CN112111759A - Method for manufacturing grain-refined and impurity-free aluminum ingot - Google Patents
Method for manufacturing grain-refined and impurity-free aluminum ingot Download PDFInfo
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- CN112111759A CN112111759A CN202010846681.9A CN202010846681A CN112111759A CN 112111759 A CN112111759 A CN 112111759A CN 202010846681 A CN202010846681 A CN 202010846681A CN 112111759 A CN112111759 A CN 112111759A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 122
- 238000000034 method Methods 0.000 title claims abstract description 62
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 146
- 238000006243 chemical reaction Methods 0.000 claims abstract description 115
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 238000002844 melting Methods 0.000 claims abstract description 55
- 230000008018 melting Effects 0.000 claims abstract description 55
- 238000005266 casting Methods 0.000 claims abstract description 54
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 50
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910001610 cryolite Inorganic materials 0.000 claims abstract description 49
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000012535 impurity Substances 0.000 claims abstract description 38
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000654 additive Substances 0.000 claims abstract description 36
- 230000000996 additive effect Effects 0.000 claims abstract description 36
- 229910052796 boron Inorganic materials 0.000 claims abstract description 36
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000007670 refining Methods 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000000465 moulding Methods 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 229910001570 bauxite Inorganic materials 0.000 claims description 45
- 238000000227 grinding Methods 0.000 claims description 40
- 239000000047 product Substances 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 15
- 239000000376 reactant Substances 0.000 claims description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 230000002571 modificatory effect Effects 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000012634 fragment Substances 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 238000009288 screen filtration Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 230000006866 deterioration Effects 0.000 claims description 4
- 229910052810 boron oxide Inorganic materials 0.000 claims description 3
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 3
- XTLNYNMNUCLWEZ-UHFFFAOYSA-N ethanol;propan-2-one Chemical compound CCO.CC(C)=O XTLNYNMNUCLWEZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 239000004519 grease Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 abstract description 10
- 230000008025 crystallization Effects 0.000 abstract description 10
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 8
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000003044 adaptive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
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- Organic Chemistry (AREA)
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Abstract
The invention provides a method for manufacturing a grain-refined and impurity-free aluminum ingot, which comprises a raw material preparation process, a raw material pretreatment process, an electrolytic melting reaction process, an impurity removal and casting process and an aluminum ingot finished product forming process, the aluminum ingot manufacturing method comprises the steps of processing and preparing aluminum ore to obtain alumina with corresponding purity, preparing the compositions of alumina, titanium oxide, cobalt oxide and cryolite with corresponding weight ratio, carrying out electrolytic melting reaction, residue filtration and casting molding, and the boron-containing metamorphic additive is adaptively added according to the real-time reaction temperature in the process of electrolytic melting reaction, so as to improve the crystallization state of the aluminum liquid in the subsequent casting and forming process by means of the boron-containing modifying additive, thereby improving the grain refining degree of the aluminum ingot and reducing the impurity content in the aluminum ingot, and obtaining the high-quality aluminum ingot finished product.
Description
Technical Field
The invention relates to the technical field of aluminum ingot production processes, in particular to a grain-refining impurity-free aluminum ingot manufacturing method.
Background
Aluminum alloys are widely used in different applications due to their light weight and high mechanical strength. At present, aluminum ingots are mainly used as raw materials for manufacturing aluminum alloy, the aluminum ingots are generally manufactured by carrying out electrolytic reaction on aluminum oxide, and other oxides and catalysts are required to be contacted in the electrolytic reaction process to improve the efficiency of the electrolytic reaction. The crystallization degree and the impurity existing state inside the aluminum ingot can influence the quality of subsequent aluminum alloy manufacturing and forming, and if the crystallization degree inside the aluminum ingot is higher or more impurities exist, the toughness, the rigidity and the corrosion resistance of the aluminum alloy can be influenced. Therefore, the prior art urgently needs a manufacturing process capable of manufacturing grain-refining and impurity-free aluminum ingots.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for manufacturing a grain-refined and impurity-free aluminum ingot, which comprises a raw material preparation process, a raw material pretreatment process, an electrolytic melting reaction process, an impurity removal and casting process and an aluminum ingot finished product forming process, wherein the method for manufacturing the aluminum ingot comprises the steps of processing and preparing aluminum ore to obtain aluminum oxide with corresponding purity, preparing compositions of the aluminum oxide, the titanium oxide, the cobalt oxide and the cryolite with corresponding weight ratios to carry out the electrolytic melting reaction, residue filtration and casting molding, and adaptively adding a boron-containing modification additive according to real-time reaction temperature in the electrolytic melting reaction process to improve the crystallization state of aluminum liquid in the subsequent casting molding process by virtue of the boron-containing modification additive, thereby improving the grain-refined degree of the aluminum ingot and reducing the impurity content in the aluminum ingot, thereby obtaining the finished product of the aluminum ingot with high quality.
