CN114480867B - Method for remelting, centrifugal and magnetic separation and grading purification of aluminum-silicon-iron alloy - Google Patents
Method for remelting, centrifugal and magnetic separation and grading purification of aluminum-silicon-iron alloy Download PDFInfo
- Publication number
- CN114480867B CN114480867B CN202011267938.1A CN202011267938A CN114480867B CN 114480867 B CN114480867 B CN 114480867B CN 202011267938 A CN202011267938 A CN 202011267938A CN 114480867 B CN114480867 B CN 114480867B
- Authority
- CN
- China
- Prior art keywords
- aluminum
- silicon
- iron alloy
- alloy
- iron
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- -1 aluminum-silicon-iron Chemical compound 0.000 title claims abstract description 85
- 229910000640 Fe alloy Inorganic materials 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 61
- 238000007885 magnetic separation Methods 0.000 title claims abstract description 13
- 238000000746 purification Methods 0.000 title claims abstract description 8
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910000676 Si alloy Inorganic materials 0.000 claims abstract description 40
- 238000001816 cooling Methods 0.000 claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 35
- 239000010703 silicon Substances 0.000 claims abstract description 34
- 239000012535 impurity Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000000155 melt Substances 0.000 claims abstract description 19
- 238000005266 casting Methods 0.000 claims abstract description 17
- 238000007670 refining Methods 0.000 claims abstract description 16
- 230000005291 magnetic effect Effects 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003723 Smelting Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 230000009471 action Effects 0.000 claims abstract description 8
- 239000002893 slag Substances 0.000 claims abstract description 8
- 230000005294 ferromagnetic effect Effects 0.000 claims abstract description 6
- 238000011068 loading method Methods 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 80
- 229910052742 iron Inorganic materials 0.000 claims description 34
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 23
- 238000000926 separation method Methods 0.000 claims description 16
- 239000013078 crystal Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 8
- 230000008018 melting Effects 0.000 claims description 8
- 229910001570 bauxite Inorganic materials 0.000 claims description 7
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 6
- 239000011707 mineral Substances 0.000 claims description 6
- 235000010755 mineral Nutrition 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229910000905 alloy phase Inorganic materials 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- 239000010881 fly ash Substances 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052622 kaolinite Inorganic materials 0.000 claims description 3
- 238000010310 metallurgical process Methods 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052656 albite Inorganic materials 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 239000010433 feldspar Substances 0.000 claims description 2
- 229940072033 potash Drugs 0.000 claims description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 2
- 235000015320 potassium carbonate Nutrition 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 abstract description 10
- 239000000956 alloy Substances 0.000 abstract description 10
- 239000007788 liquid Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 32
- 230000008569 process Effects 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000009467 reduction Effects 0.000 description 6
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000010587 phase diagram Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910018619 Si-Fe Inorganic materials 0.000 description 2
- 229910008289 Si—Fe Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910000765 intermetallic Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920005591 polysilicon Polymers 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 238000009628 steelmaking Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910018125 Al-Si Inorganic materials 0.000 description 1
- 229910018520 Al—Si Inorganic materials 0.000 description 1
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 1
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 description 1
- INJRKJPEYSAMPD-UHFFFAOYSA-N aluminum;silicic acid;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O INJRKJPEYSAMPD-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000010443 kyanite Substances 0.000 description 1
- 229910052850 kyanite Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 230000002277 temperature effect Effects 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
- B03C1/30—Combinations with other devices, not otherwise provided for
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
- C22B9/023—By filtering
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Acoustics & Sound (AREA)
- Manufacturing & Machinery (AREA)
- Silicon Compounds (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for remelting, centrifuging, magnetic separating and grading purifying aluminum-silicon-iron alloy, which comprises the following steps: (1) Putting the aluminum-silicon-iron alloy into an intermediate frequency furnace for high-temperature smelting to obtain an aluminum-silicon-iron alloy melt; (2) Casting the melt in a mould, and controlling the cooling speed and time to obtain a primary aluminum-silicon-iron alloy block; (3) Loading the alloy blocks into a heatable supergravity centrifugal device, heating at low temperature, and cooling and solidifying the molten liquid after passing through a porous filter plate under the action of supergravity to obtain aluminum-silicon alloy, wherein slag is a secondary aluminum-silicon-iron alloy block; (4) Crushing the alloy blocks, heating the crushed alloy blocks in a high-temperature furnace into which water vapor is introduced, cooling and solidifying the crushed alloy blocks, and separating the crushed alloy blocks by magnetic separation to obtain aluminum-silicon alloy containing oxide impurities and ferromagnetic substances; (5) And refining the aluminum-silicon alloy containing impurities to obtain the aluminum-silicon alloy or industrial silicon. The method has the advantages of simple and quick flow, low cost and no secondary pollution, realizes the hierarchical purification of the aluminum-silicon-iron alloy, obtains various high-grade products, and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of smelting, and particularly relates to a method for remelting, centrifuging, magnetic separating and grading purification of aluminum-silicon-iron alloy.
