CN1936085B - Method for preparing aluminium and aluminium alloy by low temperature molten-salt electrolysis - Google Patents
Method for preparing aluminium and aluminium alloy by low temperature molten-salt electrolysis Download PDFInfo
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- CN1936085B CN1936085B CN2006100478095A CN200610047809A CN1936085B CN 1936085 B CN1936085 B CN 1936085B CN 2006100478095 A CN2006100478095 A CN 2006100478095A CN 200610047809 A CN200610047809 A CN 200610047809A CN 1936085 B CN1936085 B CN 1936085B
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Abstract
The invention relates to a low temperature salt smelting electrolytic preparation aluminum and aluminum alloy that uses metal chloride or metal chloride mixture as electrolyte that has melting point lower than 800 degree centigrade, uses carbon material or noble electrode as anode, puts cathode on the bottom of graphitic cell groove and puts electrolyte on the upper of cathode, electrifying and heating, after electrolyte smelting, inserting the anode into molten salt, taking fusion electrolysis under the conditions of over A1203 decomposition voltage and lower electrolyte decomposition voltage, inter-pole gap over 0.1cm, temperature below 800 degree centigrade, electrolyzing to current lower than 1.0A, taking out cathode into smelter, smelting aluminum and casting under the condition of over 660 degree centigrade; using liquid aluminum and alumina mixture as cathode electrolyzing, and the temperature is over 660 degree centigrade, taking out aluminum from cathode, adding alumina, continuously taking electrolyzing process. The method sharply decreases electrolyzing temperature and saves electric energy.
Description
Technical field
The present invention relates to electrolysis legal system aluminum technology field, be specifically related to the method for a kind of low-temperature molten salt electrolytic preparation aluminium and aluminium alloy.
Background technology
Aluminium is important metal, and its output is only second to iron and steel, is second largest metallic substance, and China is the first product aluminium big country.Industrial metallic aluminium adopts fused salt electrolysis process production, and take aluminium oxide as raw material, ice crystal is flux and electrolyte, and aluminium liquid is negative electrode, and carbon materials is anode, and electrolysis temperature is 950 ℃, and aluminium is separated out at negative electrode in the electrolytic process, and anode is separated out oxygen and generated CO with the carbon reaction again
2Emit with CO.The shortcoming of this method is that electrolysis temperature height, power consumption are big.Therefore, people are seeking the method for low-temperature molten salt electrolytic preparation metallic aluminium always.
Summary of the invention
At the weak point of existing molten salt electrolysis aluminum technology, the invention provides the method for a kind of low-temperature molten salt electrolytic preparation aluminium and aluminium alloy.
The inventive method is an ionogen with metal chloride or metal chloride mixture, for example: NaCl and CaCl
2Or NaCl and BaCl
2Or CaCl
2With BaCl
2Mixture or pure CaCl
2Deng.Requirement ionogen fusing point≤800 ℃, the metal chloride or the metal chloride mixture that satisfy this condition all can be used as ionogen.When producing aluminium, with solid Al
2O
3Or solid aluminum, charcoal and solid-state Al
2O
3Mixture or liquid aluminium and solid-state Al
2O
3Mixture is negative electrode, and carbon element of graphite material or inert electrode are anode.With the electrolytic technology of solid state cathode is the intermittent type electrolysis.Negative electrode is placed on graphitic cell bottom, electrolyte is placed on negative electrode top, the energising heating behind the electrolyte melting, is inserted fused salt with anode, greater than Al
2O
3Decomposition voltage is less than carrying out molten-salt electrolysis under electrolyte decomposition voltage, die opening 〉=0.1cm, 600 ℃ of conditions of temperature, and electrolysis to electric current is lower than 1.0 amperes and finishes electrolysis.Take out then negative electrode and put into smelting furnace, ingot casting behind melting aluminum under ℃ condition of temperature 〉=660; With liquid aluminium and Al
2O
3Mixture is that catholyte is the continous way electrolysis.Aluminium can regularly be taken out from negative electrode in temperature 〉=660 ℃, adds Al
2O
3, electrolytic process carries out continuously.Intermittent type and continous way electrolytic process negative electrode precipitating metal aluminium, carbon annode produces carbon monoxide and carbonic acid gas, and the inert material anode produces oxygen.