The invention provides a method for manufacturing a grain-refined and impurity-free aluminum ingot, which is characterized by comprising the following steps of:
step S1, a raw material preparation process for obtaining an alumina raw material satisfying a preset purity from bauxite, and preparing a titanium oxide raw material, a cobalt oxide raw material, a cryolite raw material, and a boron-containing modificatory additive;
step S2, a raw material pretreatment step of performing a refining process on the alumina raw material, the titania raw material, the cobalt oxide raw material, and the cryolite raw material, and preparing a composition containing alumina, titania, cobalt oxide, and cryolite satisfying a predetermined weight ratio condition;
step S3, an electrolytic melting reaction process, wherein the melting reaction process is used for carrying out electrolytic melting reaction on the composition and adding the boron-containing metamorphic additive in time periods corresponding to different reaction temperature intervals in the reaction process;
step S4, impurity removal and casting processes are performed, wherein the impurity removal and casting processes are used for sequentially performing residue filtration treatment and casting molding treatment on reaction products of the electrolytic melting reaction;
step S5, an aluminum ingot finished product forming procedure, wherein the aluminum ingot finished product forming procedure is used for weighing and packaging the aluminum ingot blank obtained by casting and molding treatment so as to obtain a grain-refined aluminum ingot finished product without impurities;
further, in the step S1, the raw material preparation step specifically includes,
step S101, crushing and grinding the bauxite to obtain bauxite powder meeting a predetermined fineness condition, and performing insoluble particle separation treatment and purification treatment on the bauxite powder to obtain the alumina raw material;
step S102, cleaning and drying the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material in sequence respectively to remove oil and water components contained in the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material;
step S103, dissolving boron oxide in a dilute sulfuric acid solution to form the boron-containing metamorphic additive;
further, in the step S101, subjecting the bauxite to crushing and grinding processing to obtain bauxite powder satisfying a predetermined fineness condition, and subjecting the bauxite powder to insoluble particle separation processing and purification processing to obtain the alumina raw material specifically includes,
step S1011, the bauxite is subjected to stamping and crushing treatment so as to obtain bauxite fragments, and then the bauxite fragments are subjected to ball grinding treatment so as to obtain bauxite powder with the fineness of 25-150 meshes;
step S1012, dissolving the bauxite powder in deionized water to form a bauxite aqueous solution, and then performing a filtration screening process on the bauxite aqueous solution to separate insoluble particles contained therein;
step S1013, purifying the bauxite filtrate obtained by the filtering and screening treatment to obtain the alumina raw material;
or,
in the step S102, the titanium oxide raw material, the cobalt oxide raw material, and the cryolite raw material are sequentially subjected to cleaning treatment and drying treatment, respectively, to remove oil and fat components and water components contained therein,
step S1021, respectively cleaning the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material by adopting ethanol-acetone mixed solution and deionized water so as to remove grease components contained in the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material;
step S1022, performing drying treatment or infrared irradiation drying treatment on the washed titanium oxide raw material, cobalt oxide raw material, and cryolite raw material, thereby removing a crystal water component or a free water component contained therein;
further, in the step S2, the raw material pretreatment step specifically includes,
step S201, respectively carrying out mechanical grinding refining treatment on the alumina raw material, the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material so as to obtain powdery materials with the average grain diameter within the range of 300-800 μm;
step S202, sequentially mixing the powdered alumina, the powdered titanium oxide, the powdered cobalt oxide and the powdered cryolite according to the weight ratio of 60-100: 5-10: 2-6: 4 to 8, configured to form said composition;
further, in the step S201, the alumina raw material, the titania raw material, the cobalt oxide raw material, and the cryolite raw material are subjected to the refining process of mechanical grinding, respectively, to thereby obtain powdery materials having an average particle diameter in the range of 300 μm to 800 μm specifically including,