Background
With the progress of smelting technology and the development of the power industry, the aluminum industry is rapidly developed in China. The aluminum alloy at the present stage is obtained by fully adopting a pure aluminum and other metal blending method, and high-grade bauxite resources are required for producing the pure aluminum. At present, the shortage of bauxite resources in China can increase the production cost and directly influence the production. Therefore, the method actively exploits the non-traditional aluminum minerals to produce the aluminum-silicon-iron alloy, and has very important social and economic significance for promoting the sustainable development of the aluminum industry.
Currently, two main methods are commonly adopted for producing aluminum-silicon-iron alloy, namely a blending method and an electrothermal reduction method. The mixing method is to take aluminum ingots, industrial silicon or ferrosilicon as raw materials and prepare the material through proportional melting and mixing. However, the method has the advantages of long production flow, complex process, high production cost, high energy consumption and great influence on environment. The electrothermal reduction method is to prepare alloy by taking oxides containing aluminum, silicon and iron as raw materials, taking carbonaceous materials as reducing agents and carrying out reduction smelting by an electric arc furnace. The method not only can shorten the process flow and reduce the production cost, but also can utilize clay, kaolinite, kyanite, gangue, fly ash and other non-bauxite resources, and accords with the characteristics of aluminum ore resources in China. However, the Al-Si-Fe alloy prepared by the method has higher iron content, often exists in the form of brittle Fe-rich intermetallic compound, so that the Fe-Si-Fe alloy is mainly used as a steelmaking deoxidizer and is widely applied to steelworks. Because the steelmaking deoxidizer has limited dosage and lower price, the application market of the aluminum-silicon-iron alloy is restricted. If the aluminum-silicon-iron alloy can be subjected to iron reduction treatment, the aluminum-silicon-iron alloy can be used as the casting aluminum-silicon alloy which has higher value and meets the industrial requirements, and the aluminum-silicon-iron alloy has great significance in the market capacity of products and economic value.
In the prior art, patent CN107794390A discloses a method for removing iron from regenerated Al-Si aluminum alloy, wherein strontium added in the method is subjected to modification treatment, so that needle-shaped beta-iron phases are broken and decomposed, primary crystal silicon is refined, and the tissue distribution is more uniform; manganese plays a positive correlation role in generating Fe 2 B by reacting boron with iron, and meanwhile, manganese converts a beta-iron phase into an alpha-iron phase to play a role in precipitation; the high-melting-point high-density Fe 2 B compound generated by the reaction of boron and impurity iron has high density difference with the melt, and the iron-rich phases are settled to the bottom of the crucible under the action of gravity, so that impurity iron element in the aluminum alloy is removed. The patent CN108165810A discloses a device and a process for removing iron and silicon phases in primary aluminum-silicon alloy by a one-step method, which adopts metal element manganese as an iron remover under the action of an alternating electromagnetic field, uniformly mixes with primary aluminum-silicon alloy raw materials, heats and melts, solidifies and concentrates silicon and iron-rich phases in the alloy at the bottom under the combined action of magnetic field force and temperature effect after cooling, pours out upper molten liquid, obtains aluminum-silicon alloy for casting meeting industrial standards after cooling and solidification, and finally remelts primary silicon phase and impurity iron phase at the bottom to obtain bottom alloy molten liquid. The method for separating the iron phase by gravity sedimentation has the defects of low separation efficiency, complex process, high production cost and the like, and is difficult to apply in actual production. Accordingly, there is a need for a related method and technique for cost-effective and efficient separation.