Electrolyte of the present invention adopts the conventional method dehydration to make.Solid state cathode is with solid Al
2O
3At 10MPa～150MPa pressure lower lock block, sintering is made under 1000～1200 ℃ of air, or with solid aluminum (0～15%), charcoal (0～10%) and solid-state Al
2O
3Mix by the quality proportioning (80～100%), under the no oxygen condition, make through 1000～1200 ℃ of sintering, sintering time take guarantee solid state cathode when the electrolysis not efflorescence as principle; Liquid cathode is with liquid aluminium and solid-state Al
2O
3(addition is not to affect conduction as principle) mixture is as negative electrode.
During the preparation aluminium alloy, solid state cathode is with metal oxide and Al as the alloy constituent element
2O
3Mixing, briquetting, in air atmosphere behind 1000～1200 ℃ of sintering as negative electrode, or will mix with metallic aluminium as the metal oxide of alloy constituent element, briquetting, reducing atmosphere below 1000～1200 ℃ behind the sintering as negative electrode, or as the metal oxide of alloy constituent element, with Al
2O
3And the metallic aluminium mixing, perhaps with Al
2O
3And after the carbon mixing, briquetting, 100～1200 ℃ of sintering of reducing atmosphere as negative electrode, or will be as metal oxide and the Al of alloy constituent element
2O
3And behind metallic aluminium and carbon mixing, briquetting, 1000～1200 ℃ of sintering of reducing atmosphere as negative electrode, sintering time take guarantee solid state cathode when the electrolysis not efflorescence as principle; Liquid cathode is to be negative electrode with metal oxide and liquid aluminium mixture as the alloy constituent element; Or as metal oxide and the solid-state Al of alloy constituent element
2O
3And the liquid aluminium mixture is negative electrode, or as metal oxide and the Al of alloy constituent element
2O
3The adding liquid aluminium is negative electrode.All the other methods are the same.For example add the metal oxide TiO as the alloy constituent element
2, SrO, Sc
2O
3, Li
2O, ZrO
2Deng alloys such as preparation Al-Ti, Al-Sr, Al-Sc, Al-Li, Al-Zr, add the rare earth oxide La as the alloy constituent element
2O
3, Ce
2O
3, Er
2O
3Deng alloys such as preparation Al-La, Al-Ce, Al-Er, cathode material requires according to the stoichiometric proportion proportioning according to alloying component.
The inventive method has reduced electrolysis temperature significantly being lower than 800 ℃ of temperature ranges production metallic aluminiums, aluminium alloy, saves electric energy.By chemical analysis product is analyzed, the aluminum or aluminum alloy of production meets national standard.
Embodiment
Embodiment 1
With 2 kilograms of Al
2O
3At 30MPa pressure lower lock block, normal pressure, protective atmosphere, 1000 ℃, 10 hours sintering (perhaps 1100 ℃ of sintering are 8 hours, and perhaps 1200 ℃ of sintering are 6 hours) are made negative electrode, and negative electrode is placed on the graphitic cell bottom; NaCl-CaCl
2Be to mix 1 kilogram at 1: 1 according to mol ratio, electrolyte is made in dehydration, is put into cathode block top; Energising is heated to 600 ℃, behind the electrolyte melting, graphite anode is inserted fused salt, distance-aluminium oxide negative electrode 0.3cm place, and the 3.2V electrolysis is pressed in energising, and electrolysis is lower than 1.0 amperes to electric current.Take out negative electrode and put into smelting furnace, ingot casting after 660 ℃ of fusings.By chemical analysis, aluminium purity is more than 99% in the product.
Embodiment 2
At 2 kilograms of Al
2O
3In add 50 gram metallic aluminium particles, 130MPa pressure briquetting, normal pressure, protective atmosphere, 1000 ℃, 10 hours sintering (perhaps 1100 ℃ of sintering are 8 hours, and perhaps 1200 ℃ of sintering are 6 hours) are made negative electrode, and negative electrode is placed on the graphitic cell bottom; NaCl-CaCl
2Be to mix 1 kilogram at 1: 1 according to mol ratio, electrolyte is made in dehydration, is put into cathode block top; Energising is heated to 600 ℃, behind the electrolyte melting, graphite anode is inserted fused salt, distance-aluminium oxide negative electrode 0.3cm place, and the 3.2V electrolysis is pressed in energising, and electrolysis is lower than 1.0 amperes to electric current.Take out negative electrode and put into smelting furnace, ingot casting after 660 ℃ of fusings.By chemical analysis, aluminium purity is more than 99% in the product.