step S2011, performing coarse mechanical grinding with a first grinding speed on the alumina raw material, the titania raw material, the cobalt oxide raw material, and the cryolite raw material, respectively, and performing screen filtration on products obtained by the coarse mechanical grinding, respectively;
step S2012, performing fine mechanical grinding with a second grinding speed on the coarse ground alumina product, the coarse ground titania product, the coarse ground cobalt oxide product and the coarse ground cryolite product obtained by the screen filtration, respectively, to finally obtain powdered alumina, powdered titanium oxide, powdered cobalt oxide and powdered cryolite having an average particle size in a range of 300 μm to 800 μm, wherein the second grinding speed is greater than the first grinding speed;
further, in the step S3, the electrolytic melting reaction step specifically includes,
step S301, putting the composition into an electrolytic reaction tank, and carrying out electrolytic melting reaction in an inert gas atmosphere;
step S302, detecting real-time reaction temperature information of the electrolytic melting reaction, and adding the boron-containing metamorphic additive into the electrolytic melting reactant within a corresponding time period according to the corresponding relation between the real-time reaction temperature information and a preset reaction temperature interval;
further, the step S301 of putting the composition into an electrolytic reaction tank and performing an electrolytic melting reaction in an inert gas atmosphere specifically includes,
3011, putting the composition into the electrolytic reaction tank, and stirring the composition in a single direction at a rotation speed of 30-85 r/min;
3012, cyclically introducing argon into the electrolytic reaction tank at a flow rate of 1.5 to 4L/min to form an argon protective atmosphere in the electrolytic reaction tank;
or,
in the step S302, detecting real-time reaction temperature information of the electrolytic melting reaction, and adding the boron-containing modifying additive to the electrolytic melting reactant within a corresponding time period according to a corresponding relationship between the real-time reaction temperature information and a preset reaction temperature interval,
step S3021, detecting real-time reaction temperature information of the electrolytic melting reaction, and determining a matching relationship between the real-time reaction temperature information and a first temperature range of 0 ℃ to 100 ℃, a second temperature range of 100 ℃ to 200 ℃, and a third temperature range of 200 ℃ to 400 ℃ in the preset reaction temperature range;
step S3022, when the real-time reaction temperature information matches the first temperature interval, adding a first weight of the boron-containing modificatory additive to the electrolytically molten reactant for a corresponding time period, when the real-time reaction temperature information matches the second temperature interval, adding a second weight of the boron-containing modificatory additive to the electrolytically molten reactant for a corresponding time period, when the real-time reaction temperature information matches the third temperature interval, adding a third weight of the boron-containing modificatory additive to the electrolytically molten reactant for a corresponding time period, and the first weight < the second weight < the third weight;
further, in the step S4, the impurity removing and casting process may include,
step S401, after centrifugal stirring and precipitation are carried out on the reaction product of the electrolytic melting reaction, filtering residue precipitate formed by precipitation;
step S402, casting and forming the electrolytic aluminum liquid obtained by filtering, and actively cooling an aluminum ingot casting body obtained by casting;
further, in the step S402, the casting and forming of the filtered electrolytic aluminum liquid, and the active cooling of the aluminum ingot casting body obtained by casting specifically include,
after casting and forming the filtered electrolytic aluminum liquid, carrying out air-cooled active cooling treatment on the aluminum ingot casting body so as to cool and form the aluminum ingot casting body;
further, in step S5, the aluminum ingot forming process includes,
step S501, weighing the aluminum ingot blank obtained by the casting molding treatment so as to determine whether the aluminum ingot blank meets the preset weight requirement;
step S502, label printing and outer packaging treatment are carried out on the aluminum ingot blank meeting the preset weight requirement, and therefore the grain-refined aluminum ingot finished product without impurities is obtained.
