CN117509699A - System and method for preparing aluminum fluoride from aluminum oxide - Google Patents
System and method for preparing aluminum fluoride from aluminum oxide Download PDFInfo
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- CN117509699A CN117509699A CN202311659600.4A CN202311659600A CN117509699A CN 117509699 A CN117509699 A CN 117509699A CN 202311659600 A CN202311659600 A CN 202311659600A CN 117509699 A CN117509699 A CN 117509699A
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- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 title claims abstract description 32
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 20
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims abstract description 88
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 49
- 239000012071 phase Substances 0.000 claims abstract description 29
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000007790 solid phase Substances 0.000 claims abstract description 8
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 56
- 239000007789 gas Substances 0.000 claims description 51
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims description 46
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 29
- 239000003546 flue gas Substances 0.000 claims description 29
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 19
- 239000000428 dust Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 10
- 239000007791 liquid phase Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 15
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 7
- 239000006227 byproduct Substances 0.000 abstract description 4
- 230000006911 nucleation Effects 0.000 abstract description 3
- 238000010899 nucleation Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000012320 chlorinating reagent Substances 0.000 abstract description 2
- 238000005243 fluidization Methods 0.000 abstract description 2
- 238000005453 pelletization Methods 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012025 fluorinating agent Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009856 non-ferrous metallurgy Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/50—Fluorides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention discloses a system and a method for preparing aluminum fluoride from aluminum oxide. The invention uses silicon chloride as chlorinating agent of aluminum oxide chlorination reaction, does not need carbon matching and pelletizing, has simple operation, and is easy to separate and purify the product. The fluidized bed is adopted as a chlorination reactor, so that the mass transfer and heat transfer rate between the gas phase and the solid phase is high, and the reaction efficiency is high. The arrangement of the inner member in the chlorination reactor can obviously improve the fluidization quality and improve the gas-solid contact efficiency. Seed powder is added into the fluorination reactor, nucleation sites and matrixes can be provided, and the product is convenient to collect. The silicon chloride as a byproduct of the fluorination reaction can be recycled for the chlorination reaction, so that the recycling rate of the system is high, the production cost is effectively reduced, and good economic and social benefits are achieved.
Description
Technical Field
The invention belongs to the field of nonferrous metallurgy and environmental protection, and particularly relates to a system and a method for aluminum fluoride by using aluminum oxide.
Background
Aluminum fluoride is a main auxiliary material in the production process of electrolytic aluminum, is mainly used as an adjusting additive and a fluxing agent of electrolyte, and can be used as an adjusting additive to improve the conductivity of the electrolyte by adjusting the molecular ratio of the electrolyte; as fluxing agent, the melting point of alumina can be reduced, the heat balance in the electrolysis process can be controlled, and the electricity consumption can be reduced. In addition, aluminum fluoride can also be used as an organic synthesis catalyst, a refractive index improver for lenses or prisms, and the like.
Chinese patent application CN1830794a discloses a method for producing aluminum fluoride, which comprises pulverizing kaolinite powder to 100-200 mesh, placing into a pressurized reaction kettle together with 200-300g/l sulfuric acid solution, reacting at 130-150 ℃ for 1-2 hours to obtain aluminum sulfate solution, reacting with hydrofluoric acid, crystallizing at 130-160 ℃, washing, drying, and dewatering to obtain aluminum fluoride product. Although the method can obtain aluminum fluoride products with good physical properties, concentrated sulfuric acid is required to react under heating and pressurizing, equipment investment is large, operation conditions are severe, and large-scale continuous production is difficult. Chinese patent application CN101077788A discloses a method for producing aluminum fluoride, which comprises mixing ammonium fluoroaluminate and aluminum hydroxide in a certain proportion, and reacting at 500-600 ℃ to obtain aluminum fluoride, and by-product ammonia gas and water vapor. The method has simple principle, can prepare aluminum fluoride through one-step solid-solid reaction, but produces ammonia gas in the process, has