CN111686650A - Carbon nanotube preparation device and method - Google Patents

Abstract

The invention provides a carbon nanotube preparation device and method. The device includes a fluidized reactor, and a dismountable heating assembly is arranged on the outside of the main body of the fluidized reactor, and the heating assembly is parallel to the main body of the fluidized reactor. set and move along the horizontal direction; the upper outlet of the fluidized reactor is connected with a gas-solid separator, and the lower outlet of the fluidized reactor is connected with a product discharge pipeline. Through the improvement of the heating of the fluidized reactor and the separation of the components, the device of the invention facilitates the movement, installation and disassembly of the heating components, greatly reduces the maintenance cost, and at the same time enables the rapid separation of the products, the device is not easy to be blocked, and the production efficiency of the device is improved ; The discharge method of solid products can effectively avoid the problem that the powder is easily compacted and cause blockage during positive pressure discharge; the setting of heat exchange and cooling pipelines can effectively improve the utilization rate of heat, reduce energy consumption, and at the same time Shorten the cooling cycle of the device and reduce the time of production shutdown.

Description

A kind of carbon nanotube preparation device and method

technical field

The invention belongs to the technical field of nanomaterial preparation, and relates to a carbon nanotube preparation device and method.

Background technique

Carbon nanotubes are one-dimensional quantum materials with special structures, which have the advantages of low bulk density, large specific surface area, excellent mechanical properties, and good thermal conductivity and electrical conductivity. Although the structure of carbon nanotubes is similar to that of polymer materials, the structure The stability is obviously better than the latter, and it is one of the materials with the highest specific strength.

At present, the preparation methods of carbon nanotubes mainly include arc discharge method, laser ablation method, chemical vapor deposition method, solid-phase pyrolysis method, glow discharge method, gas combustion method and polymerization synthesis method, among which the more mature methods are chemical vapor deposition. Chemical vapor deposition, also known as hydrocarbon gas pyrolysis, is to obtain carbon nanotubes by cracking carbon-containing gas under the action of a catalyst, and the yield is high. However, due to the inherent low reaction temperature of chemical vapor deposition, carbon nanotubes are produced. The low degree of crystallinity leads to a high defect content of carbon nanotubes prepared by chemical vapor deposition, which greatly limits properties such as electrical conductivity.

CN 110217777A discloses a carbon nanotube preparation device and method. The device consists of a catalyst evaporation chamber, a chemical vapor deposition chamber and a gas-solid separation chamber connected in series. The high temperature and impact generated by an electric arc flame are used to directly remove the catalyst in the catalyst evaporation chamber. It evaporates into an ultra-fine catalyst, and enters the chemical vapor deposition chamber through the connecting channel. At the same time, the carrier gas and the carbon source gas are respectively introduced into the catalyst evaporation chamber and the chemical vapor deposition chamber. The catalyst reacts with the organic carbon source cracked at high temperature to generate carbon nanotubes. , and then separated and collected by a gas-solid separation device. The required reaction temperature of the device is high, that is, the reaction energy consumption is high, the stability of the catalyst is required to be high, and the device scale is small.

The preparation of carbon nanotubes often uses a fluidized bed reactor. Due to the structural characteristics of carbon nanotubes, it is easy to agglomerate. When using a fluidized bed reactor to produce carbon nanotubes, it is easy to agglomerate in the production of carbon nanotubes. Accumulation is formed on the inner wall, and it is difficult to be carried out with the air flow when discharging. CN 205761066U discloses a self-cleaning fluidized bed reactor for carbon nanotube production, comprising a fluidized bed reactor body with a reaction chamber and a rotating device arranged in the reaction chamber, the rotating device comprising longitudinally arranged along the center of the reaction chamber The rotating shaft and the rotating body connected with the rotating shaft, the reaction chamber is provided with an inflow port and an outflow port, the rotating shaft is communicated with the inflow port, and the rotating body is provided with a number of pipes facing the inner wall of the reaction chamber and communicating with the rotating shaft for gas outflow. This device is mainly a corresponding improvement to the problem of material sticking to the wall in the reaction chamber, but it does not involve the existing problems such as material blocking, slow cooling, and difficulty in disassembly.

