CN116281899A - Low-cost large-scale preparation method and device for nano black phosphorus-based material - Google Patents
Low-cost large-scale preparation method and device for nano black phosphorus-based material Download PDFInfo
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- CN116281899A CN116281899A CN202310241420.8A CN202310241420A CN116281899A CN 116281899 A CN116281899 A CN 116281899A CN 202310241420 A CN202310241420 A CN 202310241420A CN 116281899 A CN116281899 A CN 116281899A
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- based material
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000007789 gas Substances 0.000 claims abstract description 24
- 238000003860 storage Methods 0.000 claims abstract description 19
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 13
- 230000007704 transition Effects 0.000 claims abstract description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 12
- 239000011574 phosphorus Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000012530 fluid Substances 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 239000002274 desiccant Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- OZRUMCFJDUAWLN-UHFFFAOYSA-N [I].[Sn].[P] Chemical compound [I].[Sn].[P] OZRUMCFJDUAWLN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910021389 graphene Inorganic materials 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000012974 tin catalyst Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000741 silica gel Substances 0.000 claims description 4
- 229910002027 silica gel Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052743 krypton Inorganic materials 0.000 claims description 2
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 229910052704 radon Inorganic materials 0.000 claims description 2
- SYUHGPGVQRZVTB-UHFFFAOYSA-N radon atom Chemical compound [Rn] SYUHGPGVQRZVTB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052724 xenon Inorganic materials 0.000 claims description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 238000005243 fluidization Methods 0.000 abstract description 9
- 230000033001 locomotion Effects 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 4
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 description 4
- 238000000498 ball milling Methods 0.000 description 2
- 238000005234 chemical deposition Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/02—Preparation of phosphorus
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a low-cost large-scale preparation method of a nano black phosphorus-based material, which comprises the steps of firstly placing a phosphorus source in a storage tank, then conveying the storage tank to a fixed bed reactor for catalytic reaction to generate transitional state molecules, finally conveying the transitional state molecules to a fluidized bed reactor, carrying out fluidization movement with a carbon material under inert gas flow, and obtaining the nano black phosphorus-based material at the lower end of the fluidized bed reactor. The method and the device of the invention generate transition state gas through catalytic reaction in the fixed bed reactor, and realize the uniform load of nano black phosphorus on carbon materials while reducing the size of black phosphorus through fluidization movement in the fluidized bed reactor. The device of the method has simple structure, is easy to operate, can continuously prepare the nano black phosphorus-based material with specific size, and is favorable for realizing low-cost and large-scale preparation of the nano black phosphorus-based material.
Description
Technical Field
The invention relates to a low-cost large-scale preparation method and device of a nano black phosphorus-based material, and belongs to the technical field of nano materials.
Background
The nano black phosphorus has good application prospect in the fields of energy storage, catalysis, field effect transistors and the like due to the characteristics of high theoretical specific capacity, high carrier mobility, adjustable direct band gap and the like. However, the problem of poor stability exists when the single nano black phosphorus is applied, and the nano black phosphorus and other materials are compounded, so that the stability of the nano black phosphorus is improved, and meanwhile, the nano black phosphorus and other materials can cooperatively exert more excellent performance. Currently, the preparation method of the nano black phosphorus-based material mainly comprises a ball milling method, a high-pressure method, a solvothermal method and a chemical vapor deposition method. Wherein, the conditions required by the high-pressure method are harsh; the energy consumption for ball milling preparation is high; the nanometer black phosphorus prepared by a solvothermal method has poor crystal form. In contrast, the chemical vapor deposition method has the characteristics of simple operation and good crystal form of the prepared nano black phosphorus, and is expected to realize the efficient preparation of the nano black phosphorus-based material.
However, the traditional chemical vapor deposition method realizes the synthesis of the nano black phosphorus-based material through the regulation and control of the temperature gradient. If a temperature gradient is adopted in the whole reaction area, the black phosphorus nucleation sites are easily concentrated, and the prepared black phosphorus has larger size and is difficult to reach the nano-scale. If no temperature gradient is adopted in the whole reaction area, the nucleation sites of the black phosphorus are relatively dispersed, so that the problem that the prepared black phosphorus is larger in size is solved, but the growth positions of the black phosphorus are random due to the consistent area concentration, and the problems of low composite efficiency and uneven composite are difficult to solve because the substrate materials are often stacked at a certain fixed position.