larger pollution, and simultaneously has the problems of slower solid-solid reaction rate, easy decomposition of ammonium fluoroaluminate, difficult separation and purification of products and the like, and is difficult to realize industrial production. Chinese patent application CN101077789a discloses a method for producing aluminum fluoride, which comprises gasifying ammonium fluoride or ammonium bifluoride at 200-300 ℃ and then feeding the gasified ammonium fluoride or ammonium bifluoride and aluminum hydroxide into a fluidized bed reactor according to a certain proportion to react at 500-600 ℃ to obtain aluminum fluoride products and byproducts of ammonia gas and water vapor. The method has simple principle, can prepare aluminum fluoride through one-step gas-solid reaction, but also has the problems of ammonia pollution, difficult separation and purification of products, equipment corrosion and the like, and is difficult to produce in large scale.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a system and a method for preparing aluminum fluoride from aluminum oxide, which are simple and convenient to operate, simple in equipment, high in efficiency, convenient and easy to regulate and control, and can realize large-scale continuous production.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a system for preparing aluminum fluoride from aluminum oxide comprises an aluminum oxide bin, an aluminum oxide feeder, a chlorination fluidized bed, a primary cyclone I, a secondary cyclone I, a feed back valve I, a tailings bin, a heat exchanger I, a gas heater I, a draught fan I, a condenser I, a gasifier I, a fluorination fluidized bed, a primary cyclone II, a secondary cyclone II, a feed back valve II, a product bin, a heat exchanger II, a gas heater II, a draught fan II, a condenser II and a gasifier II;
the alumina bin, the alumina feeder and the chlorination fluidized bed are sequentially connected along the material flow direction; the air inlet, the air outlet and the discharge port of the chlorination fluidized bed are respectively connected with the air outlet of the gas heater I, the air inlet of the primary cyclone separator I and the feed inlet of the tailings bin; the discharge port of the primary cyclone separator I is connected with the feed port of the feed back valve I; the air inlet, the air outlet and the discharge port of the secondary cyclone separator I are respectively connected with the air outlet of the primary cyclone separator I, the hot gas inlet of the heat exchanger I and the feed inlet of the feed back valve I; the discharge port of the feed back valve I is connected with the upper feed back port of the chlorination fluidized bed, the air inlet of the feed back valve I is connected with the air outlet of the gas heater I, the air inlet of the gas heater I is connected with the hot air outlet of the heat exchanger I, and the cold air outlet of the heat exchanger I is connected with the air inlet of the induced draft fan I; the air outlet of the induced draft fan I is connected with the air inlet of the condenser I, the air outlet of the condenser I and the air outlet of the gasifier II are both connected with the cold air inlet of the heat exchanger I, the dust outlet of the condenser I is connected with the feed inlet of the gasifier I, and the air outlet of the gasifier I is connected with the feed inlet of the fluorinated fluidized bed;
the air inlet, the air outlet and the discharge port of the fluorinated fluidized bed are respectively connected with the air outlet of the gas heater II, the air inlet of the primary cyclone separator II and the feed inlet of the product bin; the discharge port of the primary cyclone separator II is connected with the feed port of the feed back valve II; the air inlet, the air outlet and the discharge port of the secondary cyclone separator II are respectively connected with the air outlet of the primary cyclone separator II, the hot gas inlet of the heat exchanger II and the feed inlet of the feed back valve II; the discharge port of the return valve II is connected with the upper return port of the fluorinated fluidized bed, the air inlet of the return valve II is connected with the air outlet of the gas heater II, the air inlet of the gas heater II is connected with the hot air outlet of the heat exchanger II, the cold air outlet of the heat exchanger II is connected with the air inlet of the induced draft fan II, the air outlet of the induced draft fan II is connected with the air inlet of the condenser II, the air outlet of the condenser II is connected with the cold air inlet of the heat exchanger II, and the liquid outlet of the condenser II is connected with the feed port of the gasifier II;
the room temperature silicon chloride pipeline is connected with the feed inlet of the gasifier II, and the room temperature silicon fluoride pipeline is connected with the cool air inlet of the heat exchanger II.
Further, an inner member is arranged in the chlorination fluidized bed, and the inner member is of a porous plate type structure, a paddle type structure or a hole paddle type structure.
Further, seed powder is arranged in the fluorination fluidized bed, and the seed powder is aluminum fluoride, and the particle size is 0.1-0.5mm.