The patent CN110904340A discloses a method for centrifugally removing harmful elements and impurities in an iron-containing mixture, which comprises the steps of placing an aluminum-silicon-iron high-temperature molten mixture into a centrifugal rotating device, controlling the cooling speed of the molten mixture to be 0.1-160 ℃/min, and controlling the centrifugal temperature to be 700-2600 ℃ to separate out and grow silicon crystals; then, centrifugally separating the molten mixture in a hypergravity field to obtain silicon, wherein the hypergravity coefficient is 10-4500 g, and when the hypergravity field is applied, the temperature in the device is not lower than the centrifugal temperature and gradually cooling to solidify; under the action of centrifugal overweight force, the molten mixture is subjected to sedimentation and enrichment of substances such as intermetallic compounds of iron and the like at the periphery of the hypergravity field, and low-density substances such as oxides and the like are subjected to floating and enrichment at the inner layer of the hypergravity field, so that the metal product can be purified and decontaminated. The method introduces the hypergravity centrifugation into the separation of different phases, and the separation efficiency is greatly improved compared with the prior natural gravity separation. However, this process has a fatal problem: centrifugal separation is carried out in a high-temperature liquid state, and the high-temperature molten aluminum alloy liquid has extremely strong corrosiveness to various metal materials, so that it is difficult to find a material with high strength at high temperature and high-temperature aluminum liquid corrosion resistance at low cost. Therefore, the process cannot be effectively and practically applied on a large scale.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for remelting, centrifuging, magnetically separating and classifying and purifying aluminum-silicon-iron alloy. The method can realize the high-efficiency separation of the iron-rich phase in the aluminum-silicon-iron alloy, obtain the aluminum-silicon alloy with higher added value and meeting the market requirements, and serve as industrial silicon for producing solar grade polysilicon after acid washing and impurity removal, so that the maximization of the resource utilization rate is realized, and the method has the characteristics of simple and quick flow, low cost and no secondary pollution, and is suitable for large-scale production.
The invention adopts the technical proposal for solving the technical problems that:
a remelting centrifugal magnetic separation grading purification method for aluminum-silicon-iron alloy comprises the following steps:
(1) Putting the aluminum-silicon-iron alloy into an intermediate frequency furnace for high-temperature smelting to obtain an aluminum-silicon-iron alloy melt;
(2) Casting the molten mass in a mould, controlling the cooling speed and time to separate out and grow alloy phase, and naturally cooling to room temperature to obtain a primary aluminum-silicon-iron alloy block;
(3) Loading the primary aluminum-silicon-iron alloy block into a hypergravity centrifugal device with a heating device, and heating at low temperature to enable aluminum silicon to be molten while primary crystal silicon and iron phases remain solid; starting a centrifugal machine, separating a melt through a porous filter plate under the action of supergravity, cooling and solidifying the melt to obtain aluminum-silicon alloy meeting the industrial standard for casting, wherein slag is a secondary aluminum-silicon-iron alloy block;
(4) Crushing the secondary aluminum-silicon-iron alloy blocks, heating the crushed secondary aluminum-silicon-iron alloy blocks in a high-temperature furnace into which water vapor is introduced, cooling and solidifying the secondary aluminum-silicon-iron alloy blocks, and separating the secondary aluminum-silicon-iron alloy blocks by magnetic separation to obtain aluminum-silicon alloy containing oxide impurities and ferromagnetic substances;
(5) And refining the aluminum-silicon alloy containing impurities to remove impurities to obtain aluminum-silicon alloy or industrial silicon, thereby realizing the graded purification of the aluminum-silicon-iron alloy.
In the method, the aluminum-silicon-iron alloy in the step (1) is prepared from aluminum-containing minerals through a metallurgical process, wherein the aluminum-containing minerals are aluminum-containing waste residues or low-grade aluminum ore resources, and the aluminum-containing waste residues mainly comprise aluminum oxide and silicon oxide and comprise one or more of bauxite magnetic separation tailings, coal gangue, fly ash, shale slag and the like; the low-grade aluminum ore resource refers to one or more of bauxite, kaolinite, albite, potash feldspar and the like with lower aluminum-silicon ratio.
In the method, the content range of the components of the aluminum-silicon-iron alloy in the step (1) is as follows: 10-90% of Al, 10-90% of Si and 0.7-10% of Fe.
In the method, the melting temperature in the intermediate frequency furnace in the step (1) is 1400-1600 ℃.