To sum up, the design and improvement of the carbon nanotube preparation device needs to be able to improve the production efficiency, shorten the production cycle, and make its structure suitable for the reaction, reduce energy consumption, and be suitable for large-scale application.

SUMMARY OF THE INVENTION

In view of the problems existing in the prior art, the purpose of the present invention is to provide a carbon nanotube preparation device and method. At the same time, the product can be quickly separated, the device is not easily blocked, the shutdown time can be effectively shortened, and the production efficiency can be improved.

For this purpose, the present invention adopts the following technical solutions:

In one aspect, the present invention provides a carbon nanotube preparation device, the device includes a fluidized reactor, and a detachable heating assembly is provided on the outside of the main body of the fluidized reactor, and the heating assembly is connected to the main body of the fluidized reactor. Set side by side, moving in the horizontal direction;

The upper outlet of the fluidized reactor is connected with a gas-solid separator, and the lower outlet of the fluidized reactor is connected with a product discharge pipeline.

In the present invention, the main body of the device is a fluidized reactor. By installing the heating component and the fluidized reactor separately, the mobile design of the heating component facilitates the control of reaction conditions, and can be disassembled separately, which greatly reduces the Cost; the setting of the discharge pipeline is convenient for the discharge of solid products and avoids the problem of easy blockage, and the separation of gas products is convenient for the reuse of tail gas and reduces energy consumption.

The following are the preferred technical solutions of the present invention, but not as limitations of the technical solutions provided by the present invention. Through the following technical solutions, the technical purpose and beneficial effects of the present invention can be better achieved and realized.

As a preferred technical solution of the present invention, the fluidized reactor includes a reaction section and a stripping section, the reaction section is located at the lower part, the stripping section is located at the upper part, and a detachable heating assembly is provided outside the reaction section. In the stripping section, the gas can be initially stripped, and the powder can be fixed.

As a preferred technical solution of the present invention, the heating assembly is arranged longitudinally, and the top and bottom of the heating assembly are provided with pulleys and positioning tracks, and the pulleys drive the heating assembly to move along the positioning tracks.

In the present invention, in order to move the heating assembly, a positioning track is set outside the fluidized reactor, so that the heating assembly can move along the horizontal direction of the positioning track and adjust the distance from the reactor, so that the reaction conditions can be controlled.

Preferably, there are at least 2 heating components, such as 2, 3, 4 or 5, etc. The selection of the specific number is determined by the size of the fluidized reactor and the heating component and the reaction needs. The peripheral side of the reactor is evenly arranged, which facilitates the heating and uniform reaction of materials in the reactor, and ensures the uniformity of carbon nanotube products.

As a preferred technical solution of the present invention, there are at least two gas-solid separators, and the gas-solid separators are arranged in parallel.

In the present invention, at least two gas-solid separators are arranged in parallel, and each gas-solid separator is provided with a shut-off valve in front of it to facilitate alternate use. During the cleaning process after one of them is blocked, the other can continue to be used to ensure that Continuous production efficiency, extending the period of downtime and maintenance, and the shut-off valve can be used normally under high temperature conditions.

Preferably, each gas-solid separator is provided with at least one respirator, such as one, two, three or four, 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 backflushing air hole.

In the present invention, there will be small particles attached to the respirator during the production process. When the respirator is not seriously blocked, gas can be blown into the back blowing air hole for simple cleaning, and the blown powder is collected and reused by the feeding device. .

As a preferred technical solution of the present invention, the exhaust pipeline of the gas-solid separator and the intake pipeline of the fluidized reactor constitute a heat exchange pipeline.

In the present invention, the temperature of the exhaust gas after the reaction is still relatively high, about 400° C., the direct exhaust causes heat waste and may also bring thermal damage. By exchanging heat with the reaction inlet gas, the reaction raw material gas is preheated , shorten the heating time after entering the reactor, thereby increasing the reaction rate.

