-based catalyst, a copper-based catalyst, and a rare earth metal catalyst, and the like.
Preferably, before the catalyst is added, a carrier gas is used for purging, and air is discharged.
Preferably, the organic carbon source gas comprises any one of, or a combination of at least two of, propylene, methane, propane or acetylene, typical but non-limiting examples of which are: combinations of propylene and methane, combinations of propylene and propane, combinations of methane, propane, and acetylene, combinations of propylene, methane, and propane, and the like.
In the invention, organic carbon source gas is subjected to cracking reaction under the action of a catalyst to obtain the carbon nano tube.
Preferably, the carrier comprises any one of nitrogen, helium, neon or argon, or a combination of at least two of these, typical but non-limiting examples being: combinations of nitrogen and helium, helium and neon, helium, neon and argon, and the like.
Preferably, the volume ratio of the organic carbon source gas to the carrier gas is (0.6 to 3):1, for example, 0.6:1, 1:1, 1.5:1, 2:1, 2.5:1 or 3:1, but the organic carbon source gas is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
In the invention, the carrier and the organic carbon source gas are introduced together in the reaction process, and the introduction of the carrier gas can effectively reduce the concentration of the carbon source gas, thereby avoiding the phenomenon that the reaction gas is easy to generate side reaction due to overhigh partial pressure to influence the yield and the purity of the product.
In a preferred embodiment of the present invention, the reaction temperature is 600 to 1000 ℃, for example, 600 ℃, 650 ℃, 700 ℃, 750 ℃, 800 ℃, 850 ℃, 900 ℃, 950 ℃ or 1000 ℃, but the reaction temperature is not limited to the above-mentioned values, and other values not listed in the above-mentioned range are also applicable.
Preferably, the reaction time is 60 to 90min, such as 60min, 65min, 70min, 75min, 80min, 85min, or 60min, but is not limited to the recited values, and other unrecited values within the range of values are also applicable.
As a preferable technical scheme of the invention, the reacted gas is subjected to gas-solid separation and then exchanges heat with the organic carbon source gas in the gas inlet pipeline.
Preferably, in the negative pressure discharge, the pressure of the carrier gas in the product discharge line is 0.1 to 0.8MPa, such as 0.1MPa, 0.2MPa, 0.4MPa, 0.5MPa, 0.6MPa, 0.7MPa, or 0.8MPa, but is not limited to the recited values, and other values not recited in the range of the values are also applicable; the product material flow rate is 20-180L/min, such as 20L/min, 40L/min, 60L/min, 80L/min, 100L/min, 120L/min, 140L/min, 160L/min or 180L/min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, when the fluidized reactor is stopped and cleaned, the gas circulates in the exhaust pipeline and the fluidized reactor, and the heated gas is cooled by the cooler in a circulating manner.
Compared with the prior art, the invention has the following beneficial effects:
(1) the device disclosed by the invention has the advantages that through the improvement of heating and separation components of the fluidized reactor, the movement, the installation and the disassembly of the heating components are facilitated, the maintenance cost is greatly reduced, meanwhile, the products can be quickly separated, the device is not easy to block, and the production efficiency of the device is improved;
(2) the discharging mode of the solid product can effectively avoid the problem that powder is easy to be compacted to cause blockage when discharging under positive pressure;
(3) The arrangement of the heat exchange and cooling pipelines effectively improves the utilization rate of heat, reduces energy consumption, shortens the cooling period of the device and reduces the production stop time.
Drawings
FIG. 1 is a schematic view of the structure of an apparatus for producing carbon nanotubes provided in example 1 of the present invention;
the system comprises a fluidized reactor 1, a heating assembly 2, a pulley 3, a positioning rail 4, a gas-solid separator 5, a respirator 6, a product discharge pipeline 7 and a cooler 8.
Detailed Description
In order to better explain the present invention and to facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following examples are only simple examples of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
The invention provides a carbon nanotube preparation device and a method, the device comprises a fluidized reactor 1, a detachable heating component 2 is arranged on the outer side of the main body of the fluidized reactor 1, and the heating component 2 and the main body of the fluidized reactor 1 are arranged in parallel and move along the horizontal direction;
an outlet at the upper part of the fluidized reactor 1 is connected with a gas-solid separator 5, and an outlet at the lower part of the fluidized reactor 1 is connected with a product discharge pipeline 7.