In the method, after the molten body is cast in the step (2), the temperature is reduced to 580-1050 ℃ at the speed of 1-20 ℃/min, and the temperature is kept for 30-120 min.
In the method, the primary aluminum-silicon-iron alloy block in the step (3) is heated to 580-650 ℃, then is insulated for 60-300 min, the supergravity coefficient is 200-500 g, and the separation time is 5-15 min.
In the method, in the step (3), the porous filter plate is an S310 high-temperature resistant stainless steel filter.
In the above method, the supergravity separation in step (3) is a continuous process or a batch process.
In the method, the steam inlet amount in the step (4) is 100-150 ml/min, the heating temperature is 800-950 ℃, the heating time is 30-120 min, and the magnetic field strength is 0.02-1.0T.
In the method, the refining temperature in the step (4) is 1200-1300 ℃, and the refining time is 25-30 min.
In the method, the aluminum-silicon alloy for casting meeting the industrial requirements can be produced in the steps (3) and (4), and the aluminum-silicon alloy can be used for producing industrial silicon for producing solar-grade polycrystalline silicon after pickling and impurity removal.
The present invention has been completed based on the following facts:
1. In the cooling crystallization process of the aluminum-silicon-iron melt, the segregation purification principle of the aluminum-silicon-iron melt is utilized to enable purer silicon crystals to be separated out and grow up firstly, a cooling curve is controlled to enable a silicon atom arrangement structure to form regular crystals on a solid-liquid interface, and a unique framework structure formed by the regular growth of the separated silicon crystal atom arrangement is utilized; with the further reduction of the temperature, the needle-like or flake iron phase starts to crystallize out and forms a framework structure together with the crystalline silicon; and continuously cooling, and solidifying the molten aluminum-silicon alloy to form solid blocks in framework gaps formed by the silicon phase and the iron phase.
2. When the primary aluminum-silicon-iron alloy block formed by cooling the aluminum-silicon-iron melt is reheated and melted, a specific low-temperature melting temperature can be selected according to the difference of melting temperatures of aluminum-silicon alloy, iron phase and primary silicon, so that the aluminum-silicon is melted while the primary silicon and the iron phase remain solid, and then the aluminum-silicon alloy block and the secondary aluminum-silicon-iron alloy block which accord with the industrial use standard can be separated under the action of a hypergravity field; the iron phase in the secondary aluminum-silicon-iron alloy block is gasified by water vapor to convert iron and aluminum into ferroferric oxide and aluminum oxide, then the magnetic ferroferric oxide is separated from nonmagnetic aluminum oxide and aluminum-silicon alloy by magnetic separation, and finally the nonmagnetic substance is refined to obtain the aluminum-silicon alloy for casting which meets the industrial use standard.
3. In the hypergravity centrifugation process, the skeleton structure formed by the flaky crystalline silicon and the needle-shaped or flaky iron phase is a good self-filtering device, so that the effective separation and filtration at a low temperature stage are realized.
The invention has the advantages that: the aluminum-silicon-iron alloy produced by using aluminum-containing minerals through a metallurgical process is used as a raw material, the limitation of the existing iron removal technology is overcome, a method which is efficient, environment-friendly and capable of continuous and large-scale production is provided, the efficient separation of iron-rich phases in the aluminum-silicon-iron alloy can be realized, the aluminum-silicon alloy with higher added value and meeting the market needs is obtained, and the aluminum-silicon alloy is used as industrial silicon for producing solar grade polysilicon after acid washing and impurity removal, so that the maximization of the resource utilization rate is realized, the national energy conservation and emission reduction requirements are met, and the economic benefit is remarkable.
Drawings
FIG. 1 is a phase diagram of an aluminum-silicon-iron ternary alloy of the present invention.
Fig. 2 is a process flow of the present invention.
Detailed Description
The following describes embodiments of the present invention in detail: the present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are provided, but the protection scope of the present invention is not limited to the following embodiments.