The invention also provides a working method of the system for preparing aluminum fluoride from the aluminum oxide, which comprises the following specific processes:
the alumina fine powder is stored in an alumina bin and enters a chlorination fluidized bed through an alumina feeder;
the room temperature silicon chloride enters a gasifier II from a room temperature silicon chloride pipeline, is gasified into gas phase silicon chloride by the gasifier II, then enters a gas heater I by a heat exchanger I to be heated into high temperature silicon chloride, and the high temperature silicon chloride enters a chlorination fluidized bed;
in a chlorination fluidized bed, carrying out chlorination reaction on alumina fine powder and high-temperature silicon chloride to obtain mixed flue gas of aluminum chloride and silicon chloride and chlorination slag, enabling the chlorination slag to enter a tailing bin, and enabling the mixed flue gas of aluminum chloride and silicon chloride to enter a heat exchanger I after being subjected to dust collection through a primary cyclone separator I and a secondary cyclone separator I in sequence under the action of a draught fan I, and cooling through heat exchange; the dust recovered by the first cyclone separator I and the second cyclone separator I is fluidized under the action of high-temperature silicon chloride in a feed back valve I and returns to a chlorination fluidized bed, mixed flue gas of the dedusted aluminum chloride and the silicon chloride is subjected to heat exchange and cooling and then enters a condenser I to be condensed to obtain solid-phase aluminum chloride and gas-phase silicon chloride, the gas-phase silicon chloride is sent into a heat exchanger I and is heated to be hot silicon chloride through heat exchange with the mixed flue gas of the dedusted aluminum chloride and the silicon chloride, then enters a gas heater I to be further heated to be high-temperature silicon chloride, and the solid-phase aluminum chloride is gasified by a gasifier I to obtain gas-phase aluminum chloride and enters a fluorination fluidized bed;
the room temperature silicon fluoride enters a gas heater II from a room temperature silicon fluoride pipeline through a heat exchanger II to be heated into high temperature silicon fluoride; in a fluorinated fluidized bed, carrying out fluorination reaction on gas-phase aluminum chloride and high-temperature silicon fluoride to obtain mixed flue gas of silicon fluoride and silicon chloride and aluminum fluoride, enabling the mixed flue gas of silicon fluoride and silicon chloride to enter a product bin, sequentially collecting dust by a primary cyclone separator II and a secondary cyclone separator II under the action of a draught fan II, enabling the mixed flue gas to enter a heat exchanger II, carrying out heat exchange and cooling, enabling dust recovered by the primary cyclone separator II and the secondary cyclone separator II to be fluidized in a feed back valve II under the action of the high-temperature silicon fluoride, and enabling the mixed flue gas of the dedusted silicon fluoride and silicon chloride to enter a condenser II for condensation after heat exchange and cooling to obtain gas-phase silicon fluoride and liquid-phase silicon chloride; the liquid-phase silicon chloride is sent into a gasifier II to be gasified into gas-phase silicon chloride, the gas-phase silicon chloride enters a heat exchanger I to be heated into hot silicon chloride through heat exchange with mixed flue gas of aluminum chloride and silicon chloride after dust removal, and the hot silicon chloride enters a gas heater I to be further heated into high-temperature silicon chloride; the gas phase silicon fluoride enters a heat exchanger II, and the mixed flue gas of the dedusted silicon fluoride and the dedusted silicon chloride is heated to be hot silicon fluoride through heat exchange, and the hot silicon fluoride enters a gas heater II to be further heated to be high-temperature silicon fluoride.
Further, the alumina fine powder has a particle size of less than 1 μm.
Further, the temperature of the chlorination reaction is 700-900 ℃ and the time is 0.5-1h.
Further, the temperature of the fluorination reaction is 500-700 ℃ and the time is 0.5-1h.
Further, the condensation temperature in the condenser I is 70-170 ℃, and the condensation temperature in the condenser II is 20-50 ℃.
The invention has the beneficial effects that:
1. the invention adopts silicon chloride as chlorinating agent of aluminum oxide chlorination reaction, does not need carbon matching and pelletizing, has simple operation and simple flow, and is easy to separate and purify the product.
2. According to the invention, the silicon fluoride is used as a fluorinating agent to react with the gas-phase aluminum chloride to prepare aluminum fluoride, the gas-gas reaction is efficient and rapid, the silicon chloride as a byproduct of the fluorination reaction can be recycled for the chlorination reaction, the recycling rate of the system is high, and the production cost is effectively reduced.
3. The invention adopts the gas-solid fluidized bed as the chlorination reactor, has good mixing contact between gas and solid phases, fast mass and heat transfer rate and high reaction efficiency, and is convenient for continuous operation and large-scale treatment.
4. The inner member arranged in the chlorination reactor can break bubbles and prevent fine particles from agglomerating, so that the fluidization quality is obviously improved, and the gas-solid contact efficiency is improved; seed powder is added into the fluorination reactor, nucleation sites and matrixes can be provided for the fluorination reaction, the fluorination reaction is promoted, and the product obtained by the reaction is convenient to collect.