Preferably, a cooler is further provided on the exhaust pipeline of the gas-solid separator.

In the present invention, after the shutdown, the reactor can be rapidly cooled by gas circulation, and a condenser is arranged on the exhaust pipeline to take away the heat carried by the heated gas, so as to facilitate the recycling of the gas, shorten the cooling cycle, and reduce the Downtime.

As a preferred technical solution of the present invention, the product discharge pipeline is provided with a flowing carrier gas.

In the present invention, the pressure in the discharge pipeline is lower than that at the outlet of the reactor through the rapid flow of the carrier gas, so as to realize the jet-type negative pressure discharge of the reaction product, and avoid the material powder being easily at the outlet during positive pressure discharge. The problem of blockage caused by compaction. Among them, the carrier gas can be selected as 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 device, the method comprising:

The catalyst is placed in a fluidized reactor, heated and heated, and then an organic carbon source gas and a carrier gas are introduced to react. After the reaction, the gas is discharged after gas-solid separation, and the solid product is discharged under negative pressure to obtain carbon nanotubes.

As a preferred technical solution of the present invention, the catalyst includes 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, the combination is typical but not Limiting examples are: 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 to discharge air.

Preferably, the organic carbon source gas comprises any one or a combination of at least two of propylene, methane, propane or acetylene. Typical but non-limiting examples of the combination include: a combination of propylene and methane, a combination of propylene and propane , a combination of methane, propane and acetylene, a combination of propylene, methane and propane, etc.

In the present invention, the organic carbon source gas undergoes a cracking reaction under the action of a catalyst to obtain carbon nanotubes.

Preferably, the carrier comprises any one or a combination of at least two of nitrogen, helium, neon or argon, and typical but non-limiting examples of the combination are: a combination of nitrogen and helium, helium and neon A combination of gas, helium, neon, and argon, etc.

Preferably, the volume ratio of the organic carbon source gas to the carrier gas is (0.6-3):1, such as 0.6:1, 1:1, 1.5:1, 2:1, 2.5:1 or 3:1, etc., However, it is not limited to the recited numerical values, and other unrecited numerical values within the numerical range are equally applicable.

In the present 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, avoid the reaction gas from being prone to side reactions due to excessive partial pressure, and affect the yield of the product with purity.

As a preferred technical solution of the present invention, the reaction temperature is 600-1000°C, such as 600°C, 650°C, 700°C, 750°C, 800°C, 850°C, 900°C, 950°C or 1000°C, etc. Not limited to the recited values, other non-recited values within this range of values are equally applicable.

Preferably, the reaction time is 60～90min, such as 60min, 65min, 70min, 75min, 80min, 85min or 60min, etc., but is not limited to the enumerated numerical values, and other unenumerated numerical values within this numerical range are also applicable.

As a preferred technical solution of the present invention, the reacted gas is subjected to heat exchange with the organic carbon source gas in the intake pipeline after gas-solid separation.

Preferably, when the negative pressure is discharging, the pressure of the carrier gas in the product discharging pipeline is 0.1-0.8 MPa, for example, 0.1 MPa, 0.2 MPa, 0.2 MPa, 0.4 MPa, 0.5 MPa, 0.6 MPa, 0.7 MPa or 0.8 MPa MPa, etc., but not limited to the listed values, other unlisted values within this value range are also applicable; product material flow 20 ~ 180L/min, such as 20L/min, 40L/min, 60L/min, 80L/min, 100L/min, 120L/min, 140L/min, 160L/min or 180L/min, etc., but not limited to the listed values, and other unlisted values within the numerical range are also applicable.

Preferably, when the fluidized reactor is shut down for cleaning, the gas circulates in the exhaust pipeline and the fluidized reactor, and the heated gas is circulated and cooled by the cooler.