Example 1
A method for remelting, centrifugally separating and classifying and purifying an aluminum-silicon-iron alloy is shown in a process flow chart as shown in figure 2 and comprises the following steps:
100kg of aluminum-silicon-iron alloy is put into an intermediate frequency furnace for high-temperature smelting, and the melting temperature is 1400-1600 ℃, wherein the mass fraction of Al in the aluminum-silicon-iron alloy is 51.84%, the mass fraction of Si is 44.01% and the mass fraction of Fe is 2.70%, so as to obtain aluminum-silicon-iron alloy melt; casting the melt in a mould, cooling to 830 ℃ at 3 ℃/min, preserving heat for 60min at the temperature, and cooling to room temperature to obtain the primary aluminum-silicon-iron alloy block. As shown in figure 1, the alloy phase diagram of the invention shows that when the cooling temperature is reduced to 950-1000 ℃, silicon crystals are firstly precipitated and grown up, as the cooling temperature is reduced, the silicon content in the melt is gradually reduced, when the temperature is reduced to 750-800 ℃, needle-shaped or sheet-shaped iron phases start to crystallize out, the temperature is continuously reduced to below 577 ℃, and the molten aluminum-silicon alloy is solidified and exists in framework gaps formed by the silicon phases to form solid blocks.
100Kg of primary aluminum-silicon-iron alloy blocks are put into a hypergravity centrifugal device with a heating device, heated to 650 ℃, kept at the temperature for 180 minutes, melted aluminum-silicon and primary silicon and iron phases still kept solid, the centrifugal device is started, the hypergravity coefficient is 212g, the separation time is 10 minutes, under the hypergravity effect, the melt is separated through a porous filter plate, and the melt is cooled and solidified to obtain 54.21kg of aluminum-silicon alloy for casting meeting the industrial standard, wherein the mass fraction of Fe is 0.55%, the mass fraction of Si is 12.23%, and the slag is 45.79kg of secondary aluminum-silicon-iron alloy blocks.
Crushing 45.79kg of secondary aluminum-silicon-iron alloy blocks in a ball mill, heating in a high-temperature furnace into which water vapor is introduced, wherein the water vapor is introduced into the furnace for 100ml/min, the heating temperature is 850 ℃, the heat preservation time is 60min, cooling and solidifying, separating by magnetic separation under the magnetic field intensity of 0.25T, separating ferromagnetic substances from aluminum-silicon alloy containing oxide impurities, refining the impurity-containing aluminum-silicon alloy, and removing impurities, wherein the refining temperature is 1200-1300 ℃, the refining time is 25-30 min, and 41.89kg of aluminum-silicon alloy for casting meeting the industrial standard is obtained, wherein the mass fraction of Fe is 0.68%, and the mass fraction of Si is 89.23%.
Example 2
A method for remelting, centrifugally separating and classifying and purifying an aluminum-silicon-iron alloy is shown in a process flow chart as shown in figure 2 and comprises the following steps:
100kg of aluminum-silicon-iron alloy is put into an intermediate frequency furnace for high-temperature smelting, and the melting temperature is 1400-1600 ℃, wherein the mass fraction of Al in the aluminum-silicon-iron alloy is 51.84%, the mass fraction of Si is 44.01% and the mass fraction of Fe is 2.70%, so as to obtain aluminum-silicon-iron alloy melt; casting the melt in a mould, cooling to 700 ℃ at 2 ℃/min, preserving heat for 60min at the temperature, and cooling to room temperature to obtain the primary aluminum-silicon-iron alloy block. As shown in figure 1, the alloy phase diagram of the invention shows that when the cooling temperature is reduced to 950-1000 ℃, silicon crystals are firstly precipitated and grown up, as the cooling temperature is reduced, the silicon content in the melt is gradually reduced, when the temperature is reduced to 750-800 ℃, needle-shaped or sheet-shaped iron phases start to crystallize out, the temperature is continuously reduced to below 577 ℃, and the molten aluminum-silicon alloy is solidified and exists in framework gaps formed by the silicon phases to form solid blocks.
100Kg of primary aluminum-silicon-iron alloy blocks are put into a hypergravity centrifugal device with a heating device, heated to 650 ℃, kept at the temperature for 300min, melted to enable primary silicon and iron phases to remain solid, the centrifugal device is started, the hypergravity coefficient is 212g, the separation time is 10min, under the hypergravity effect, the melt is separated through a porous filter plate, 50.92kg of aluminum-silicon alloy for casting meeting the industrial standard is obtained after cooling and solidifying the melt, wherein the mass fraction of Fe is 0.41%, the mass fraction of Si is 11.75%, and the slag is 49.08kg of secondary aluminum-silicon-iron alloy blocks.