Embodiment 3
At 2 kilograms of Al
2O
3In add 50 gram charcoal particles, 80MPa pressure briquetting, normal pressure, protective atmosphere, 1000 ℃, 10 hours sintering (perhaps 1100 ℃ of sintering are 8 hours, and perhaps 1200 ℃ of sintering are 6 hours) are made negative electrode, and negative electrode is placed on the graphitic cell bottom; NaCl-CaCl
2Be to mix 1 kilogram at 1: 1 according to mol ratio, electrolyte is made in dehydration, is put into cathode block top; Energising is heated to 600 ℃, behind the electrolyte melting, graphite anode is inserted fused salt, distance-aluminium oxide negative electrode 0.3cm place, and the 3.2V electrolysis is pressed in energising, and electrolysis is lower than 1.0 amperes to electric current.Take out negative electrode and put into smelting furnace, ingot casting after 660 ℃ of fusings.By chemical analysis, aluminium purity is more than 99% in the product.
Embodiment 4
At 2 kilograms of Al
2O
3Middle 50 gram metallic aluminium particles and the 50 gram charcoal particles of adding, 30MPa pressure briquetting, normal pressure, (perhaps 1100 ℃ of sintering are 8 hours for protective atmosphere, 1000 ℃, 10 hours sintering, perhaps 1200 ℃ of sintering are 6 hours) make negative electrode, negative electrode is placed on the graphitic cell bottom; NaCl-CaCl
2Be to mix 1 kilogram at 1: 1 according to mol ratio, electrolyte is made in dehydration, is put into cathode block top; Energising is heated to 600 ℃, behind the electrolyte melting, graphite anode is inserted fused salt, distance-aluminium oxide negative electrode 0.3cm place, and the 3.2V electrolysis is pressed in energising, and electrolysis is lower than 1.0 amperes to electric current.Take out negative electrode and put into smelting furnace, ingot casting after 660 ℃ of fusings.By chemical analysis, aluminium purity is more than 99% in the product.
Embodiment 5
By quality proportioning solid aluminum 6%, charcoal 4% and solid-state Al
2O
390% mixes, 30MPa pressure briquetting, and normal pressure, protective atmosphere, 1000 ℃, 10 hours sintering (perhaps 1100 ℃ of sintering are 8 hours, and perhaps 1200 ℃ of sintering are 6 hours) are made negative electrode, and negative electrode is placed on the graphitic cell bottom; NaCl-CaCl
2Be to mix 1 kilogram at 1: 1 according to mol ratio, electrolyte is made in dehydration, is put into cathode block top; Energising is heated to 600 ℃, behind the electrolyte melting, graphite anode is inserted fused salt, distance-aluminium oxide negative electrode 0.3cm place, and the 3.2V electrolysis is pressed in energising, and electrolysis is lower than 1.0 amperes to electric current.Take out negative electrode and put into smelting furnace, ingot casting after 660 ℃ of fusings.By chemical analysis, aluminium purity is more than 99% in the product.
Embodiment 6
By quality proportioning solid aluminum 12%, charcoal 8% and solid-state Al
2O
380% mixes, 30MPa pressure briquetting, and normal pressure, protective atmosphere, 1000 ℃, 10 hours sintering (perhaps 1100 ℃ of sintering are 8 hours, and perhaps 1200 ℃ of sintering are 6 hours) are made negative electrode, and negative electrode is placed on the graphitic cell bottom; NaCl-CaCl
2Be to mix 1 kilogram at 1: 1 according to mol ratio, electrolyte is made in dehydration, is put into cathode block top; Energising is heated to 600 ℃, behind the electrolyte melting, graphite anode is inserted fused salt, distance-aluminium oxide negative electrode 0.3cm place, and the 3.2V electrolysis is pressed in energising, and electrolysis is lower than 1.0 amperes to electric current.Take out negative electrode and put into smelting furnace, ingot casting after 660 ℃ of fusings.By chemical analysis, aluminium purity is more than 99% in the product.
Embodiment 7
2 kilograms of metallic aluminiums are put into the graphitic cell bottom, add 500 gram aluminium oxide, add then 1: 1 NaCl-CaCl of mol ratio
21 kilogram in mixture, energising is heated to 680 ℃, after metallic aluminium, the salt fusing, the graphite anode rod is inserted fused salt, apart from liquid aluminium liquid level 0.5cm place, the 3.3V electrolysis is pressed in energising, and electrolysis is after 8 hours, by the ceramic funnel that is inserted on the negative electrode aluminium liquid liquid level alumina powder is added in the aluminium liquid, carries out continuous electrolysis.Add 500 gram aluminum oxide powders every 8 hours, adopt the siphon method that the aluminium in the negative electrode is taken out ingot casting simultaneously, make metallic aluminium.By chemical analysis, aluminium purity is more than 99% in the product.