Compared with the prior art, the present invention has the following beneficial effects:

(1) The device of the present invention facilitates the movement, installation and disassembly of the heating assembly through the improvement of the heating of the fluidized reactor and the separation component, which greatly reduces the maintenance cost, and at the same time, the product can be quickly separated, the device is not easily blocked, and the device production efficiency;

(2) the discharging method of the solid product of the present invention can effectively avoid the problem that the powder is easily compacted and causes blockage when the positive pressure is discharging;

(3) The arrangement of heat exchange and cooling pipelines in the present invention effectively improves the utilization rate of heat, reduces energy consumption, shortens the cooling cycle of the device, and reduces the time of production shutdown.

Description of drawings

1 is a schematic structural diagram of a carbon nanotube preparation device provided in Example 1 of the present invention;

Among them, 1- fluidized reactor, 2- heating assembly, 3- pulley, 4- positioning track, 5- gas-solid separator, 6- breathing apparatus, 7- product discharge pipeline, 8- cooler.

Detailed ways

In order to better illustrate the present invention and facilitate understanding of the technical solutions of the present invention, the present invention is further described in detail below. However, the following embodiments are only simple examples of the present invention, and do not represent or limit the protection scope of the present invention, and the protection scope of the present invention is subject to the claims.

The specific embodiment of the present invention provides a carbon nanotube preparation device and method, the device includes a fluidized reactor 1, and a detachable heating component 2 is provided on the outside of the main body of the fluidized reactor 1. The heating component 2 is arranged in parallel with the main body of the fluidized reactor 1 and moves in the horizontal direction;

The upper outlet of the fluidized reactor 1 is connected with a gas-solid separator 5 , and the lower outlet of the fluidized reactor 1 is connected with a product discharge pipeline 7 .

The method comprises: placing the catalyst in the fluidized reactor 1, heating and raising the temperature, then introducing organic carbon source gas and carrier gas to react, the reacted gas is discharged after gas-solid separation, and the solid product is discharged under negative pressure to obtain carbon nanotubes.

The following are typical but non-limiting examples of the present invention:

Example 1:

This embodiment provides a carbon nanotube preparation device. The schematic structural diagram of the device is shown in FIG. 1 , including a fluidized reactor 1. The outer side of the main body of the fluidized reactor 1 is provided with a detachable heating assembly 2. The heating assembly 2 is arranged side by side with the main body of the fluidized reactor 1 and moves in the horizontal direction;

The upper outlet of the fluidized reactor 1 is connected with a gas-solid separator 5 , and the lower outlet of the fluidized reactor 1 is connected with a product discharge pipeline 7 .

The fluidized reactor 1 includes a reaction section and a stripping section, the reaction section is located at the lower part, the stripping section is located at the upper part, and a detachable heating assembly 2 is provided outside the reaction section.

The heating assembly 2 is arranged longitudinally. The top and bottom of the heating assembly 2 are provided with pulleys 3 and a positioning track 4. The pulley 3 drives the heating assembly 2 to move along the positioning track 4; The outside of the chemical reactor 1 is symmetrically arranged.

Two gas-solid separators 5 are provided, and the gas-solid separators 5 are arranged in parallel; each gas-solid separator 5 is provided with three breathing apparatuses.

The lower part of the gas-solid separator 5 is connected with a feeding device, and the upper part of the gas-solid separator 5 is provided with a back blowing air hole.

The exhaust pipeline of the gas-solid separator 5 and the intake pipeline of the fluidized reactor 1 constitute a heat exchange pipeline; the exhaust pipeline of the gas-solid separator 5 is also provided with a cooler 8 .

The product discharge pipeline 7 is provided with flowing nitrogen, so that the material jet at the outlet of the fluidized reactor 1 is ejected.

Example 2:

This embodiment provides a carbon nanotube preparation device, the device includes a fluidized reactor 1, and a dismountable heating component 2 is provided on the outside of the main body of the fluidized reactor 1, and the heating component 2 reacts with the fluidized reactor 1. The main body of the device 1 is arranged side by side and moves in the horizontal direction;

The upper outlet of the fluidized reactor 1 is connected with a gas-solid separator 5 , and the lower outlet of the fluidized reactor 1 is connected with a product discharge pipeline 7 .