In summary, the invention provides the system and the method for preparing the aluminum fluoride from the aluminum oxide, which are simple and convenient to operate, simple in equipment, high-efficiency and convenient, and easy to regulate, and can realize large-scale continuous and high-efficiency production of the aluminum fluoride.
Drawings
Fig. 1 is a schematic diagram of a system structure in embodiment 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings, and it should be noted that, while the present embodiment provides a detailed implementation and a specific operation process on the premise of the present technical solution, the protection scope of the present invention is not limited to the present embodiment.
Example 1
The embodiment provides a system for preparing aluminum fluoride from aluminum oxide, which is shown in fig. 1 and comprises an aluminum oxide bin 1, an aluminum oxide feeder 2, a chlorination fluidized bed 3, an inner member 4, a primary cyclone separator I5, a secondary cyclone separator I6, a feed back valve I7, a tailings bin 8, a heat exchanger I9, a gas heater I10, a draught fan I11, a condenser I12, a gasifier I13, a fluorination fluidized bed 14, seed powder 15, a primary cyclone separator II 16, a secondary cyclone separator II 17, a feed back valve II 18, a product bin 19, a heat exchanger II 20, a gas heater II 21, a draught fan II 22, a condenser II 23 and a gasifier II 24;
the aluminum oxide bin 1, the aluminum oxide feeder 2 and the chlorination fluidized bed 3 are sequentially connected along the material flow direction; the air inlet, the air outlet and the discharge port of the chlorination fluidized bed 3 are respectively connected with the air outlet of the gas heater I10, the air inlet of the primary cyclone separator I5 and the feed inlet of the tailings bin 8; the discharge port of the primary cyclone separator I5 is connected with the feed port of the feed back valve I7; the air inlet, the air outlet and the discharge outlet of the secondary cyclone separator I6 are respectively connected with the air outlet of the primary cyclone separator I5, the hot air inlet of the heat exchanger I9 and the feed inlet of the feed back valve I7; the discharge port of the feed back valve I7 is connected with the upper feed back port of the chlorination fluidized bed 3, the air inlet of the feed back valve I7 is connected with the air outlet of the gas heater I10, the air inlet of the gas heater I10 is connected with the hot air outlet of the heat exchanger I9, and the cold air outlet of the heat exchanger I9 is connected with the air inlet of the induced draft fan I11; the air outlet of the induced draft fan I11 is connected with the air inlet of the condenser I12, the air outlet of the condenser I12 and the air outlet of the gasifier II 24 are both connected with the cold air inlet of the heat exchanger I9, the dust outlet of the condenser I12 is connected with the feed inlet of the gasifier I13, and the air outlet of the gasifier I13 is connected with the feed inlet of the fluorinated fluidized bed 14;
the air inlet, the air outlet and the discharge port of the fluorinated fluidized bed 14 are respectively connected with the air outlet of the gas heater II 21, the air inlet of the primary cyclone separator II 16 and the feed inlet of the product bin 19; the discharge port of the primary cyclone separator II 16 is connected with the feed port of the feed back valve II 18; the air inlet, the air outlet and the discharge outlet of the secondary cyclone separator II 17 are respectively connected with the air outlet of the primary cyclone separator II 16, the hot air inlet of the heat exchanger II 20 and the feed inlet of the feed back valve II 18; the discharge port of the return valve II 18 is connected with the upper return port of the fluorinated fluidized bed 14, the air inlet of the return valve II 18 is connected with the air outlet of the gas heater II 21, the air inlet of the gas heater II 21 is connected with the hot air outlet of the heat exchanger II 20, the cold air outlet of the heat exchanger II 20 is connected with the air inlet of the induced draft fan II 22, the air outlet of the induced draft fan II 22 is connected with the air inlet of the condenser II 23, the air outlet of the condenser II 23 is connected with the cold air inlet of the heat exchanger II 20, and the liquid outlet of the condenser II 23 is connected with the feed port of the gasifier II 24;
the room temperature silicon chloride pipeline is connected with the feed inlet of the gasifier II 24, and the room temperature silicon fluoride pipeline is connected with the cold air inlet of the heat exchanger II 20.