Crushing 49.08kg of secondary aluminum-silicon-iron alloy blocks in a ball mill, heating in a high-temperature furnace into which water vapor is introduced, wherein the water vapor is introduced into the furnace for heating at the temperature of 900 ℃, the heat preservation time is 120min, cooling and solidifying, separating by magnetic separation under the magnetic field intensity of 0.50T, separating ferromagnetic substances from aluminum-silicon alloy containing oxide impurities, and refining the aluminum-silicon alloy containing impurities to remove impurities, wherein the refining temperature is 1200-1300 ℃, the refining time is 25-30 min, and 40.22kg of industrial silicon with the purity of 94.55% is obtained.
Example 3
A method for remelting, centrifugally separating and classifying and purifying an aluminum-silicon-iron alloy is shown in a process flow chart as shown in figure 2 and comprises the following steps:
100kg of aluminum-silicon-iron alloy is put into an intermediate frequency furnace for high-temperature smelting, and the melting temperature is 1400-1600 ℃, wherein the mass fraction of Al in the aluminum-silicon-iron alloy is 53.46%, the mass fraction of Si is 39.43% and the mass fraction of Fe is 5.20%, so as to obtain aluminum-silicon-iron alloy melt; casting the melt in a mould, cooling to 650 ℃ at a speed of 5 ℃/min, preserving heat for 60min at the temperature, and cooling to room temperature to obtain the primary aluminum-silicon-iron alloy block. As shown in figure 1, the alloy phase diagram of the invention shows that when the cooling temperature is reduced to 900-950 ℃, silicon crystals are firstly precipitated and grown up, as the cooling temperature is reduced, the silicon content in the melt is gradually reduced, when the temperature is reduced to 800-850 ℃, needle-shaped or sheet-shaped iron phases start to crystallize out, the temperature is continuously reduced to below 577 ℃, and the molten aluminum-silicon alloy is solidified and exists in framework gaps formed by the silicon phases to form solid blocks.
100Kg of primary aluminum-silicon-iron alloy blocks are put into a hypergravity centrifugal device with a heating device, heated to 650 ℃, kept at a temperature for 180 minutes, melted aluminum-silicon and primary silicon and iron phases still kept solid, the centrifugal device is started, the hypergravity coefficient is 212g, the separation time is 10 minutes, under the hypergravity effect, the melt is separated through a porous filter plate, 52.13kg of aluminum-silicon alloy for casting meeting the industrial standard is obtained after cooling and solidifying the melt, wherein the mass fraction of Fe is 0.37%, the mass fraction of Si is 11.09%, and the slag is 47.87kg of secondary aluminum-silicon-iron alloy blocks.
Crushing 47.87kg of secondary aluminum-silicon-iron alloy blocks, putting the blocks into a ball mill for crushing, heating in a high-temperature furnace into which water vapor is introduced, wherein the water vapor is introduced into the furnace for heating at the temperature of 950 ℃, the heat preservation time is 30min, cooling and solidifying, separating by magnetic separation under the magnetic field intensity of 0.50T, separating ferromagnetic substances from aluminum-silicon alloy containing oxide impurities, and refining the aluminum-silicon alloy containing impurities for impurity removal, wherein the refining temperature is 1200-1300 ℃, the refining time is 25-30 min, and 40.25kg of aluminum-silicon alloy for casting meeting the industrial standard is obtained, wherein the mass fraction of Fe is 0.65%, and the mass fraction of Si is 83.60%.
The present application has been described in terms of embodiments, and it will be appreciated by those of skill in the art that various changes can be made to the features and embodiments, or equivalents can be substituted, without departing from the spirit and scope of the application. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the application without departing from the essential scope thereof. Therefore, it is intended that the application not be limited to the particular embodiment disclosed, but that the application will include all embodiments falling within the scope of the appended claims.