Compared with the prior art, the grain-refining impurity-free aluminum ingot manufacturing method comprises a raw material preparation process, a raw material pretreatment process, an electrolytic melting reaction process, an impurity removal and casting process and an aluminum ingot finished product forming process, the aluminum ingot manufacturing method comprises the steps of processing and preparing aluminum ore to obtain aluminum oxide with corresponding purity, preparing aluminum oxide, titanium oxide, cobalt oxide and cryolite compositions with corresponding weight ratios to carry out electrolytic melting reaction, residue filtration and casting forming, and adaptively adding a boron-containing modification additive according to a real-time reaction temperature in the electrolytic melting reaction process to improve the crystallization state of aluminum liquid in the subsequent casting forming process by means of the boron-containing modification additive, so that the grain-refining degree of the aluminum ingot is improved, the impurity content in the aluminum ingot is reduced, and a high-quality aluminum ingot finished product is obtained.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the embodiments or technical descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic overall flow chart of a grain-refining impurity-free aluminum ingot manufacturing method provided by the invention.
Fig. 2 is a schematic view of a refining flow of step S1 in the method for manufacturing a grain-refined aluminum ingot.
Fig. 3 is a schematic view of a refining flow of step S2 in the method for manufacturing a grain-refined aluminum ingot.
Fig. 4 is a schematic view of a refining flow of step S3 in the method for manufacturing a grain-refined aluminum ingot without impurities according to the present invention.
Fig. 5 is a schematic view of a refining flow of step S4 in the method for manufacturing a grain-refined aluminum ingot without impurities according to the present invention.
Fig. 6 is a schematic view of a refining flow of step S5 in the method for manufacturing a grain-refined aluminum ingot without impurities according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a schematic overall flow chart of the method for manufacturing a grain-refined aluminum ingot without impurities is provided. The method for manufacturing the grain-refined aluminum ingot without impurities comprises the following steps:
a step S1 of raw material preparation for obtaining an alumina raw material satisfying a preset purity from bauxite, and preparing a titanium oxide raw material, a cobalt oxide raw material, a cryolite raw material, and a boron-containing modificatory additive;
step S2, a raw material pretreatment step for refining the alumina raw material, the titania raw material, the cobalt oxide raw material, and the cryolite raw material and preparing a composition containing alumina, titania, cobalt oxide, and cryolite satisfying a predetermined weight ratio condition;
step S3, an electrolytic melting reaction process, wherein the melting reaction process is used for carrying out electrolytic melting reaction on the composition and adding the boron-containing metamorphic additive in time periods corresponding to different reaction temperature intervals in the reaction process;
step S4, impurity removing and casting process, wherein the impurity removing and casting process is used for sequentially carrying out residue filtering treatment and casting molding treatment on the reaction product of the electrolytic melting reaction;
and step S5, an aluminum ingot finished product forming procedure, wherein the aluminum ingot finished product forming procedure is used for weighing and packaging the aluminum ingot blank obtained by the casting and forming treatment so as to obtain the aluminum ingot finished product with grain refining and no impurity.
Preferably, the grain-refining impurity-free aluminum ingot manufacturing method is characterized in that a cobalt oxide raw material and a boron-containing modification additive are added on the basis of a common aluminum oxide raw material, a titanium oxide raw material and a cryolite raw material, wherein the cobalt oxide raw material can improve the corrosion resistance of the aluminum ingot, and the boron-containing modification additive can control the electrolytic reaction progress of the aluminum oxide and the precipitation speed of elemental aluminum in the electrolytic melting reaction process of the aluminum oxide, so that the phenomenon that the integral crystallization inside the aluminum ingot is influenced due to large-area crystallization of the elemental aluminum in the electrolytic process is avoided, and the grain-refining forming of the aluminum ingot is ensured.
Referring to fig. 2, a schematic view of a refining flow of step S1 in the method for manufacturing a grain-refined aluminum ingot according to the present invention is shown. In step S1, the raw material preparation process specifically includes,
step S101, grinding the bauxite to obtain bauxite powder meeting a predetermined fineness condition, and performing insoluble particle separation treatment and purification treatment on the bauxite powder to obtain the alumina raw material;
step S102, cleaning and drying the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material in sequence respectively to remove oil and water components contained therein;
step S103, boron oxide is dissolved in dilute sulfuric acid solution to form the boron-containing metamorphic additive.