In this embodiment, the chlorination fluidized bed 3 is provided with an inner member 4, and the inner member 4 is in a porous plate structure, a paddle structure or a hole paddle structure, and is used for breaking agglomerates, eliminating bubbles and strengthening gas-solid contact.
In this embodiment, the fluorinated fluidized bed 14 is provided with seed powder 15, where the seed powder 15 is aluminum fluoride, and the particle size is 0.1-0.5mm, and is used to provide nucleation sites and a matrix for the fluorination reaction.
Example 2
The embodiment provides a working method of the system for preparing aluminum fluoride from aluminum oxide in embodiment 1, which comprises the following specific steps:
the alumina fine powder is stored in an alumina bin 1 and enters a chlorination fluidized bed 3 through an alumina feeder 2;
the room temperature silicon chloride enters a gasifier II 24 from a room temperature silicon chloride pipeline, is gasified into gas phase silicon chloride by the gasifier II 24, then enters a gas heater I10 by a heat exchanger I9 to be heated into high temperature silicon chloride, and the high temperature silicon chloride enters a chlorination fluidized bed 3;
in the chlorination fluidized bed 3, aluminum oxide fine powder and high-temperature silicon chloride are subjected to chlorination reaction with the assistance of an inner component to obtain mixed flue gas of aluminum chloride and silicon chloride and chlorination slag, the chlorination slag enters a tailings bin 8, and the mixed flue gas of aluminum chloride and silicon chloride enters a heat exchanger I9 after being subjected to dust collection by a primary cyclone separator I5 and a secondary cyclone separator I6 in sequence under the action of a draught fan I11 and is subjected to heat exchange and cooling; the dust recovered by the first cyclone separator I5 and the second cyclone separator I6 is fluidized under the action of high-temperature silicon chloride in a feed back valve I7 and returns to the chlorination fluidized bed 3, the mixed flue gas of the dedusted aluminum chloride and the silicon chloride is cooled by heat exchange and then enters a condenser I12 to be condensed to obtain solid-phase aluminum chloride and gas-phase silicon chloride, the gas-phase silicon chloride is sent into a heat exchanger I9 to be heated into hot silicon chloride by heat exchange with the mixed flue gas of the dedusted aluminum chloride and the silicon chloride, then enters a gas heater I10 to be further heated into high-temperature silicon chloride, and the solid-phase aluminum chloride is gasified by a gasifier I13 to obtain gas-phase aluminum chloride and enters a fluorinated fluidized bed 14;
the room temperature silicon fluoride is heated into high temperature silicon fluoride from a room temperature silicon fluoride pipeline through a heat exchanger II 20 and a gas heater II 21; in the fluorination fluidized bed 14, gas-phase aluminum chloride and high-temperature silicon fluoride are subjected to fluorination reaction under the action of seed powder to obtain mixed flue gas of silicon fluoride and silicon chloride and aluminum fluoride, the aluminum fluoride enters a product bin 19, the mixed flue gas of the silicon fluoride and the silicon chloride is sequentially subjected to dust collection by a primary cyclone II 16 and a secondary cyclone II 17 under the action of a draught fan II 22 and then enters a heat exchanger II 20 to be subjected to heat exchange and cooling, dust recovered by the primary cyclone II 16 and the secondary cyclone II 17 is fluidized in a feed back valve II 18 under the action of the high-temperature silicon fluoride and returns to the fluorination fluidized bed 14, and the mixed flue gas of the dedusted silicon fluoride and the silicon chloride enters a condenser II 23 to be condensed to obtain gas-phase silicon fluoride and liquid-phase silicon chloride; the liquid-phase silicon chloride is sent into a gasifier II 24 to be gasified into gas-phase silicon chloride, the gas-phase silicon chloride enters a heat exchanger I9 to be heated into hot silicon chloride through heat exchange with mixed flue gas of aluminum chloride and silicon chloride after dust removal, and the hot silicon chloride enters a gas heater I10 to be further heated into high-temperature silicon chloride; the gas phase silicon fluoride enters a heat exchanger II 20, and the mixed flue gas of the dedusted silicon fluoride and silicon chloride is heated to be hot silicon fluoride through heat exchange, and the hot silicon fluoride enters a gas heater II 21 to be further heated to be high-temperature silicon fluoride.
In this embodiment, the alumina fine powder has a particle size of less than 1 μm.
In this example, the temperature of the chlorination reaction was 700℃for 1 hour.
In this example, the temperature of the fluorination reaction was 500℃and the time was 1h.