The fluidization technology can effectively solve the problems. Therefore, on the basis of a chemical vapor deposition method, the development of the low-cost large-scale preparation method and the device of the nano black phosphorus-based material based on the fluidization technology has important significance for promoting the application of the nano black phosphorus-based material in more fields.
Disclosure of Invention
The invention aims to provide a low-cost large-scale preparation method and device for a nano black phosphorus-based material, which are used for realizing continuous preparation of the nano black phosphorus-based material by controlling a carbon material and generating a fluidization state of the nano black phosphorus-based material under the action of air flow so as to obtain the nano black phosphorus-based material with high preparation efficiency and uniform composition.
The invention provides a preparation method for continuously preparing a nano black phosphorus-based material by a fluidized bed, which comprises the following specific steps:
(1) The phosphorus source is placed in the storage tank and is heated, and the phosphorus source is converted into P by heating 4 A molecule;
(2) P is transported by a transporting device 4 The molecules are conveyed into a fixed bed reactor and heated, P 4 Drying the molecules by a drying agent fixed bed in the reactor, wherein the dried P 4 Reacting the molecules with a phosphorus-iodine-tin catalyst fixed bed to generate transition state gas;
(3) And (3) delivering the transition state gas into a fluidized bed reactor, heating the fluidized bed reactor, and fluidizing with the carbon material under the inert gas flow, so that the uniform loading of the nano black phosphorus on the carbon material is realized while the size of the black phosphorus is reduced, and the nano black phosphorus-based material is generated.
The phosphorus source in the step (1) is elemental phosphorus or phosphide in any form;
the heating temperature of the storage tank in the step (1) is more than or equal to 40 ℃;
the heating temperature of the fixed bed reactor in the step (2) is more than or equal to 280 ℃;
the dryer in the step (2) comprises a water-absorbing resin dryer, a silica gel dryer, a calcium chloride dryer and other substances capable of removing moisture in the wet substances;
the heating temperature of the fluidized bed reactor in the step (3) is more than or equal to 400 ℃;
the inert gas flow in the step (3) is any one or mixture of a plurality of nitrogen, helium, neon, argon, krypton, xenon and radon in any proportion;
the carbon material in the step (3) comprises graphene, carbon nanotubes, porous carbon and the like.
The invention relates to a low-cost large-scale preparation method and a device for a nano black phosphorus-based material, which comprise a raw material storage tank, a fluid delivery pump, a fluid flowmeter, a valve switch, an inert gas inlet pipeline, a fixed bed reactor, a fluidized bed reactor, a feed inlet pipeline, a gas outlet pipeline and a sealing gate valve. The yellow phosphorus storage tank is communicated with the fluid delivery pump, the fixed bed reactor is connected with the fluid delivery pump, the front end and the tail end of the fixed bed reactor are provided with valve switches, the front end of the fixed bed reactor is provided with a fluid flowmeter, the top end of the fluidized bed reactor is provided with a gas outlet, the inclined upper side of the fluidized bed reactor is provided with a feed inlet, the bottom of the fluidized bed reactor is provided with a gas outlet, the bottom of the fluidized bed reactor is connected with a sealing gate valve, the inclined lower side of the fluidized bed reactor is provided with an inert gas inlet, and the inclined lower side of the fluidized bed reactor is provided with a pipeline connected with the fixed bed reactor.
Further, a drying agent fixed bed and a catalyst fixed bed are arranged in the fixed bed reactor;
further, a pressure controller is arranged at the tail end of the fixed bed reactor;
further, the feed inlet is inserted from the side surface of the top of the fluidized bed reactor;
further, the inert gas inlet is inserted from the bottom side of the fluidized bed reactor;
further, the joint of the fixed bed reactor and the fluidized bed reactor is a three-way regulating valve, wherein two ports are respectively connected with the fixed bed reactor and the fluidized bed reactor, and the other port is an inert gas inlet;
further, a heating device is arranged inside or outside the whole reaction device.
The method and the device of the invention generate catalytic reaction in a fixed bed reactor to generate transition state gas, generate nano black phosphorus through fluidization movement in a fluidized bed reactor, and deposit on a carbon material to generate nano black phosphorus-based material. The device of the method has simple structure, is easy to operate, can continuously prepare the nano black phosphorus-based material with specific size, and is favorable for realizing low-cost and large-scale preparation of the nano black phosphorus-based material. The device of the invention has the following obvious characteristics:
1. the device can be used for preparing the nano black phosphorus-based material in one step.
2. The device has universality and is suitable for preparing the nano composite material by most chemical deposition methods.