Preferably, in the step S101, subjecting the bauxite to a crushing and grinding process to obtain a bauxite powder satisfying a predetermined fineness condition, and subjecting the bauxite powder to an insoluble particle separating process and a purifying process to obtain the alumina raw material specifically includes,
step S1011, the bauxite is subjected to stamping and crushing treatment so as to obtain bauxite fragments, and then the bauxite fragments are subjected to ball grinding treatment so as to obtain bauxite powder with the fineness of 25-150 meshes;
step S1012, dissolving the bauxite powder in deionized water to form a bauxite aqueous solution, and then performing a filtration screening process on the bauxite aqueous solution to separate insoluble particles contained therein;
step S1013, the bauxite filtrate obtained by the filtering and screening process is subjected to a purification process, thereby obtaining the alumina raw material.
Preferably, in the step S102, the titanium oxide raw material, the cobalt oxide raw material, and the cryolite raw material are sequentially subjected to a cleaning process and a drying process, respectively, to thereby remove oil and water components contained therein specifically including,
step S1021, respectively cleaning the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material by adopting ethanol-acetone mixed solution and deionized water so as to remove grease components contained in the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material;
step S1022, the titanium oxide raw material, the cobalt oxide raw material, and the cryolite raw material after cleaning are subjected to drying treatment or infrared irradiation drying treatment, thereby removing a crystal water component or a free water component contained therein.
Referring to fig. 3, it is a schematic view of a refining flow of step S2 in the method for manufacturing a grain-refined aluminum ingot according to the present invention. In step S2, the raw material pretreatment step specifically includes,
step S201, respectively carrying out mechanical grinding refining treatment on the alumina raw material, the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material so as to obtain powdery materials with the average grain diameter within the range of 300-800 μm;
step S202, sequentially mixing the powdered alumina, the powdered titanium oxide, the powdered cobalt oxide and the powdered cryolite according to the weight ratio of 60-100: 5-10: 2-6: 4-8, in a weight ratio to form the composition.
Preferably, in the step S201, the alumina raw material, the titania raw material, the cobalt oxide raw material and the cryolite raw material are subjected to a refining process of mechanical grinding, respectively, to thereby obtain powdery materials having an average particle diameter in the range of 300 μm to 800 μm specifically including,
step S2011, performing coarse mechanical grinding with a first grinding speed on the alumina raw material, the titania raw material, the cobalt oxide raw material, and the cryolite raw material, respectively, and performing screen filtration on products obtained by the coarse mechanical grinding, respectively;
step S2012, fine mechanical grinding with a second grinding speed is performed on the coarse ground alumina product, the coarse ground titania product, the coarse ground cobalt oxide product, and the coarse ground cryolite product obtained by filtering with the screen, so as to finally obtain powdered alumina, powdered titania, powdered cobalt oxide, and powdered cryolite having an average particle size in a range of 300 μm to 800 μm, where the second grinding speed is greater than the first grinding speed.
Referring to fig. 4, a schematic view of a refining flow of step S3 in the method for manufacturing a grain-refined aluminum ingot according to the present invention is shown. In step S3, the electrolytic melting reaction process specifically includes,
step S301, putting the composition into an electrolytic reaction tank, and carrying out electrolytic melting reaction in an inert gas atmosphere;
step S302, detecting real-time reaction temperature information of the electrolytic melting reaction, and adding the boron-containing deterioration additive into the electrolytic melting reactant within a corresponding time period according to the corresponding relation between the real-time reaction temperature information and a preset reaction temperature interval.
Preferably, in the step S301, the step of putting the composition into an electrolytic reaction tank and performing an electrolytic melting reaction in an inert gas atmosphere specifically includes,
3011, putting the composition into the electrolytic reaction tank, and stirring the composition in a single direction at a rotation speed of 30-85 r/min;
3012, circularly introducing argon gas into the electrolytic reaction tank at a flow rate of 1.5-4L/min to form an argon gas protective atmosphere in the electrolytic reaction tank.