Embodiment 8
Change the aluminum oxide in preparation metallic aluminium embodiment 1 or 2 mixture of aluminum oxide and strontium oxide into, total aluminium strontium amount of substance ratio is 1: 1 (also can according to objective requirement proportioning aluminium strontium), carries out electrolysis by its program.By chemical analysis, the content of aluminium and strontium is more than 99% in the product.
Embodiment 9
Change the aluminum oxide among the preparation metallic aluminium embodiment 5 mixture of aluminum oxide and Scium trioxide into, join in the metal aluminium liquid, total aluminium scandium amount of substance ratio is 1: 1 (also can according to objective requirement proportioning aluminium scandium), carries out electrolysis by its program.By chemical analysis, the content of aluminium and scandium is more than 99% in the product.
Embodiment 10
Change aluminum oxide in preparation metallic aluminium embodiment 1 or 2 mixture of aluminum oxide and titanium dioxide into, total aluminium titanium amount of substance ratio is 3: 1 (also can according to objective requirement proportioning aluminium titanium), carries out electrolysis by its program.By chemical analysis, the content of aluminium and titanium is more than 99% in the product.
Embodiment 11
Change the aluminum oxide among the preparation metallic aluminium embodiment 5 mixture of aluminum oxide and Erbium trioxide into, join in the metal aluminium liquid, total aluminium erbium amount of substance ratio is 1: 1 (also can according to objective requirement proportioning aluminium erbium), carries out electrolysis by its program.By chemical analysis, the content of aluminium and erbium is more than 99% in the product.
Embodiment 12
Change the aluminum oxide among the preparation metallic aluminium embodiment 5 mixture of aluminum oxide and lanthanum trioxide into, join in the metal aluminium liquid, the mass ratio of total aluminium lanthanum is 1: 1 (also can according to objective requirement proportioning aluminium lanthanum), carries out electrolysis by its program.By chemical analysis, the content of aluminium and lanthanum is more than 99% in the product.
Embodiment 13
Change the aluminum oxide among the preparation metallic aluminium embodiment 5 into aluminum oxide and zirconic mixture, join in the metal aluminium liquid, the amount ratio of total aluminium zirconium material is 1: 1 (also can according to objective requirement proportioning aluminium zirconium), carries out electrolysis by its program.By chemical analysis, the content of aluminium and zirconium is more than 99% in the product.
Embodiment 14
Change aluminum oxide in preparation metallic aluminium embodiment 1 or 2 mixture of aluminum oxide and Lithium Oxide 98min into, total aluminium lithium amount of substance ratio is 1: 1 (also can according to objective requirement proportioning aluminium lithium), carries out electrolysis by its program.By chemical analysis, the content of aluminium and lithium is more than 99% in the product.
Embodiment 15
Change the aluminum oxide among the preparation metallic aluminium embodiment 5 mixture of aluminum oxide and tantalum oxide into, join in the metal aluminium liquid, total aluminium tantalum amount of substance ratio is 1: 1 (also can according to objective requirement proportioning aluminium tantalum), carries out electrolysis by its program.By chemical analysis, the content of aluminium and tantalum is more than 99% in the product.
Embodiment 16
Change aluminum oxide in preparation metallic aluminium embodiment 1 or 2 mixture of aluminum oxide and niobium oxides into, total aluminium niobium amount of substance ratio is 1: 1 (also can according to objective requirement proportioning aluminium niobium), carries out electrolysis by its program.By chemical analysis, the content of aluminium and niobium is more than 99% in the product.
Embodiment 17
Change the aluminum oxide among the preparation metallic aluminium embodiment 5 mixture of aluminum oxide and dysprosium oxide into, join in the metal aluminium liquid, total aluminium dysprosium amount of substance ratio is 1: 1 (also can according to objective requirement proportioning aluminium dysprosium), carries out electrolysis by its program.By chemical analysis, the content of aluminium and dysprosium is more than 99% in the product.