In this example, the condensing temperature in the condenser I was 70 ℃ and the condensing temperature in the condenser II was 20 ℃.
Example 3
This embodiment is substantially the same as embodiment 2, except that the description is not repeated, except that: in this example, the temperature of the chlorination reaction was 900 ℃ for 0.5h; the temperature of the fluorination reaction is 700 ℃ and the time is 0.5h; the condensing temperature in the condenser I is 170 ℃, and the condensing temperature in the condenser II is 50 ℃.
Example 4
This embodiment is substantially the same as embodiment 2, except that the description is not repeated, except that: in this example, the temperature of the chlorination reaction was 800℃for 0.7h; the temperature of the fluorination reaction is 600 ℃ and the time is 0.7h; the condensing temperature in the condenser I is 120 ℃, and the condensing temperature in the condenser II is 30 ℃.
Various modifications and variations of the present invention will be apparent to those skilled in the art in light of the foregoing teachings and are intended to be included within the scope of the following claims.
Claims (8)
1. The system for preparing aluminum fluoride from aluminum oxide is characterized by comprising an aluminum oxide bin, an aluminum oxide feeder, a chlorination fluidized bed, a primary cyclone I, a secondary cyclone I, a feed back valve I, a tailing bin, a heat exchanger I, a gas heater I, a draught fan I, a condenser I, a gasifier I, a fluorination fluidized bed, a primary cyclone II, a secondary cyclone II, a feed back valve II, a product bin, a heat exchanger II, a gas heater II, a draught fan II, a condenser II and a gasifier II;
the alumina bin, the alumina feeder and the chlorination fluidized bed are sequentially connected along the material flow direction; the air inlet, the air outlet and the discharge port of the chlorination fluidized bed are respectively connected with the air outlet of the gas heater I, the air inlet of the primary cyclone separator I and the feed inlet of the tailings bin; the discharge port of the primary cyclone separator I is connected with the feed port of the feed back valve I; the air inlet, the air outlet and the discharge port of the secondary cyclone separator I are respectively connected with the air outlet of the primary cyclone separator I, the hot gas inlet of the heat exchanger I and the feed inlet of the feed back valve I; the discharge port of the feed back valve I is connected with the upper feed back port of the chlorination fluidized bed, the air inlet of the feed back valve I is connected with the air outlet of the gas heater I, the air inlet of the gas heater I is connected with the hot air outlet of the heat exchanger I, and the cold air outlet of the heat exchanger I is connected with the air inlet of the induced draft fan I; the air outlet of the induced draft fan I is connected with the air inlet of the condenser I, the air outlet of the condenser I and the air outlet of the gasifier II are both connected with the cold air inlet of the heat exchanger I, the dust outlet of the condenser I is connected with the feed inlet of the gasifier I, and the air outlet of the gasifier I is connected with the feed inlet of the fluorinated fluidized bed;
the air inlet, the air outlet and the discharge port of the fluorinated fluidized bed are respectively connected with the air outlet of the gas heater II, the air inlet of the primary cyclone separator II and the feed inlet of the product bin; the discharge port of the primary cyclone separator II is connected with the feed port of the feed back valve II; the air inlet, the air outlet and the discharge port of the secondary cyclone separator II are respectively connected with the air outlet of the primary cyclone separator II, the hot gas inlet of the heat exchanger II and the feed inlet of the feed back valve II; the discharge port of the return valve II is connected with the upper return port of the fluorinated fluidized bed, the air inlet of the return valve II is connected with the air outlet of the gas heater II, the air inlet of the gas heater II is connected with the hot air outlet of the heat exchanger II, the cold air outlet of the heat exchanger II is connected with the air inlet of the induced draft fan II, the air outlet of the induced draft fan II is connected with the air inlet of the condenser II, the air outlet of the condenser II is connected with the cold air inlet of the heat exchanger II, and the liquid outlet of the condenser II is connected with the feed port of the gasifier II;
the room temperature silicon chloride pipeline is connected with the feed inlet of the gasifier II, and the room temperature silicon fluoride pipeline is connected with the cool air inlet of the heat exchanger II.
2. The system of claim 1, wherein an inner member is disposed in the chlorination fluidized bed, the inner member being in a porous plate structure, a paddle structure, or a hole-paddle structure.
3. The system of claim 1, wherein the fluorinated fluidized bed has seed powder disposed therein, the seed powder being aluminum fluoride having a particle size of 0.1-0.5mm.