Preferably, in the step S302, detecting real-time reaction temperature information of the electrolytic melting reaction, and adding the boron-containing modifying additive to the electrolytic melting reactant within a corresponding time period according to a corresponding relationship between the real-time reaction temperature information and a preset reaction temperature interval specifically includes,
step S3021, detecting real-time reaction temperature information of the electrolytic melting reaction, and determining a matching relationship between the real-time reaction temperature information and a first temperature range of 0 ℃ to 100 ℃, a second temperature range of 100 ℃ to 200 ℃, and a third temperature range of 200 ℃ to 400 ℃ in the preset reaction temperature range;
step S3022, when the real-time reaction temperature information matches the first temperature interval, adding a first weight of the boron-containing modificatory additive to the electrolytically molten reactant in the corresponding time period, when the real-time reaction temperature information matches the second temperature interval, adding a second weight of the boron-containing modificatory additive to the electrolytically molten reactant in the corresponding time period, when the real-time reaction temperature information matches the third temperature interval, adding a third weight of the boron-containing modificatory additive to the electrolytically molten reactant in the corresponding time period, and the first weight < the second weight < the third weight.
In the electrolytic melting reaction process, the speed and progress of electrolytic precipitation of the simple substance aluminum can be influenced by the temperature of the electrolytic melting reaction, the precipitation speed and progress of the simple substance aluminum and the crystallization degree of the simple substance aluminum can be effectively adjusted by adding the boron-containing deterioration additive with the adaptive weight in different reaction temperature intervals, and in addition, the higher the electrolytic melting reaction temperature is, the larger the weight of the boron-containing deterioration additive is, the more the crystallization degree of the simple substance aluminum can be favorably adjusted, so that the condition of large-area crystal blocks is effectively avoided.
Referring to fig. 5, a schematic view of a refining flow of step S4 in the method for manufacturing a grain-refined aluminum ingot according to the present invention is shown. In the step S4, the impurity removing and casting process may include,
step S401, after centrifugal stirring and precipitation are carried out on the reaction product of the electrolytic melting reaction, filtering residue precipitate formed by precipitation;
and S402, casting and forming the electrolytic aluminum liquid obtained by filtering, and actively cooling the aluminum ingot casting body obtained by casting.
Preferably, in the step S402, the casting and forming of the filtered electrolytic aluminum liquid, and the active cooling of the aluminum ingot casting body obtained by casting specifically include,
and after casting and forming the filtered electrolytic aluminum liquid, carrying out air-cooled active cooling treatment on the aluminum ingot casting body so as to cool and form the aluminum ingot casting body.
Referring to fig. 6, it is a schematic view of a refining flow of step S5 in the method for manufacturing a grain-refined aluminum ingot according to the present invention. In step S5, the aluminum ingot forming process includes,
step S501, weighing the aluminum ingot blank obtained by the casting molding treatment so as to determine whether the aluminum ingot blank meets the preset weight requirement;
step S502, label printing and outer package processing are carried out on the aluminum ingot blank meeting the preset weight requirement, and therefore the grain-refined aluminum ingot finished product without impurities is obtained.
As is apparent from the above description of the embodiments, the method for manufacturing a grain-refined impurity-free aluminum ingot includes a raw material preparation step, a raw material pretreatment step, an electrolytic melting reaction step, an impurity removal and casting step, and an aluminum ingot product formation step, the aluminum ingot manufacturing method comprises the steps of processing and preparing aluminum ore to obtain alumina with corresponding purity, preparing the compositions of alumina, titanium oxide, cobalt oxide and cryolite with corresponding weight ratio, carrying out electrolytic melting reaction, residue filtration and casting molding, and the boron-containing metamorphic additive is adaptively added according to the real-time reaction temperature in the process of electrolytic melting reaction, so as to improve the crystallization state of the aluminum liquid in the subsequent casting and forming process by means of the boron-containing modifying additive, thereby improving the grain refining degree of the aluminum ingot and reducing the impurity content in the aluminum ingot, and obtaining the high-quality aluminum ingot finished product.