3. Can continuously feed, discharge and replace the catalyst, thereby realizing the continuous preparation of the nano black phosphorus-based material.
4. The controllable preparation of the nano black phosphorus-based material can be realized by regulating and controlling the fluidized motion state and the transition state molecular concentration in the fluidized bed.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained from them without inventive faculty for a person skilled in the art.
FIG. 1 is a schematic structural view of a reaction apparatus according to the present invention.
In fig. 1, 1 is a raw material storage tank, 2 is a fluid transfer pump, 3 is a valve switch, 4 is a fluid flow meter, 5 is an inert gas inlet, 6 is a desiccant fixed bed, 7 is a catalyst fixed bed, 8 is a fixed bed reactor, 9 is a feed inlet, 10 is a gas outlet, 11 is a fluidized bed reactor, and 12 is a seal gate valve.
As shown in FIG. 1, the reaction device for continuously preparing nano black phosphorus based by the fluidized bed comprises a raw material storage tank 1, a fluid delivery pump 2, a valve switch 3, a fluid flowmeter 4, an inert gas inlet 5, a fixed bed reactor 8, a fluidized bed reactor 11, a feed inlet 9, a gas outlet 10 and a sealing gate valve 12; the yellow phosphorus storage tank 1 is communicated with the fluid delivery pump 2, the fixed bed reactor 8 is connected with the fluid delivery pump 2, the front end and the tail end of the fixed bed reactor 8 are provided with valve switches 3, the front end of the fixed bed reactor is provided with a fluid flowmeter 4, the top end of the fluidized bed reactor 11 is provided with a gas outlet 10, the inclined upper part of the fluidized bed reactor 11 is provided with a feed inlet 9, the bottom of the fluidized bed reactor 11 is provided with a gas outlet 10, the bottom of the fluidized bed reactor 11 is connected with a sealing gate valve 12, the inclined lower part of the fluidized bed reactor 11 is provided with an inert gas inlet 5, the inclined lower part of the fluidized bed reactor 11 is provided with a pipeline connected with the fixed bed reactor 8, the fixed bed reactor 8 is internally provided with a drying agent fixed bed and a catalyst fixed bed, and the tail end of the fixed bed reactor 8 is provided with a pressure controller. According to different technological requirements, the device is suitable for preparing nano composite materials by most chemical deposition methods.
Detailed Description
The invention is described in further detail below by means of the figures and examples, but the scope of the invention is not limited to the description.
Example 1: a low-cost large-scale preparation method and device for nano black phosphorus-based materials comprises the following specific steps:
(1) Yellow phosphorus is placed in a storage tank, the storage tank is heated to 40 ℃, and the yellow phosphorus is converted into P by heating 4 A molecule;
(2) P is transported by a transporting device 4 The molecules are conveyed into a fixed bed reactor, the fixed bed reactor is heated to 520 ℃, and P 4 Drying the molecules by a water-absorbent resin drying agent fixed bed in the reactor, wherein the dried P 4 Reacting the molecules with a phosphorus-iodine-tin catalyst fixed bed to generate transition state gas;
(3) And (3) delivering the transition state gas into a fluidized bed reactor, heating the fluidized bed reactor to 480 ℃, and performing fluidization movement with the graphene under the argon gas flow, so that the uniform loading of the nano black phosphorus on the carbon material is realized while the size of the black phosphorus is reduced, and the nano black phosphorus-based material is generated.
Example 2: a low-cost large-scale preparation method and device for nano black phosphorus-based materials comprises the following specific steps:
(1) Red phosphorus is placed in a storage tank, the storage tank is heated to 500 ℃, and the red phosphorus is converted into P by heating 4 A molecule;
(2) P is transported by a transporting device 4 The molecules are transported into a fixed bed reactor, the fixed bed reactor is heated to 500 ℃, and P 4 Drying the molecules by a silica gel drying agent fixed bed in the reactor, wherein the dried molecules are P 4 Molecular and phosphorus-iodine-tin catalyst fixed bed reaction to generateA transition state gas;
(3) And (3) delivering the transition state gas into a fluidized bed reactor, heating the fluidized bed reactor to 490 ℃, and performing fluidization movement with the graphene under nitrogen gas flow, so that the uniform loading of the nano black phosphorus on the carbon material is realized while the size of the black phosphorus is reduced, and the nano black phosphorus-based material is generated.