The method comprises the following steps: placing the catalyst in a fluidized reactor 1, heating, introducing organic carbon source gas and carrier gas, reacting, discharging the reacted gas after gas-solid separation, and discharging the solid product under negative pressure to obtain the carbon nano tube.
The following are typical but non-limiting examples of the invention:
example 1:
the embodiment provides a carbon nanotube preparation device, the structural schematic diagram of which is shown in fig. 1, and the device comprises a fluidized reactor 1, wherein a detachable heating component 2 is arranged on the outer side of the main body of the fluidized reactor 1, and the heating component 2 is arranged in parallel with the main body of the fluidized reactor 1 and moves along the horizontal direction;
an outlet at the upper part of the fluidized reactor 1 is connected with a gas-solid separator 5, and an outlet at the lower part of the fluidized reactor 1 is connected with a product discharging pipeline 7.
The fluidized reactor 1 comprises a reaction section and a stripping section, the reaction section is positioned at the lower part, the stripping section is positioned at the upper part, and the outer side of the reaction section is provided with a detachable heating component 2.
The heating assembly 2 is longitudinally arranged, pulleys 3 and a positioning rail 4 are arranged at the top and the bottom of the heating assembly 2, and the pulleys 3 drive the heating assembly 2 to move along the positioning rail 4; the number of the heating assemblies 2 is 2, and the heating assemblies are symmetrically arranged along the outer side of the fluidized reactor 1.
2 gas-solid separators 5 are arranged, and the gas-solid separators 5 are arranged in parallel; each gas-solid separator 5 is provided with 3 respirators.
The lower part of the gas-solid separator 5 is connected with a material receiving device, and the upper part of the gas-solid separator 5 is provided with a back blowing hole.
The exhaust pipeline of the gas-solid separator 5 and the air inlet pipeline of the fluidized reactor 1 form a heat exchange pipeline; and a cooler 8 is also arranged on the exhaust pipeline of the gas-solid separator 5.
And flowing nitrogen is arranged in the product discharge pipeline 7, so that the material at the outlet of the fluidized reactor 1 is jetted out in a jet mode.
Example 2:
the embodiment provides a carbon nanotube preparation device, which comprises a fluidized reactor 1, wherein a detachable heating component 2 is arranged on the outer side of the main body of the fluidized reactor 1, and the heating component 2 and the main body of the fluidized reactor 1 are arranged in parallel and move along the horizontal direction;
an outlet at the upper part of the fluidized reactor 1 is connected with a gas-solid separator 5, and an outlet at the lower part of the fluidized reactor 1 is connected with a product discharging pipeline 7.
The fluidized reactor 1 comprises a reaction section and a stripping section, the reaction section is positioned at the lower part, the stripping section is positioned at the upper part, and the outer side of the reaction section is provided with a detachable heating component 2.
The heating assembly 2 is longitudinally arranged, pulleys 3 and a positioning rail 4 are arranged at the top and the bottom of the heating assembly 2, and the pulleys 3 drive the heating assembly 2 to move along the positioning rail 4; the number of the heating assemblies 2 is 4, and the heating assemblies are uniformly arranged on the outer side of the fluidized reactor 1.
The number of the gas-solid separators 5 is 3, and the gas-solid separators 5 are arranged in parallel; each gas-solid separator 5 is provided with 2 respirators.
The lower part of the gas-solid separator 5 is connected with a material receiving device, and the upper part of the gas-solid separator 5 is provided with a back blowing hole.
The exhaust pipeline of the gas-solid separator 5 and the air inlet pipeline of the fluidized reactor 1 form a heat exchange pipeline; and a cooler 8 is also arranged on the exhaust pipeline of the gas-solid separator 5.
And flowing neon is arranged in the product discharge pipeline 7, so that the material at the outlet of the fluidized reactor 1 is jetted out in a jet mode.