The fluidized reactor 1 includes a reaction section and a stripping section, the reaction section is located at the lower part, the stripping section is located at the upper part, and a detachable heating assembly 2 is provided outside the reaction section.

The heating assembly 2 is arranged longitudinally. The top and bottom of the heating assembly 2 are provided with pulleys 3 and a positioning track 4. The pulley 3 drives the heating assembly 2 to move along the positioning track 4; The outside of the chemical reactor 1 is evenly arranged.

There are three gas-solid separators 5, and the gas-solid separators 5 are arranged in parallel; each gas-solid separator 5 is provided with two breathing apparatuses.

The lower part of the gas-solid separator 5 is connected with a feeding device, and the upper part of the gas-solid separator 5 is provided with a back blowing air hole.

The exhaust pipeline of the gas-solid separator 5 and the intake pipeline of the fluidized reactor 1 constitute a heat exchange pipeline; the exhaust pipeline of the gas-solid separator 5 is also provided with a cooler 8 .

The product discharge pipeline 7 is provided with flowing neon gas, so that the material jet at the outlet of the fluidized reactor 1 is ejected.

Example 3:

The present embodiment provides a method for preparing carbon nanotubes. The method is carried out by using the device of Embodiment 1, and includes the following steps:

The fluidized reactor 1 was purged with nitrogen gas, the air was discharged, and then the Ni/Y/Cu three-way catalyst was added, the heating component 2 was started and the temperature was raised to 800 ° C, propylene and nitrogen with a volume ratio of 1.5:1 were introduced, and the reaction was carried out for 80 min. The reacted gas enters the exhaust pipeline and the propylene in the intake pipeline through gas-solid separation for heat exchange, the solid product is discharged under negative pressure, the pressure of nitrogen in the product discharge pipeline 7 is 0.4MPa, and the flow rate of the product material is is 100L/min, and carbon nanotubes are obtained through separation;

After the fluidized reactor 1 is stopped, nitrogen is used to circulate in the exhaust pipeline and the fluidized reactor 1 to cool down the reactor, and the heat absorbed by the nitrogen is taken away by the cooler 8 .

In this example, after the reaction, the conversion rate of propylene can reach 65%, the carbon nanotube diameters are evenly distributed, and the tube walls are clean; the device theoretically does not need to be shut down for cleaning without switching products, and the cooling rate is fast after the operation is stopped. The cooling time can be shortened by more than 60%.

Example 4:

The present embodiment provides a method for preparing carbon nanotubes. The method is carried out by using the device of Embodiment 1, and includes the following steps:

The fluidized reactor 1 was purged with argon gas, the air was discharged, then Ni/Ce/Cu ternary catalyst was added, the heating component 2 was started to heat up to 1000°C, and propylene and argon gas with a volume ratio of 0.6:1 were introduced to react. 60min, the reacted gas enters the exhaust pipeline and the propylene in the intake pipeline through gas-solid separation for heat exchange, the solid product is discharged under negative pressure, and the pressure of nitrogen in the product discharge pipeline 7 is 0.1MPa, wherein the product material The flow rate is 30L/min, and carbon nanotubes are obtained after separation;

After the fluidized reactor 1 is stopped, argon gas is used to circulate in the exhaust pipeline and the fluidized reactor 1 to cool down the reactor, and the heat absorbed by the argon gas is taken away by the cooler 8 .

In this example, after the reaction, the conversion rate of propylene can reach 68%, the diameter of carbon nanotubes is evenly distributed, and the tube wall is clean; the device theoretically does not need to be shut down for cleaning without switching products, and the cooling rate is fast after stopping operation, The cooling time can be shortened by more than 70%.