Claims (10)
1. The method for manufacturing the aluminum ingot with grain refining and no impurity is characterized by comprising the following steps:
step S1, a raw material preparation process for obtaining an alumina raw material satisfying a preset purity from bauxite, and preparing a titanium oxide raw material, a cobalt oxide raw material, a cryolite raw material, and a boron-containing modificatory additive;
step S2, a raw material pretreatment step of performing a refining process on the alumina raw material, the titania raw material, the cobalt oxide raw material, and the cryolite raw material, and preparing a composition containing alumina, titania, cobalt oxide, and cryolite satisfying a predetermined weight ratio condition;
step S3, an electrolytic melting reaction process, wherein the melting reaction process is used for carrying out electrolytic melting reaction on the composition and adding the boron-containing metamorphic additive in time periods corresponding to different reaction temperature intervals in the reaction process;
step S4, impurity removal and casting processes are performed, wherein the impurity removal and casting processes are used for sequentially performing residue filtration treatment and casting molding treatment on reaction products of the electrolytic melting reaction;
and step S5, an aluminum ingot finished product forming procedure, wherein the aluminum ingot finished product forming procedure is used for weighing and packaging the aluminum ingot blank obtained by the casting and forming treatment so as to obtain the grain-refined aluminum ingot finished product without impurities.
2. The method of claim 1 for producing a refined crystalline aluminum ingot without impurities, wherein:
in the step S1, the raw material preparation step specifically includes,
step S101, crushing and grinding the bauxite to obtain bauxite powder meeting a predetermined fineness condition, and performing insoluble particle separation treatment and purification treatment on the bauxite powder to obtain the alumina raw material;
step S102, cleaning and drying the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material in sequence respectively to remove oil and water components contained in the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material;
step S103, boron oxide is dissolved in dilute sulfuric acid solution, so as to form the boron-containing metamorphic additive.
3. The method of claim 1 for producing a refined crystalline aluminum ingot without impurities, wherein:
in the step S101, subjecting the bauxite to crushing and grinding processing to obtain bauxite powder satisfying a predetermined fineness condition, and subjecting the bauxite powder to insoluble particle separation processing and purification processing to obtain the alumina raw material specifically includes,
step S1011, the bauxite is subjected to stamping and crushing treatment so as to obtain bauxite fragments, and then the bauxite fragments are subjected to ball grinding treatment so as to obtain bauxite powder with the fineness of 25-150 meshes;
step S1012, dissolving the bauxite powder in deionized water to form a bauxite aqueous solution, and then performing a filtration screening process on the bauxite aqueous solution to separate insoluble particles contained therein;
step S1013, purifying the bauxite filtrate obtained by the filtering and screening treatment to obtain the alumina raw material;
or,
in the step S102, the titanium oxide raw material, the cobalt oxide raw material, and the cryolite raw material are sequentially subjected to cleaning treatment and drying treatment, respectively, to remove oil and fat components and water components contained therein,
step S1021, respectively cleaning the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material by adopting ethanol-acetone mixed solution and deionized water so as to remove grease components contained in the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material;
step S1022, the titanium oxide raw material, the cobalt oxide raw material, and the cryolite raw material after cleaning are subjected to drying treatment or infrared irradiation drying treatment, so that the crystallized water component or the free water component contained therein is removed.
4. The method of claim 1 for producing a refined crystalline aluminum ingot without impurities, wherein:
in the step S2, the raw material pretreatment step specifically includes,
step S201, respectively carrying out mechanical grinding refining treatment on the alumina raw material, the titanium oxide raw material, the cobalt oxide raw material and the cryolite raw material so as to obtain powdery materials with the average grain diameter within the range of 300-800 μm;
step S202, sequentially mixing the powdered alumina, the powdered titanium oxide, the powdered cobalt oxide and the powdered cryolite according to the weight ratio of 60-100: 5-10: 2-6: 4 to 8 by weight, configured to form said composition.