Example 3:
this example provides a method for preparing carbon nanotubes, the method using the apparatus of example 1, comprising the steps of:
purging the fluidized reactor 1 by using nitrogen, discharging air, adding a Ni/Y/Cu ternary catalyst, starting the heating assembly 2, raising the temperature to 800 ℃, introducing propylene and nitrogen with a volume ratio of 1.5:1, reacting for 80min, allowing the reacted gas to enter an exhaust pipeline through gas-solid separation, exchanging heat with the propylene in an air inlet pipeline, discharging a solid product under negative pressure, controlling the pressure of the nitrogen in a product discharging pipeline 7 to be 0.4MPa, wherein the flow of the product material is 100L/min, and separating to obtain the carbon nano tube;
After the fluidized reactor 1 is stopped, nitrogen is adopted to circulate in the exhaust pipeline and the fluidized reactor 1 to cool the reactor, and the heat absorbed by the nitrogen is taken away by a cooler 8.
In the embodiment, after the reaction, the conversion rate of propylene can reach 65%, the carbon nano tubes are uniformly distributed in tube diameter, and the tube walls are clean; the device theoretically does not need blowing out and cleaning without switching products, the cooling rate is high after the device stops running, and the cooling time can be shortened by over 60 percent.
Example 4:
this example provides a method for preparing carbon nanotubes, the method using the apparatus of example 1, comprising the steps of:
purging the fluidized reactor 1 by using argon gas, discharging air, adding a Ni/Ce/Cu ternary catalyst, starting the heating assembly 2, raising the temperature to 1000 ℃, introducing propylene and argon gas with the volume ratio of 0.6:1, reacting for 60min, allowing the reacted gas to enter an exhaust pipeline through gas-solid separation to exchange heat with the propylene in an air inlet pipeline, discharging a solid product under negative pressure, allowing the pressure of nitrogen in a product discharging pipeline 7 to be 0.1MPa, wherein the flow of the product material is 30L/min, and separating to obtain the carbon nano tube;
after the fluidized reactor 1 is stopped, argon is adopted to circulate in the exhaust pipeline and the fluidized reactor 1 to cool the reactor, and the heat absorbed by the argon is taken away by the cooler 8.
In the embodiment, after the reaction, the conversion rate of propylene can reach 68 percent, the carbon nano tubes are uniformly distributed in tube diameter, and the tube walls are clean; the device theoretically does not need blowing out for cleaning without switching products, the cooling rate is high after the device stops running, and the cooling time can be shortened by more than 70%.
Example 5:
this example provides a method for preparing carbon nanotubes, which is performed using the apparatus of example 2, and includes the following steps:
blowing the fluidized reactor 1 by neon, discharging air, adding a Co/Ce composite catalyst, starting a heating assembly 2, heating to 600 ℃, introducing propylene and neon with a volume ratio of 3:1, reacting for 90min, allowing the reacted gas to enter an exhaust pipeline through gas-solid separation for heat exchange with the propylene in an air inlet pipeline, discharging a solid product under negative pressure, allowing the pressure of the neon in a product discharging pipeline 7 to be 0.8MPa, wherein the flow of the product material is 180L/min, and separating to obtain a carbon nano tube;
after the fluidized reactor 1 is stopped, argon is adopted to circulate in the exhaust pipeline and the fluidized reactor 1 to cool the reactor, and the heat absorbed by the argon is taken away by the cooler 8.
In the embodiment, after the reaction, the conversion rate of propylene can reach 71%, the carbon nano tubes are uniformly distributed in tube diameter, and the tube walls are clean; the device theoretically does not need blowing out for cleaning without switching products, the cooling rate is high after the device stops running, and the cooling time can be shortened by more than 50%.
The device is convenient to move, install and disassemble by improving the heating of the fluidized reactor and the separation component, greatly reduces the maintenance cost, can quickly separate products, is not easy to block, and improves the production efficiency of the device; the solid product discharging mode can effectively avoid the problem that powder is easy to be compacted to cause blockage when discharging under positive pressure; the heat exchange and cooling pipelines are arranged, so that the heat utilization rate is effectively improved, the energy consumption is reduced, the cooling period of the device is shortened, and the production stop time is reduced.