Example 5:

The present embodiment provides a method for preparing carbon nanotubes. The method is carried out by using the device of embodiment 2, and includes the following steps:

The fluidized reactor 1 was purged with neon gas, the air was exhausted, the Co/Ce composite catalyst was added, the heating element 2 was started and the temperature was raised to 600° C., propylene and neon gas with a volume ratio of 3:1 were introduced, and the reaction was performed for 90 min. The latter gas enters the exhaust pipeline and the propylene in the intake pipeline through gas-solid separation for heat exchange, and the solid product is discharged under negative pressure. The pressure of the neon gas in the product discharge pipeline 7 is 0.8MPa, and the flow rate of the product material is is 180L/min, and carbon nanotubes are obtained through separation;

After the fluidized reactor 1 is stopped, argon gas is used to circulate in the exhaust pipeline and the fluidized reactor 1 to cool down the reactor, and the heat absorbed by the argon gas is taken away by the cooler 8 .

In this example, after the reaction, the conversion rate of propylene can reach 71%, the carbon nanotube diameters are evenly distributed, and the tube walls are clean; the device theoretically does not need to be shut down for cleaning without switching products, and the cooling rate is fast after the operation is stopped. The cooling time can be shortened by more than 50%.

Combining the above embodiments, it can be seen that the device of the present invention facilitates the movement, installation and disassembly of the heating assembly through the improvement of the heating and separation components of the fluidized reactor, which greatly reduces the maintenance cost, and at the same time enables the rapid separation of products, The device is not easy to be blocked, and the production efficiency of the device is improved; the discharge method of solid products can effectively avoid the problem that the powder is easily compacted and cause blockage when the material is discharged under positive pressure; the setting of heat exchange and cooling pipelines effectively improves the heat dissipation Utilization rate, reduce energy consumption, shorten the cooling cycle of the device, and reduce the time of production shutdown.

The applicant declares that the present invention illustrates the detailed apparatus and method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed apparatus and method, that is, it does not mean that the present invention must rely on the above-mentioned detailed apparatus and method to be implemented. Those skilled in the art should understand that any improvement to the present invention, equivalent replacement of the device of the present invention, addition of auxiliary devices, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims (10)

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;

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.

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 member is provided at an outer side of the reaction section.

3. The apparatus of claim 1 or 2, wherein the heating assembly is disposed longitudinally, and a pulley and a positioning rail are disposed at the top and the bottom of the heating assembly, and the pulley drives the heating assembly to move along the positioning rail;

preferably, the heating assemblies are at least 2 and are uniformly arranged along the peripheral side of the fluidized reactor.

4. The carbon nanotube production apparatus according to any one of claims 1 to 3, wherein the gas-solid separators are provided in number of at least 2, and the gas-solid separators are arranged in parallel;

preferably, at least 1 respirator is arranged in each gas-solid separator;

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.

5. The carbon nanotube production apparatus according to any one of claims 1 to 4, wherein the exhaust line of the gas-solid separator and the inlet line of the fluidized reactor constitute a heat exchange line;

preferably, a cooler is further arranged on the exhaust pipeline of the gas-solid separator.

6. The carbon nanotube production apparatus according to any one of claims 1 to 4, wherein a flowing carrier gas is provided in the product discharge line.

7. A method for preparing carbon nanotubes using the apparatus of any one of claims 1 to 6, 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.

8. The process of claim 7, wherein 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;

preferably, before the catalyst is added, carrier gas is adopted for purging, and air is discharged;

preferably, the organic carbon source gas comprises any one or a combination of at least two of propylene, methane, propane or acetylene;

preferably, the carrier comprises any one of nitrogen, helium, neon or argon or a combination of at least two of the same;

preferably, the volume ratio of the organic carbon source gas to the carrier gas is (0.6-3): 1.

9. The method according to claim 7 or 8, wherein the temperature of the reaction is 600 to 1000 ℃;

preferably, the reaction time is 60-90 min.

10. The method according to any one of claims 7 to 9, wherein the reacted gas undergoes gas-solid separation and then exchanges heat with the organic carbon source gas in the gas inlet pipeline;

preferably, during the negative-pressure discharging, the pressure of carrier gas in the product discharging pipeline is 0.1-0.8 MPa, and the flow of product materials is 20-180L/min;

preferably, when the fluidized reactor is stopped and cleaned, the gas circulates in the exhaust pipeline and the fluidized reactor, and the gas after passing through the fluidized reactor is cooled by the cooler in a circulating manner.

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