5. The method of manufacturing a grain-refined, impurity-free aluminum ingot according to claim 4, wherein:
in the step S201, the alumina raw material, the titania raw material, the cobalt oxide raw material and the cryolite raw material are subjected to refining treatment by mechanical grinding, respectively, to thereby obtain powdery materials having an average particle diameter in the range of 300 μm to 800 μm,
step S2011, performing coarse mechanical grinding with a first grinding speed on the alumina raw material, the titania raw material, the cobalt oxide raw material, and the cryolite raw material, respectively, and performing screen filtration on products obtained by the coarse mechanical grinding, respectively;
step S2012, fine mechanical grinding with a second grinding speed is performed on the alumina coarse grinding product, the titania coarse grinding product, the cobalt oxide coarse grinding product and the cryolite coarse grinding product obtained by the screen filtration, respectively, to finally obtain powdered alumina, powdered titania, powdered cobalt oxide and powdered cryolite having an average particle diameter in a range of 300 μm to 800 μm, wherein the second grinding speed is greater than the first grinding speed.
6. The method of claim 1 for producing a refined crystalline aluminum ingot without impurities, wherein:
in the step S3, the electrolytic melting reaction step specifically includes,
step S301, putting the composition into an electrolytic reaction tank, and carrying out electrolytic melting reaction in an inert gas atmosphere;
step S302, detecting real-time reaction temperature information of the electrolytic melting reaction, and adding the boron-containing deterioration additive into the electrolytic melting reactant within a corresponding time period according to the corresponding relation between the real-time reaction temperature information and a preset reaction temperature interval.
7. The method of claim 6, further comprising the step of:
specifically, the step S301 of putting the composition into an electrolytic reaction tank and performing an electrolytic melting reaction in an inert gas atmosphere includes,
3011, putting the composition into the electrolytic reaction tank, and stirring the composition in a single direction at a rotation speed of 30-85 r/min;
3012, cyclically introducing argon into the electrolytic reaction tank at a flow rate of 1.5 to 4L/min to form an argon protective atmosphere in the electrolytic reaction tank;
or,
in the step S302, detecting real-time reaction temperature information of the electrolytic melting reaction, and adding the boron-containing modifying additive to the electrolytic melting reactant within a corresponding time period according to a corresponding relationship between the real-time reaction temperature information and a preset reaction temperature interval,
step S3021, detecting real-time reaction temperature information of the electrolytic melting reaction, and determining a matching relationship between the real-time reaction temperature information and a first temperature range of 0 ℃ to 100 ℃, a second temperature range of 100 ℃ to 200 ℃, and a third temperature range of 200 ℃ to 400 ℃ in the preset reaction temperature range;
step S3022, when the real-time reaction temperature information matches the first temperature interval, adding a first weight of the boron-containing modificatory additive to the electrolytically molten reactant in a corresponding time period, when the real-time reaction temperature information matches the second temperature interval, adding a second weight of the boron-containing modificatory additive to the electrolytically molten reactant in a corresponding time period, when the real-time reaction temperature information matches the third temperature interval, adding a third weight of the boron-containing modificatory additive to the electrolytically molten reactant in a corresponding time period, and the first weight < the second weight < the third weight.
8. The method of claim 1 for producing a refined crystalline aluminum ingot without impurities, wherein:
in the step S4, the impurity removing and casting process may include,
step S401, after centrifugal stirring and precipitation are carried out on the reaction product of the electrolytic melting reaction, filtering residue precipitate formed by precipitation;
and S402, casting and forming the filtered electrolytic aluminum liquid, and actively cooling the cast aluminum ingot body.
9. The method of claim 8 for producing a refined crystalline aluminum ingot without impurities, wherein:
in the step S402, the casting and forming of the filtered electrolytic aluminum liquid, and the active cooling of the cast aluminum ingot body obtained by casting specifically include,
and after casting and forming the filtered electrolytic aluminum liquid, carrying out air-cooled active cooling treatment on the aluminum ingot casting body so as to cool and form the aluminum ingot casting body.
10. The method of claim 1 for producing a refined crystalline aluminum ingot without impurities, wherein:
in step S5, the aluminum ingot forming process includes,
step S501, weighing the aluminum ingot blank obtained by the casting molding treatment so as to determine whether the aluminum ingot blank meets the preset weight requirement;
step S502, label printing and outer packaging treatment are carried out on the aluminum ingot blank meeting the preset weight requirement, and therefore the grain-refined aluminum ingot finished product without impurities is obtained.
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