Example 3: a low-cost large-scale preparation method and device for nano black phosphorus-based materials comprises the following specific steps:
(1) Red phosphorus is placed in a storage tank, the storage tank is heated to 500 ℃, and the red phosphorus is converted into P by heating 4 A molecule;
(2) P is transported by a transporting device 4 The molecules are transported into a fixed bed reactor, the fixed bed reactor is heated to 500 ℃, and P 4 Drying the molecules by a silica gel drying agent fixed bed in the reactor, wherein the dried molecules are P 4 Reacting the molecules with a phosphorus-iodine-tin catalyst fixed bed to generate transition state gas;
(3) And (3) delivering the transition state gas into a fluidized bed reactor, heating the fluidized bed reactor to 490 ℃, and performing fluidization movement with graphene under neon gas flow, so that the uniform loading of nano black phosphorus on the carbon material is realized while the size of the black phosphorus is reduced, and the nano black phosphorus-based material is generated.
Claims (9)
1. The low-cost large-scale preparation method of the nano black phosphorus-based material is characterized by comprising the following specific steps of:
(1) The phosphorus source is placed in the storage tank and is heated, and the phosphorus source is converted into P by heating 4 A molecule;
(2) P is transported by a transporting device 4 The molecules are conveyed into a fixed bed reactor and heated, P 4 Drying the molecules by a drying agent fixed bed in the reactor, wherein the dried P 4 Reacting the molecules with a phosphorus-iodine-tin catalyst fixed bed to generate transition state gas;
(3) And (3) delivering the transition state gas into a fluidized bed reactor, heating the fluidized bed reactor, and fluidizing with the carbon material under the inert gas flow, so that the uniform loading of the nano black phosphorus on the carbon material is realized while the size of the black phosphorus is reduced, and the nano black phosphorus-based material is generated.
2. The low-cost large-scale preparation method of the nano black phosphorus-based material according to claim 1, which is characterized by comprising the following steps: the phosphorus source in the step (1) is elemental phosphorus or phosphide in any form.
3. The low-cost large-scale preparation method of the nano black phosphorus-based material according to claim 1, which is characterized by comprising the following steps: the heating temperature of the storage tank in the step (1) is more than or equal to 40 ℃.
4. The low-cost large-scale preparation method of the nano black phosphorus-based material according to claim 1, which is characterized by comprising the following steps: the heating temperature of the fixed bed reactor in the step (2) is more than or equal to 280 ℃.
5. The low-cost large-scale preparation method of the nano black phosphorus-based material according to claim 1, which is characterized by comprising the following steps: the dryer in the step (2) comprises a water-absorbing resin dryer, a silica gel dryer, a calcium chloride dryer and the like which can remove moisture in the wet substance.
6. The low-cost large-scale preparation method of the nano black phosphorus-based material according to claim 1, which is characterized by comprising the following steps: in the step (3), the heating temperature of the fluidized bed reactor is more than or equal to 400 ℃.
7. The low-cost large-scale preparation method of the nano black phosphorus-based material according to claim 1, which is characterized by comprising the following steps: the inert gas flow in the step (3) is any one or more of nitrogen, helium, neon, argon, krypton, xenon and radon which are mixed in any proportion.
8. The low-cost large-scale preparation method of the nano black phosphorus-based material according to claim 1, which is characterized by comprising the following steps: the carbon material in the step (3) comprises graphene, carbon nanotubes, porous carbon and the like.
9. The low-cost large-scale preparation device of the nano black phosphorus-based material is characterized by comprising a raw material storage tank, a fluid delivery pump, a fluid flowmeter, a valve switch, an inert gas inlet pipeline, a fixed bed reactor, a fluidized bed reactor, a feed inlet pipeline, a gas outlet pipeline and a sealing gate valve; the raw material storage tank is communicated with the fluid delivery pump, the fixed bed reactor is connected with the fluid delivery pump, the front end and the tail end of the fixed bed reactor are provided with valve switches, the front end of the fixed bed reactor is provided with a fluid flowmeter, the tail end of the fixed bed reactor is provided with a pressure controller, the top end of the fluidized bed reactor is provided with a gas outlet, a feed inlet pipeline is arranged above the fluidized bed reactor in an inclined way, the bottom of the fluidized bed reactor is provided with a gas outlet, the bottom of the fluidized bed reactor is connected with a sealing gate valve, an inert gas inlet pipeline is arranged below the fluidized bed reactor in an inclined way, the pipeline is arranged below the fluidized bed reactor in an inclined way and is connected with the fixed bed reactor, and a heating device is arranged inside or outside the whole reaction device.
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