The applicant states that the present invention is illustrated by the detailed apparatus and method of the present invention through the above embodiments, but the present invention is not limited to the above detailed apparatus and method, i.e. it is not meant to imply that the present invention must be implemented by the above detailed apparatus and method. It will be apparent to those skilled in the art that any modifications to the present invention, equivalents of the means for substitution and addition of means for carrying out the invention, selection of specific means, etc., are within the scope and disclosure of the invention.
Claims (19)
1. The carbon nanotube preparation device is characterized by comprising a fluidized reactor, wherein a detachable heating component is arranged on the outer side of the main body of the fluidized reactor, and the heating component and the main body of the fluidized reactor are arranged in parallel and move along the horizontal direction; the heating assembly is longitudinally arranged, pulleys and positioning rails are arranged at the top and the bottom of the heating assembly, and the pulleys drive the heating assembly to move along the positioning rails;
An outlet at the upper part of the fluidized reactor is connected with a gas-solid separator, the lower part of the gas-solid separator is connected with a material receiving device, and the upper part of the gas-solid separator is provided with a back blowing hole; the lower outlet of the fluidized reactor is connected with a product discharge pipeline, and flowing carrier gas is arranged in the product discharge pipeline.
2. The carbon nanotube production apparatus according to claim 1, wherein the fluidized reactor comprises a reaction section and a stripping section, the reaction section is located at a lower portion, the stripping section is located at an upper portion, and a detachable heating assembly is provided at an outer side of the reaction section.
3. The carbon nanotube production apparatus according to claim 1, wherein the number of the heating units is at least 2, and the heating units are uniformly arranged along the circumferential side of the fluidized reactor.
4. The carbon nanotube production apparatus according to claim 1, wherein the number of the gas-solid separators is at least 2, and the gas-solid separators are arranged in parallel.
5. The carbon nanotube production apparatus according to claim 4, wherein at least 1 respirator is provided in each gas-solid separator.
6. The apparatus of claim 1, wherein the gas outlet line of the gas-solid separator and the gas inlet line of the fluidized reactor form a heat exchange line.
7. The carbon nanotube production apparatus according to claim 6, wherein a cooler is further provided on the gas discharge line of the gas-solid separator.
8. A method for preparing carbon nanotubes using the apparatus of any one of claims 1 to 7, comprising:
placing the catalyst in a fluidized reactor, heating to raise the temperature, then introducing organic carbon source gas and carrier gas to react, discharging the reacted gas after gas-solid separation, and discharging the solid product under negative pressure to obtain the carbon nano tube.
9. The method of claim 8, wherein the catalyst comprises a transition metal catalyst.
10. The method of claim 9, wherein the catalyst is any one of nickel-based, cobalt-based, iron-based, copper-based, or rare earth metal catalyst or a combination of at least two thereof.
11. The method of claim 8, wherein prior to the introduction of the catalyst, the carrier gas is used to purge the air.
12. The method of claim 8, wherein the organic carbon source gas comprises any one of propylene, methane, propane, or acetylene, or a combination of at least two thereof.
13. The method of claim 8, wherein the carrier comprises any one of nitrogen, helium, neon, or argon, or a combination of at least two thereof.
14. The method according to claim 8, wherein the volume ratio of the organic carbon source gas to the carrier gas is (0.6-3): 1.
15. The method according to claim 8, wherein the reaction temperature is 600 to 1000 ℃.
16. The method according to claim 8, wherein the reaction time is 60 to 90 min.
17. The method as claimed in claim 8, wherein the reacted gas undergoes gas-solid separation and then exchanges heat with the organic carbon source gas in the gas inlet pipeline.
18. The method according to claim 8, wherein during the negative pressure discharging, the pressure of the carrier gas in the product discharging pipeline is 0.1-0.8 MPa, and the flow rate of the product material is 20-180L/min.
19. The method as claimed in claim 8, wherein when the fluidized reactor is stopped for cleaning, the gas circulates in the exhaust pipeline and the fluidized reactor, and the gas after passing through the fluidized reactor is cooled by a cooler in a circulating manner.
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