Claims (8)
1. The method for remelting, centrifugally separating and classifying the purified aluminum-silicon-iron alloy is characterized by comprising the following steps of: (1) Putting the aluminum-silicon-iron alloy into an intermediate frequency furnace for high-temperature smelting to obtain an aluminum-silicon-iron alloy melt; (2) Casting the molten mass in a mould, controlling the cooling speed and time, cooling to 580-1050 ℃ at the speed of 1-20 ℃/min, preserving heat for 30-120 min, precipitating and growing alloy phase, and naturally cooling to room temperature to obtain a primary aluminum-silicon-iron alloy block; (3) Loading the primary aluminum-silicon-iron alloy block into a hypergravity centrifugal device with a heating device, heating at low temperature, and preserving heat for 60-300 min after the primary aluminum-silicon-iron alloy block is heated to 580-650 ℃ to enable aluminum silicon to be melted and primary crystal silicon and iron phases to remain solid; starting a centrifugal machine, wherein the separation time is 5-15 min under the action of supergravity, the supergravity coefficient is 200-500 g, the melt is separated through a porous filter plate, the melt is cooled and solidified to obtain aluminum-silicon alloy for casting meeting the industrial standard, and the slag is a secondary aluminum-silicon-iron alloy block; (4) Crushing the secondary aluminum-silicon-iron alloy blocks, heating the crushed blocks in a high-temperature furnace into which water vapor is introduced, cooling and solidifying the blocks, and separating the blocks by magnetic separation to obtain aluminum-silicon alloy containing oxide impurities and ferromagnetic substances; (5) And refining the aluminum-silicon alloy containing impurities to remove impurities to obtain aluminum-silicon alloy or industrial silicon, thereby realizing the graded purification of the aluminum-silicon-iron alloy.
2. The method for remelting, centrifuging, magnetic separating and classifying the purified aluminum-silicon-iron alloy according to claim 1, wherein in the step (1), the aluminum-silicon-iron alloy is prepared from aluminum-containing minerals through a metallurgical process, the aluminum-containing minerals are aluminum-containing waste residues or low-grade aluminum ore resources, and the aluminum-containing waste residues mainly comprise aluminum oxide and silicon oxide, and comprise one or a mixture of a plurality of bauxite magnetic separation tailings, coal gangue, fly ash, shale slag and the like; the low-grade aluminum ore resource refers to one or more of bauxite, kaolinite, albite, potash feldspar and the like with lower aluminum-silicon ratio.
3. The method for remelting, centrifugally separating and classifying and purifying the aluminum-silicon-iron alloy according to claim 1, wherein in the step (1), the content range of the aluminum-silicon-iron alloy is as follows: 10-90% of Al, 10-90% of Si and 0.7-10% of Fe.
4. The method for remelting, centrifugally separating and classifying to purify the aluminum-silicon-iron alloy according to claim 1, wherein in the step (1), the melting temperature in the intermediate frequency furnace is 1400-1600 ℃.
5. The method for remelting, centrifugally separating and classifying to purify the aluminum-silicon-iron alloy according to claim 1, wherein in the step (3), the porous filter plate is an S310 high-temperature resistant stainless steel filter.
6. The method for purifying an aluminum-silicon-iron alloy by remelting, centrifugal and magnetic separation in a grading manner according to claim 1, wherein in the step (3), the supergravity separation is continuous treatment or intermittent batch treatment.
7. The method for purifying the aluminum-silicon-iron alloy by remelting, centrifuging, magnetic separating and classifying according to claim 1, wherein in the step (4), the steam inlet amount is 100-150 ml/min, the heating temperature is 800-950 ℃, the heating time is 30-120 min, and the magnetic field strength is 0.02-1.0T.