4. A method of operating a system for preparing aluminum fluoride from aluminum oxide as claimed in any one of claims 1 to 3, comprising the steps of:
the alumina fine powder is stored in an alumina bin and enters a chlorination fluidized bed through an alumina feeder;
the room temperature silicon chloride enters a gasifier II from a room temperature silicon chloride pipeline, is gasified into gas phase silicon chloride by the gasifier II, then enters a gas heater I by a heat exchanger I to be heated into high temperature silicon chloride, and the high temperature silicon chloride enters a chlorination fluidized bed;
in a chlorination fluidized bed, carrying out chlorination reaction on alumina fine powder and high-temperature silicon chloride to obtain mixed flue gas of aluminum chloride and silicon chloride and chlorination slag, enabling the chlorination slag to enter a tailing bin, and enabling the mixed flue gas of aluminum chloride and silicon chloride to enter a heat exchanger I after being subjected to dust collection through a primary cyclone separator I and a secondary cyclone separator I in sequence under the action of a draught fan I, and cooling through heat exchange; the dust recovered by the first cyclone separator I and the second cyclone separator I is fluidized under the action of high-temperature silicon chloride in a feed back valve I and returns to a chlorination fluidized bed, mixed flue gas of the dedusted aluminum chloride and the silicon chloride is subjected to heat exchange and cooling and then enters a condenser I to be condensed to obtain solid-phase aluminum chloride and gas-phase silicon chloride, the gas-phase silicon chloride is sent into a heat exchanger I and is heated to be hot silicon chloride through heat exchange with the mixed flue gas of the dedusted aluminum chloride and the silicon chloride, then enters a gas heater I to be further heated to be high-temperature silicon chloride, and the solid-phase aluminum chloride is gasified by a gasifier I to obtain gas-phase aluminum chloride and enters a fluorination fluidized bed;
the room temperature silicon fluoride enters a gas heater II from a room temperature silicon fluoride pipeline through a heat exchanger II to be heated into high temperature silicon fluoride; in a fluorinated fluidized bed, carrying out fluorination reaction on gas-phase aluminum chloride and high-temperature silicon fluoride to obtain mixed flue gas of silicon fluoride and silicon chloride and aluminum fluoride, enabling the mixed flue gas of silicon fluoride and silicon chloride to enter a product bin, sequentially collecting dust by a primary cyclone separator II and a secondary cyclone separator II under the action of a draught fan II, enabling the mixed flue gas to enter a heat exchanger II, carrying out heat exchange and cooling, enabling dust recovered by the primary cyclone separator II and the secondary cyclone separator II to be fluidized in a feed back valve II under the action of the high-temperature silicon fluoride, and enabling the mixed flue gas of the dedusted silicon fluoride and silicon chloride to enter a condenser II for condensation after heat exchange and cooling to obtain gas-phase silicon fluoride and liquid-phase silicon chloride; the liquid-phase silicon chloride is sent into a gasifier II to be gasified into gas-phase silicon chloride, the gas-phase silicon chloride enters a heat exchanger I to be heated into hot silicon chloride through heat exchange with mixed flue gas of aluminum chloride and silicon chloride after dust removal, and the hot silicon chloride enters a gas heater I to be further heated into high-temperature silicon chloride; the gas phase silicon fluoride enters a heat exchanger II, and the mixed flue gas of the dedusted silicon fluoride and the dedusted silicon chloride is heated to be hot silicon fluoride through heat exchange, and the hot silicon fluoride enters a gas heater II to be further heated to be high-temperature silicon fluoride.
5. The method of claim 4, wherein the alumina fines have a particle size of less than 1 μm.
6. The process according to claim 4, wherein the chlorination reaction is carried out at a temperature of 700 to 900℃for a period of 0.5 to 1 hour.
7. The process of claim 4, wherein the fluorination reaction is carried out at a temperature of 500 to 700℃for a period of 0.5 to 1 hour.
8. The method according to claim 4, wherein the condensing temperature in the condenser I is 70-170 ℃ and the condensing temperature in the condenser II is 20-50 ℃.
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| CN202311659600.4A CN117509699A (en) | 2023-12-06 | 2023-12-06 | System and method for preparing aluminum fluoride from aluminum oxide |
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| CN202311659600.4A CN117509699A (en) | 2023-12-06 | 2023-12-06 | System and method for preparing aluminum fluoride from aluminum oxide |
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