Claims (5)
1. a low temperature molten salt electrolysis prepares the method for aluminium and aluminium alloy, it is characterized in that mixing in 1: 1 in molar ratio with metal sodium chloride and metal calcium chloride, electrolyte is made in dehydration, and carbon element of graphite material or inert electrode are anode, is the batch (-type) electrolysis with the technology of solid state cathode electrolysis, negative electrode is placed on the graphitic cell bottom, electrolyte is placed on negative electrode top, and the energising heating is behind the electrolyte melting, anode is inserted fused salt, greater than Al
2O
3Decomposition voltage is less than carrying out molten-salt electrolysis under electrolyte decomposition voltage, die opening 〉=0.1cm, 600 ℃ of conditions of temperature, and electrolysis to electric current is lower than 1.0 amperes and finishes electrolysis, takes out then negative electrode and puts into smelting furnace, ingot casting behind melting aluminum under ℃ condition of temperature 〉=660; With liquid aluminium and Al
2O
3Mixture is that catholyte is the continous way electrolysis, and aluminium is regularly taken out from negative electrode in temperature 〉=660 ℃, adds Al
2O
3, electrolytic process carries out continuously; When producing aluminium, with solid Al
2O
3, or solid aluminum, charcoal and solid-state Al
2O
3Mixture, or liquid aluminium and solid-state Al
2O
3Mixture is negative electrode; During the preparation aluminium alloy, will be as metal oxide and the Al of alloy constituent element
2O
3Be mixed and made into negative electrode, or will be mixed and made into negative electrode as metal oxide and the metallic aluminium of alloy constituent element, or will be as the metal oxide of alloy constituent element, with Al
2O
3And the metallic aluminium mixing, perhaps with Al
2O
3And the carbon mixing, make negative electrode, or will be as metal oxide and the Al of alloy constituent element
2O
3Reach metallic aluminium and carbon and be mixed and made into negative electrode; When adopting liquid cathode, be to be negative electrode with metal oxide and liquid aluminium mixture as the alloy constituent element; Or as metal oxide and the solid-state Al of alloy constituent element
2O
3And liquid aluminium is mixed into negative electrode.
2. the method for preparing aluminium and aluminium alloy according to the described low temperature molten salt electrolysis of claim 1 is when is characterized in that producing aluminium, when with solid aluminum, charcoal and solid-state Al
2O
3When mixture is negative electrode, be solid aluminum 0～15%, charcoal 0～10% and solid-state Al by the quality proportioning
2O
380～100%.
3. prepare the method for aluminium and aluminium alloy according to claim 1 or 2 described low temperature molten salt electrolysis, solid state cathode is with solid Al when it is characterized in that producing aluminium
2O
3At 10MPa～150MPa lower lock block, sintering is made under 1000～1200 ℃ of air, or with solid aluminum, charcoal and solid-state Al
2O
3Mix by proportioning, under the no oxygen condition, make through 1000～1200 ℃ of sintering; Liquid cathode is with liquid aluminium and solid-state Al
2O
3Mixture is negative electrode.
4. the method for preparing aluminium and aluminium alloy according to the described low temperature molten salt electrolysis of claim 1, when it is characterized in that preparing aluminium alloy, will be as metal oxide and the Al of alloy constituent element
2O
3Mixing, briquetting, in air atmosphere behind 1000～1200 ℃ of sintering as negative electrode; Or will mix with metallic aluminium as the metal oxide of alloy constituent element, briquetting, reducing atmosphere below 1000～1200 ℃ behind the sintering as negative electrode; Or will be as the metal oxide of alloy constituent element, with Al
2O
3And the metallic aluminium mixing, perhaps with Al
2O
3And after the carbon mixing, briquetting, 1000～1200 ℃ of sintering of reducing atmosphere as negative electrode; Or will be as metal oxide and the Al of alloy constituent element
2O
3And behind metallic aluminium and carbon mixing, briquetting, 1000～1200 ℃ of sintering of reducing atmosphere as negative electrode, cathode material requires according to the stoichiometric proportion proportioning according to alloying component.
5. prepare the method for aluminium and aluminium alloy according to claim 1 or 4 described low temperature molten salt electrolysis, it is characterized in that adding the metal oxide TiO as the alloy constituent element
2, SrO, Sc
2O
3, Li
2O, ZrO
2Preparation Al-Ti, Al-Sr, Al-Sc, Al-Li, Al-Zr alloy add the rare earth oxide La as the alloy constituent element
2O
3, Ce
2O
3, Er
2O
3Preparation Al-La, Al-Ce, Al-Er alloy, cathode material requires according to the stoichiometric proportion proportioning according to alloying component.
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|---|---|---|---|
| CN2006100478095A CN1936085B (en) | 2006-09-19 | 2006-09-19 | Method for preparing aluminium and aluminium alloy by low temperature molten-salt electrolysis |
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|---|---|---|---|
| CN2006100478095A CN1936085B (en) | 2006-09-19 | 2006-09-19 | Method for preparing aluminium and aluminium alloy by low temperature molten-salt electrolysis |
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| CN1936085B true CN1936085B (en) | 2010-04-14 |
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Cited By (1)
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| CN1936085A (en) | 2007-03-28 |
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