8. The method for remelting, centrifugally separating and classifying and purifying the aluminum-silicon-iron alloy according to claim 1, wherein in the step (5), the refining temperature is 1200-1300 ℃ and the refining time is 25-30 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011267938.1A CN114480867B (en) | 2020-11-13 | 2020-11-13 | Method for remelting, centrifugal and magnetic separation and grading purification of aluminum-silicon-iron alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011267938.1A CN114480867B (en) | 2020-11-13 | 2020-11-13 | Method for remelting, centrifugal and magnetic separation and grading purification of aluminum-silicon-iron alloy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114480867A CN114480867A (en) | 2022-05-13 |
| CN114480867B true CN114480867B (en) | 2024-06-21 |
Family
ID=81490907
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011267938.1A Active CN114480867B (en) | 2020-11-13 | 2020-11-13 | Method for remelting, centrifugal and magnetic separation and grading purification of aluminum-silicon-iron alloy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114480867B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105821218A (en) * | 2016-05-10 | 2016-08-03 | 北京科技大学 | Method of removing impurity element copper in crude lead through supergravity |
| CN110846513A (en) * | 2019-12-10 | 2020-02-28 | 刘旭 | Method for filtering and centrifugally separating mixture containing aluminum, silicon, iron and the like, removing impurities and purifying |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005095658A1 (en) * | 2004-03-19 | 2005-10-13 | Corus Technology Bv | Method for the purification of a molten metal |
| CN104342561A (en) * | 2014-11-24 | 2015-02-11 | 阳谷祥光铜业有限公司 | Method for recovering copper, iron and silicon from copper smelting slag |
| CN108165810B (en) * | 2017-12-11 | 2019-09-27 | 昆明理工大学 | Device and process for removing iron and silicon phases in primary aluminum-silicon alloy in one step |
-
2020
- 2020-11-13 CN CN202011267938.1A patent/CN114480867B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105821218A (en) * | 2016-05-10 | 2016-08-03 | 北京科技大学 | Method of removing impurity element copper in crude lead through supergravity |
| CN110846513A (en) * | 2019-12-10 | 2020-02-28 | 刘旭 | Method for filtering and centrifugally separating mixture containing aluminum, silicon, iron and the like, removing impurities and purifying |
Non-Patent Citations (1)
| Title |
|---|
| 用一次铝硅合金制取铸造铝硅合金的研究;周祥宇;《东北大学硕士学位论文》;第32、33页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114480867A (en) | 2022-05-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110846513A (en) | Method for filtering and centrifugally separating mixture containing aluminum, silicon, iron and the like, removing impurities and purifying | |
| CN114477187B (en) | Method for extracting industrial silicon from aluminum-silicon-iron alloy | |
| CN101921934A (en) | High-performance uniformity aluminium alloy ingot and production method thereof | |
| CN110902685A (en) | Method for separating silicon-containing mixture to obtain industrial silicon | |
| US11780734B2 (en) | Process for the production of commercial grade silicon | |
| CN110904340A (en) | Method for removing harmful elements and impurities in iron-containing mixture by centrifugation | |
| CN102464320A (en) | Metallurgical chemical refining method for silicon | |
| CN113913621B (en) | Method for preparing aluminum-silicon-iron alloy by using high-aluminum gangue and purifying in grading manner | |
| Meng et al. | Effective separation of fusing agent from refined magnesium slag by supergravity technology | |
| Meng et al. | Enrichment and separation behaviors of impurities from stripped copper wire with super-gravity fields | |
| CN114480867B (en) | Method for remelting, centrifugal and magnetic separation and grading purification of aluminum-silicon-iron alloy | |
| CN104071790B (en) | Electromagnetic agitation silicon alloy melt silicon purifying plant and method | |
| CN114480855B (en) | Method for preparing aluminum-silicon-iron alloy by using high-alumina fly ash and purifying in grading manner | |
| Gu et al. | Synergetic recovery of Ti and Fe from Ti-bearing blast furnace slag and red mud by diamond wire saw silicon waste | |
| CN114480868B (en) | Method for purifying aluminum-silicon-iron alloy by high-temperature remelting centrifugal separation and classification | |
| CN114480890B (en) | Method for purifying aluminum-silicon-iron alloy by low-temperature and high-temperature two-step remelting centrifugal separation | |
| CN113897492B (en) | Method for purifying aluminum-silicon-iron alloy by high-temperature and low-temperature two-step remelting centrifugal separation | |
| CN114480865B (en) | Method for purifying aluminum-silicon-iron alloy by low-temperature remelting centrifugal separation and classification | |
| CN114480891B (en) | Method for extracting aluminum-silicon alloy from aluminum-silicon-iron alloy | |
| CN112110450A (en) | A method for removing impurity boron in metallurgical grade silicon | |
| CN114480864B (en) | Method for remelting, centrifugal and electroselection grading purification of aluminum-silicon-iron alloy | |
| JPS5933641B2 (en) | Processing method for converter slag | |
| CN114480866A (en) | Method for remelting centrifugal flotation and graded purification of ferro-silicon-aluminum alloy | |
| CN108101064B (en) | Method for separating hard impurities in silicon by temperature gradient | |
| CN119663003A (en) | A method for extracting aluminum silicon alloy from waste ferrosilicon alloy |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |