CN109735873A - A kind of production technology of high-quality aluminium ingot - Google Patents
A kind of production technology of high-quality aluminium ingot Download PDFInfo
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- CN109735873A CN109735873A CN201910224718.1A CN201910224718A CN109735873A CN 109735873 A CN109735873 A CN 109735873A CN 201910224718 A CN201910224718 A CN 201910224718A CN 109735873 A CN109735873 A CN 109735873A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 175
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 175
- 239000004411 aluminium Substances 0.000 title claims abstract description 74
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 39
- 238000005516 engineering process Methods 0.000 title claims abstract description 21
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 105
- 238000005266 casting Methods 0.000 claims abstract description 47
- 239000003792 electrolyte Substances 0.000 claims abstract description 39
- 239000000843 powder Substances 0.000 claims abstract description 31
- 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 27
- 238000007670 refining Methods 0.000 claims abstract description 27
- 238000007872 degassing Methods 0.000 claims abstract description 26
- 238000012545 processing Methods 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 23
- 239000012535 impurity Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 16
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims abstract description 11
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000004806 packaging method and process Methods 0.000 claims abstract description 6
- 238000012805 post-processing Methods 0.000 claims abstract description 6
- 210000004027 cell Anatomy 0.000 claims description 42
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 238000002844 melting Methods 0.000 claims description 22
- 230000008018 melting Effects 0.000 claims description 22
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 18
- 239000004615 ingredient Substances 0.000 claims description 16
- 238000004458 analytical method Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 238000005070 sampling Methods 0.000 claims description 11
- 229910000521 B alloy Inorganic materials 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000002826 coolant Substances 0.000 claims description 10
- 239000006260 foam Substances 0.000 claims description 10
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- 238000000354 decomposition reaction Methods 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 5
- 239000002362 mulch Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 239000002893 slag Substances 0.000 claims description 5
- 235000013024 sodium fluoride Nutrition 0.000 claims description 5
- 239000011775 sodium fluoride Substances 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- 229910052720 vanadium Inorganic materials 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 238000003682 fluorination reaction Methods 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 19
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 description 14
- 238000005204 segregation Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 241000894007 species Species 0.000 description 4
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 3
- 241000720974 Protium Species 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 231100001010 corrosive Toxicity 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
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- Electrolytic Production Of Metals (AREA)
Abstract
The invention discloses a kind of production technologies of high-quality aluminium ingot, select including 1. raw material: determining the impurity content in alumina powder；2. preparing electrolyte: aluminum fluoride, calcirm-fluoride and lithium fluoride is added into ice crystal and is configured to electrolyte；3. electrolysis: electrolysis production high-temperature electrolysis molten aluminum；4. refining: the high-temperature electrolysis molten aluminum that electrolysis is generated carries out high melt；5. post-processing: high-temperature electrolysis molten aluminum being transferred in chute, then carries out crystal grain refinement processing, online degassing processing and on-line filtration to high-temperature electrolysis molten aluminum, obtains molten aluminum melt；6. casting: molten aluminum melt being cast online using casting machine, casting forms aluminium ingot casting；7. being packaged: by aluminium ingot casting after on-line cooling, high-quality aluminium ingot can be obtained after carrying out sawing, bundling, packaging.The present invention has the advantages that technology controlling and process is simple, production cost is low, high production efficiency, pollution are small, and, purity is high stable using quality of ingot aluminum produced by the present invention, purity can reach 99.8% or more.
Description
Technical field
The invention belongs to aluminum electrolysis production technique technical fields, and in particular to a kind of production technology of high-quality aluminium ingot.
Background technique
Rafifinal plays more and more important work in some high-new industries due to many special performances having
With being usually used in holding some strong corrosives acid using the container that its acidresistant property makes, utilize ductility and good conductivity
Characteristic, it is 15 μm of filament that rafifinal, which can be drawn into diameter, is widely used in integrated circuits as wiring, together
When, rafifinal has preferable low-temperature conductive performance, for collecting the high energy ion energies such as the magnetic wave beam in space as promotion
In addition, rafifinal is also widely used " solar sail " of spacecraft movement in sputtering target material market, electronics industry.
The three-layer liquid electrolysis method that aluminium purifying industrial stock was invented in American in 1901.1970s, with the development of technology and
Raising of the people to environmental requirement, the developed countries such as Japan, France have developed the segregation method of relatively advanced environmental protection, segregation method root
According to the segregation phenomena in metal solidification process, realize that the purpose of purification, energy consumption are far below three-layer liquid method using physical method.China
Fine aluminium industry start from first Fushun Aluminium Works, aluminium manufacturer, country in 1958, build up first three-layer liquid electrolysis method production line.Relative to
Lag is compared in the fine aluminium industry starting evening in China, developed country, development, and three-layer liquid electrolysis method is still the main manufacturer of fine aluminium
Method.China currently has some producers to produce fine aluminium with segregation method, but due to block of foreign technology etc., product purity does not have
Have and reaches satisfactory result.The rafifinal yield in China and domestic demand amount difference are larger, and aluminium produces for over ten years with China
Amount is unbecoming in status is held a safe lead, and since investment research and development are less, resulting theoretical result is also extremely limited, and is limited high-quality
Amount, high-purity, high benefit product put goods on the market.However, in order to further improve the purity and efficiency of aluminium purification, state
A large amount of research work had also been made in interior many units in recent years, on the basis of traditional three-layer liquid method, segregation method, developed
The production technology that rafifinal is produced using cryolite-alumina fused salt electrolysis process, although the technique theoretically can be real
The production of existing rafifinal, but in actual production process, it is electrolysed the selection of raw material, the material selection of electrolytic cell, anode yin
Selection of pole material etc. can all influence the quality of electrolytic aluminium liquid, and with the extension of electrolysis time, electrolysis needs to consume a large amount of
Anode, the impurity content of anode body can enter electrolytic cell with electrolysis, pollute molten aluminum, it is necessary to frequently replacement sun
Pole, serious influence production efficiency.Therefore, low a kind of simple process, production cost, high production efficiency, purification effect are developed
The production technology of the significant high-quality aluminium ingot of fruit is desirability.
Summary of the invention
In order to solve the problems, such as background technique, the purpose of the present invention is to provide a kind of simple process, it is produced into
This low, high production efficiency, the production technology of the significant high-quality aluminium ingot of refining effect.
The production technology of high-quality aluminium ingot of the present invention, the following steps are included:
1. raw material selects: selective oxidation aluminium powder is less than 100um, alumina powder as raw material, the particle diameter of the alumina powder
Middle SiO2、Fe2O3、Ga2O3、ZnO、TiO2Impurity content is controlled respectively in 80ppm, 80ppm, 50ppm, 5ppm and 40ppm or less；
2. preparing electrolyte: aluminum fluoride being added into ice crystal, makes mole of the sodium fluoride and aluminum fluoride in ice crystal mixture
Than for (2~3): 1, the calcirm-fluoride of mixture quality 2~15% and 2~10% fluorination is then added into ice crystal mixture again
Lithium is configured to electrolyte；
3. electrolysis: first by step 2. electrolyte merging electrolytic cell obtained, the material of electrolytic cell is high purity graphite, by electrolytic cell
940~960 DEG C are heated to, then the alumina powder of electrolyte quality 5~10% is added into electrolytic cell, obtains the mixed of molten condition
Close electrolyte, backward electrolytic cell in be inserted into carbon anode, and cell surface and carbon anode surface are carried out with mulch is kept the temperature
Covering, is then passed through direct current into electrolytic cell, decomposition voltage is 3.8~4.2V, Faradaic current is 18~22A, electric current is close
Degree is 0.5~1A/cm3Under conditions of be electrolysed 1~2h, be added later every 10~15min into electrolytic cell electrolyte quality 5~
10% alumina powder is electrolysed, electrolysis production high-temperature electrolysis molten aluminum；
4. refining: with the continuous progress of electrolysis, the high-temperature electrolysis molten aluminum that generation is 3. electrolysed through step is continuous using pouring aluminium ladle
After suction then cooling agent is added into high temperature melting furnace, drops the temperature of high-temperature electrolysis molten aluminum into high temperature melting furnace for transport
To 750~780 DEG C, the cooling agent is pure aluminium powder, is passed through nitrogen and refining agent into high temperature melting furnace again later, keeps 750
~780 DEG C of temperature carries out high melt to high-temperature electrolysis molten aluminum, is sampled after 15~20min of melting to high-temperature electrolysis molten aluminum
Analysis, is adjusted each ingredient of the underproof high-temperature electrolysis molten aluminum of sampling analysis, each ingredient is made to reach preset content；
5. post-processing: the high-temperature electrolysis molten aluminum after 4. sampling analysis is qualified through step being first transferred to chute from high temperature melting furnace
It is interior, crystal grain refinement processing, AL-Ti-B alloy wire then are carried out to high-temperature electrolysis molten aluminum using AL-Ti-B alloy wire in chute
Dosage be 2~3kg/t.AL, online degassing processing and on-line filtration are carried out to high-temperature electrolysis molten aluminum again later, obtains meeting and pour
The molten aluminum melt of casting；
6. casting: the molten aluminum melt 5. handled through step to be cast online using casting machine, casting forms aluminium ingot casting,
The temperature cast online is 710~720 DEG C, and the speed of casting is 35~45m/min；
7. being packaged: 6. step being obtained to aluminium ingot casting after on-line cooling, Gao Pin can be obtained after carrying out sawing, bundling, packaging
Matter aluminium ingot.
Further, step 3. in, the content of Si, Fe, Ni, Ga, V, Ti, Zn impurity in the carbon anode exists respectively
200ppm, 200 ppm, 100 ppm, 80 ppm, 50 ppm, 10 ppm and 8ppm or less.
Further, step 3. in, when electrolysis production high-temperature electrolysis molten aluminum, electrolyte level control in 16~19cm,
The flat control of aluminum water is in 28~32cm.
Further, step 4. in, to high-temperature electrolysis molten aluminum carry out composition detection when, it is desirable that high-temperature electrolysis molten aluminum
Each composition range (wt.%) is AL:99.50~99.99, Si≤0.10, Fe≤0.10, impurity summation≤0.30.
Further, step 4. in, be passed through nitrogen and refining agent refining be blown into 0.3 in high melt furnace bottom~
The nitrogen and sodium chloride that 0.5MPa purity is 99.9%, sodium chloride dosage are 1~3kg/t.AL, and the slag inclusion removed in melt is gentle
Body.
Further, step 5. in, the gaseous species of online degassing processing are N2-CL2Mixed gas, and N2-CL2It is mixed
The air pressure for closing gas is 0.3~0.5MPa, and the equipment of online degassing processing is rotary degassing device, the rotor of rotary degassing device
Revolving speed is 300~500rpm.
Further, step 5. in, on-line filtration uses foam ceramic filter, and the mesh diameter of foam ceramic filter is 0.2
~0.8mm.
Further, step 7. in, in such a way that cool water shower is cooling, the flow of cooling water is on-line cooling
100~150m3/min。
The beneficial effect comprise that: first is that the present invention has carried out strictly the component content of aluminium oxide from source
Control, improve good raw material to improve the quality of electrolytic aluminium liquid and guarantee；Second is that optimizing the composition of raw materials of electrolyte, it is
Aluminium electroloysis provides good technical conditions, can guarantee that preferable aluminium electroloysis is horizontal；Third is that stringent controls aluminium oxide electricity
Process conditions in solution preocess can not only significantly improve the quality of electrolytic aluminium liquid, and can reduce the consumption of anode carbon block；
Fourth is that by carrying out crystal grain refinement processing to the electrolytic aluminium liquid after refining, it is able to solve that oxidation impurities in electrolytic aluminium liquid are more, hydrogen contains
Measure high problem, by after line degassing processing and on-line filtration processing can further improve the product of electrolytic aluminium liquid
Matter, and then improve the purity and quality of aluminium ingot after casting.The present invention is with technology controlling and process is simple, production cost is low, production efficiency
Advantage high, pollution is small, purity is high stable using quality of ingot aluminum produced by the present invention, purity can reach 99.8% or more, more
Add and meets the development of today's society and the development of enterprise.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but the present invention is limited in any way,
Based on present invention teach that it is made it is any transform or replace, all belong to the scope of protection of the present invention.
Embodiment 1
1. raw material selects: for selective oxidation aluminium powder as raw material, the particle diameter of the alumina powder is 99um, in alumina powder
SiO2、Fe2O3、Ga2O3、ZnO、TiO2Impurity content is controlled respectively in 78ppm, 78ppm, 40ppm, 4ppm and 38ppm；
2. preparing electrolyte: aluminum fluoride being added into ice crystal, makes mole of the sodium fluoride and aluminum fluoride in ice crystal mixture
Than the calcirm-fluoride of mixture quality 2% being then added into ice crystal mixture again and 10% lithium fluoride is configured to for 2~3:1
Electrolyte；
3. electrolysis: first by step 2. electrolyte merging electrolytic cell obtained, the material of electrolytic cell is high purity graphite, by electrolytic cell
940 DEG C are heated to, then the alumina powder of electrolyte quality 5% is added into electrolytic cell, obtains the mixed electrolyte of molten condition,
Backward electrolytic cell in be inserted into carbon anode, and cell surface and carbon anode surface are covered with heat preservation mulch, it is described
The content of Si, Fe, Ni, Ga, V, Ti, Zn impurity in carbon anode is respectively in 180ppm, 180 ppm, 80 ppm, 79ppm, 40
Ppm, 9 ppm, 7ppm, control the component content of carbon anode, also have certain effect to the component content in control electrolytic aluminium liquid,
Then direct current is passed through into electrolytic cell, decomposition voltage be 3.8V, Faradaic current 18A, current density 0.5A/cm3's
Under the conditions of be electrolysed 1h, the alumina powder that electrolyte quality 5% is added into electrolytic cell every 10min later is electrolysed, electrolysis life
High-temperature electrolysis molten aluminum is produced, when electrolysis production high-temperature electrolysis molten aluminum, electrolyte level control is in 16cm, and the flat control of aluminum water is in 28cm；
4. refining: with the continuous progress of electrolysis, the high-temperature electrolysis molten aluminum that generation is 3. electrolysed through step is continuous using pouring aluminium ladle
After suction then cooling agent is added into high temperature melting furnace, drops the temperature of high-temperature electrolysis molten aluminum into high temperature melting furnace for transport
To 750 DEG C, the cooling agent is pure aluminium powder, is passed through nitrogen and refining agent into high temperature melting furnace again later, is passed through nitrogen and essence
Refining agent refining is to be blown into the nitrogen and sodium chloride that 0.3MPa purity is 99.9% in high melt furnace bottom, and sodium chloride dosage is
1kg/t.AL removes slag inclusion and gas in melt, and 750 DEG C of temperature is kept to carry out high melt to high-temperature electrolysis molten aluminum, melts
Analysis is sampled to high-temperature electrolysis molten aluminum after refining 15min, when carrying out composition detection to high-temperature electrolysis molten aluminum, it is desirable that high-temperature electric
Solve molten aluminum each composition range (wt.%) be AL:99.50~99.99, Si≤0.10, Fe≤0.10, impurity summation≤0.30, it is right
Each ingredient of the underproof high-temperature electrolysis molten aluminum of sampling analysis is adjusted, and each ingredient is made to reach preset content；
5. post-processing: the high-temperature electrolysis molten aluminum after 4. sampling analysis is qualified through step being first transferred to chute from high temperature melting furnace
It is interior, crystal grain refinement processing, AL-Ti-B alloy wire then are carried out to high-temperature electrolysis molten aluminum using AL-Ti-B alloy wire in chute
Dosage be 2kg/t.AL, online degassing processing and on-line filtration are carried out to high-temperature electrolysis molten aluminum again later, obtain meeting casting
Molten aluminum melt, the gaseous species of online degassing processing are N2-CL2Mixed gas, and N2-CL2The air pressure of mixed gas is
0.3MPa, the equipment of online degassing processing are rotary degassing device, and the rotor speed of rotary degassing device is 300rpm,；
6. casting: the molten aluminum melt 5. handled through step to be cast online using casting machine, casting forms aluminium ingot casting,
The temperature cast online is 710 DEG C, and the speed of casting is 35m/min, and on-line filtration uses foam ceramic filter, foam ceramic filter
Mesh diameter is 0.2mm；
7. being packaged: 6. step being obtained to aluminium ingot casting after on-line cooling, Gao Pin can be obtained after carrying out sawing, bundling, packaging
Matter aluminium ingot, for on-line cooling in such a way that cool water shower is cooling, the flow of cooling water is 100m3/min。
The present embodiment 1 does certain control requirement to the impurity element for influencing molten aluminum quality in electrolysis raw material, i.e. control oxygen
Change the ingredient of aluminum feedstock, electrolyte ingredient and carbon anode, and with after reasonable electrolysis process and refinery practice cooperation, can produce
High-temperature electrolysis molten aluminum of the purity 99.89% or more out, high-temperature electrolysis molten aluminum after post treatment after, can thoroughly eliminate high temperature
The oxide being mingled with and protium in electrolytic aluminium liquid etc. are able to produce out high-quality after the casting of dedicated casting machine
Aluminium ingot, purity is high stable using quality of ingot aluminum made from embodiment 1, purity can reach 99.91%.
Embodiment 2
1. raw material selects: for selective oxidation aluminium powder as raw material, the particle diameter of the alumina powder is 50um, in alumina powder
SiO2、Fe2O3、Ga2O3、ZnO、TiO2Impurity content is controlled respectively in 50ppm, 50ppm, 25ppm, 3ppm and 30ppm；
2. preparing electrolyte: aluminum fluoride being added into ice crystal, makes mole of the sodium fluoride and aluminum fluoride in ice crystal mixture
Than the calcirm-fluoride of mixture quality 10% being then added into ice crystal mixture again and 6% lithium fluoride is configured to electricity for 2.5:1
Xie Zhi；
3. electrolysis: first by step 2. electrolyte merging electrolytic cell obtained, the material of electrolytic cell is high purity graphite, by electrolytic cell
950 DEG C are heated to, then the alumina powder of electrolyte quality 6% is added into electrolytic cell, obtains the mixed electrolyte of molten condition,
Backward electrolytic cell in be inserted into carbon anode, the content of Si, Fe, Ni, Ga, V, Ti, Zn impurity in the carbon anode exists respectively,
100ppm, 100 ppm, 50 ppm, 40 ppm, 30 ppm, 2 ppm and 5ppm, and with heat preservation mulch to cell surface and
Carbon anode surface is covered, and direct current is then passed through into electrolytic cell, decomposition voltage be 4V, Faradaic current 20A, electric current
Density is 0.8A/cm3Under conditions of be electrolysed 1.5h, the oxidation of electrolyte quality 6% is added into electrolytic cell every 13min later
Aluminium powder is electrolysed, electrolysis production high-temperature electrolysis molten aluminum, and when electrolysis production high-temperature electrolysis molten aluminum, electrolyte level control exists
17.5cm, the flat control of aluminum water is in 30cm；
4. refining: with the continuous progress of electrolysis, the high-temperature electrolysis molten aluminum that generation is 3. electrolysed through step is continuous using pouring aluminium ladle
After suction then cooling agent is added into high temperature melting furnace, drops the temperature of high-temperature electrolysis molten aluminum into high temperature melting furnace for transport
To 765 DEG C, the cooling agent is pure aluminium powder, is passed through nitrogen and refining agent into high temperature melting furnace again later, is passed through nitrogen and essence
Refining agent refining is to be blown into the nitrogen and sodium chloride that 0.3MPa purity is 99.9% in high melt furnace bottom, and sodium chloride dosage is
1kg/t.AL removes slag inclusion and gas in melt, and 765 DEG C of temperature is kept to carry out high melt to high-temperature electrolysis molten aluminum, melts
Analysis is sampled to high-temperature electrolysis molten aluminum after refining 18min, when carrying out composition detection to high-temperature electrolysis molten aluminum, it is desirable that high-temperature electric
Solve molten aluminum each composition range (wt.%) be AL:99.50~99.99, Si≤0.10, Fe≤0.10, impurity summation≤0.30, it is right
Each ingredient of the underproof high-temperature electrolysis molten aluminum of sampling analysis is adjusted, and each ingredient is made to reach preset content；
5. post-processing: the high-temperature electrolysis molten aluminum after 4. sampling analysis is qualified through step being first transferred to chute from high temperature melting furnace
It is interior, crystal grain refinement processing, AL-Ti-B alloy wire then are carried out to high-temperature electrolysis molten aluminum using AL-Ti-B alloy wire in chute
Dosage be 2.5kg/t.AL, online degassing processing and on-line filtration are carried out to high-temperature electrolysis molten aluminum again later, obtains meeting and pour
The molten aluminum melt of casting, the gaseous species of online degassing processing are N2-CL2Mixed gas, and N2-CL2The air pressure of mixed gas is
0.4MPa, the equipment of online degassing processing are rotary degassing device, and the rotor speed of rotary degassing device is 400rpm, online mistake
Filter uses foam ceramic filter, and the mesh diameter of foam ceramic filter is 0.5mm；
6. casting: the molten aluminum melt 5. handled through step to be cast online using casting machine, casting forms aluminium ingot casting,
The temperature cast online is 715 DEG C, and the speed of casting is 40m/min；
7. being packaged: 6. step being obtained to aluminium ingot casting after on-line cooling, Gao Pin can be obtained after carrying out sawing, bundling, packaging
Matter aluminium ingot, for on-line cooling in such a way that cool water shower is cooling, the flow of cooling water is 120m3/min。
The present embodiment 2 does certain control requirement to the impurity element for influencing molten aluminum quality in electrolysis raw material, i.e. control oxygen
Change the ingredient of aluminum feedstock, electrolyte ingredient and carbon anode, and with after reasonable electrolysis process and refinery practice cooperation, can produce
High-temperature electrolysis molten aluminum of the purity 99.95% or more out, high-temperature electrolysis molten aluminum after post treatment after, can thoroughly eliminate high temperature
The oxide being mingled with and protium in electrolytic aluminium liquid etc. are able to produce out high-quality after the casting of dedicated casting machine
Aluminium ingot, purity is high stable using quality of ingot aluminum made from embodiment 2, purity can reach 99.99%.
Embodiment 3
1. raw material selects: for selective oxidation aluminium powder as raw material, the particle diameter of the alumina powder is 20um, in alumina powder
SiO2、Fe2O3、Ga2O3、ZnO、TiO2Impurity content is controlled respectively in 50ppm, 30ppm, 30ppm, 1ppm and 30ppm；
2. preparing electrolyte: aluminum fluoride being added into ice crystal, makes mole of the sodium fluoride and aluminum fluoride in ice crystal mixture
Than the calcirm-fluoride of mixture quality 15% being then added into ice crystal mixture again and 2% lithium fluoride is configured to be electrolysed for 3:1
Matter；
3. electrolysis: first by step 2. electrolyte merging electrolytic cell obtained, the material of electrolytic cell is high purity graphite, by electrolytic cell
960 DEG C are heated to, then the alumina powder of electrolyte quality 10% is added into electrolytic cell, obtains the mixed electrolyte of molten condition,
Backward electrolytic cell in be inserted into carbon anode, the content of Si, Fe, Ni, Ga, V, Ti, Zn impurity in the carbon anode exists respectively
50ppm, 50ppm, 20 ppm, 60ppm, 35 ppm, 1 ppm and 2ppm, and with heat preservation mulch to cell surface and carbon sun
Pole surface is covered, and direct current is then passed through into electrolytic cell, decomposition voltage be 4.2V, Faradaic current 22A, electric current it is close
Degree is 1A/cm3Under conditions of be electrolysed 2h, be added later every 15min into electrolytic cell the alumina powder of electrolyte quality 10% into
Row electrolysis, electrolysis production high-temperature electrolysis molten aluminum, when electrolysis production high-temperature electrolysis molten aluminum, electrolyte level is controlled in 19cm, aluminum water
Flat control is in 32cm；
4. refining: with the continuous progress of electrolysis, the high-temperature electrolysis molten aluminum that generation is 3. electrolysed through step is continuous using pouring aluminium ladle
After suction then cooling agent is added into high temperature melting furnace, drops the temperature of high-temperature electrolysis molten aluminum into high temperature melting furnace for transport
To 780 DEG C, the cooling agent is pure aluminium powder, is passed through nitrogen and refining agent into high temperature melting furnace again later, is passed through nitrogen and essence
Refining agent refining is to be blown into the nitrogen and sodium chloride that 0.5MPa purity is 99.9% in high melt furnace bottom, and sodium chloride dosage is
3kg/t.AL removes slag inclusion and gas in melt, and 780 DEG C of temperature is kept to carry out high melt to high-temperature electrolysis molten aluminum, melts
Analysis is sampled to high-temperature electrolysis molten aluminum after refining 20min, when carrying out composition detection to high-temperature electrolysis molten aluminum, it is desirable that high-temperature electric
Solve molten aluminum each composition range (wt.%) be AL:99.50~99.99, Si≤0.10, Fe≤0.10, impurity summation≤0.30, it is right
Each ingredient of the underproof high-temperature electrolysis molten aluminum of sampling analysis is adjusted, and each ingredient is made to reach preset content；
5. post-processing: the high-temperature electrolysis molten aluminum after 4. sampling analysis is qualified through step being first transferred to chute from high temperature melting furnace
It is interior, crystal grain refinement processing, AL-Ti-B alloy wire then are carried out to high-temperature electrolysis molten aluminum using AL-Ti-B alloy wire in chute
Dosage be 3kg/t.AL, online degassing processing and on-line filtration are carried out to high-temperature electrolysis molten aluminum again later, obtain meeting casting
Molten aluminum melt, the gaseous species of online degassing processing are N2-CL2Mixed gas, and N2-CL2The air pressure of mixed gas is
0.5MPa, the equipment of online degassing processing are rotary degassing device, and the rotor speed of rotary degassing device is 500rpm, online mistake
Filter uses foam ceramic filter, and the mesh diameter of foam ceramic filter is 0.8mm；
6. casting: the molten aluminum melt 5. handled through step to be cast online using casting machine, casting forms aluminium ingot casting,
The temperature cast online is 720 DEG C, and the speed of casting is 45m/min；
7. being packaged: 6. step being obtained to aluminium ingot casting after on-line cooling, Gao Pin can be obtained after carrying out sawing, bundling, packaging
Matter aluminium ingot, for on-line cooling in such a way that cool water shower is cooling, the flow of cooling water is 150m3/min。
The present embodiment 3 does certain control requirement to the impurity element for influencing molten aluminum quality in electrolysis raw material, i.e. control oxygen
Change the ingredient of aluminum feedstock, electrolyte ingredient and carbon anode, and with after reasonable electrolysis process and refinery practice cooperation, can produce
High-temperature electrolysis molten aluminum of the purity 99.9% or more out, high-temperature electrolysis molten aluminum after post treatment after, can thoroughly eliminate high-temperature electric
The oxide being mingled with and the protium etc. in molten aluminum are solved, after the casting of dedicated casting machine, is able to produce out the aluminium of high-quality
Ingot, purity is high stable using quality of ingot aluminum made from embodiment 3, purity can reach 99.93%.
To sum up, the present invention have the advantages that technology controlling and process is simple, production cost is low, high production efficiency, pollution it is small, compared to pass
The purifying technique of system, purification efficiency and refining effect have all obtained significantly improving, and can generate preferable economic benefit and society
Meeting benefit, use easy to spread.
Claims (8)
1. a kind of production technology of high-quality aluminium ingot, which comprises the following steps:
1. raw material selects: selective oxidation aluminium powder is less than 100um, alumina powder as raw material, the particle diameter of the alumina powder
Middle SiO2、Fe2O3、Ga2O3、ZnO、TiO2Impurity content is controlled respectively in 80ppm, 80ppm, 50ppm, 5ppm and 40ppm or less；
2. preparing electrolyte: aluminum fluoride being added into ice crystal, makes mole of the sodium fluoride and aluminum fluoride in ice crystal mixture
Than for (2~3): 1, the calcirm-fluoride of mixture quality 2~15% and 2~10% fluorination is then added into ice crystal mixture again
Lithium is configured to electrolyte；
3. electrolysis: first by step 2. electrolyte merging electrolytic cell obtained, the material of electrolytic cell is high purity graphite, by electrolytic cell
940~960 DEG C are heated to, then the alumina powder of electrolyte quality 5~10% is added into electrolytic cell, obtains the mixed of molten condition
Close electrolyte, backward electrolytic cell in be inserted into carbon anode, and cell surface and carbon anode surface are carried out with mulch is kept the temperature
Covering, is then passed through direct current into electrolytic cell, decomposition voltage is 3.8~4.2V, Faradaic current is 18~22A, electric current is close
Degree is 0.5~1A/cm3Under conditions of be electrolysed 1~2h, be added later every 10~15min into electrolytic cell electrolyte quality 5~
10% alumina powder is electrolysed, electrolysis production high-temperature electrolysis molten aluminum；
4. refining: with the continuous progress of electrolysis, the high-temperature electrolysis molten aluminum that generation is 3. electrolysed through step is continuous using pouring aluminium ladle
After suction then cooling agent is added into high temperature melting furnace, drops the temperature of high-temperature electrolysis molten aluminum into high temperature melting furnace for transport
To 750~780 DEG C, the cooling agent is pure aluminium powder, is passed through nitrogen and refining agent into high temperature melting furnace again after aluminium ingot, is kept
750~780 DEG C of temperature carries out high melt to high-temperature electrolysis molten aluminum, carries out after 15~20min of melting to high-temperature electrolysis molten aluminum
Sampling analysis is adjusted each ingredient of the underproof high-temperature electrolysis molten aluminum of sampling analysis, so that each ingredient is reached preset and contain
Amount；
5. post-processing: the high-temperature electrolysis molten aluminum after 4. sampling analysis is qualified through step being first transferred to chute from high temperature melting furnace
It is interior, crystal grain refinement processing, AL-Ti-B alloy wire then are carried out to high-temperature electrolysis molten aluminum using AL-Ti-B alloy wire in chute
Dosage be 2~3kg/t.AL, online degassing processing and on-line filtration are carried out to high-temperature electrolysis molten aluminum again later, obtains meeting and pour
The molten aluminum melt of casting；
6. casting: the molten aluminum melt 5. handled through step to be cast online using casting machine, casting forms aluminium ingot casting,
The temperature cast online is 710~720 DEG C, and the speed of casting is 35~45m/min；
7. being packaged: 6. step being obtained to aluminium ingot casting after on-line cooling, Gao Pin can be obtained after carrying out sawing, bundling, packaging
Matter aluminium ingot.
2. a kind of production technology of high-quality aluminium ingot according to claim 1, it is characterised in that: step 3. in, it is described
The content of Si, Fe, Ni, Ga, V, Ti, Zn impurity in carbon anode is respectively in 200ppm, 200 ppm, 100 ppm, 80 ppm, 50
Ppm, 10 ppm and 8ppm or less.
3. a kind of production technology of high-quality aluminium ingot according to claim 1, it is characterised in that: step 3. in, electrolysis
When producing high-temperature electrolysis molten aluminum, electrolyte level control is in 16~19cm, and the flat control of aluminum water is in 28~32cm.
4. a kind of production technology of high-quality aluminium ingot according to claim 1, it is characterised in that: step 4. in, right
High-temperature electrolysis molten aluminum carry out composition detection when, it is desirable that each composition range (wt.%) of high-temperature electrolysis molten aluminum be AL:99.50~
99.99, Si≤0.10, Fe≤0.10, impurity summation≤0.30.
5. a kind of production technology of high-quality aluminium ingot according to claim 1, it is characterised in that: step 4. in, be passed through
Nitrogen and refining agent refining are to be blown into the nitrogen and sodium chloride that 0.3~0.5MPa purity is 99.9%, chlorine in high melt furnace bottom
Change sodium dosage is 1~3kg/t.AL, removes slag inclusion and gas in melt.
6. a kind of production technology of high-quality aluminium ingot according to claim 1, it is characterised in that: step 5. in, online
The gaseous species of degassing processing are N2-CL2Mixed gas, and N2-CL2The air pressure of mixed gas is 0.3~0.5MPa, is removed online
The equipment of gas disposal is rotary degassing device, and the rotor speed of rotary degassing device is 300~500rpm.
7. a kind of production technology of high-quality aluminium ingot according to claim 1, it is characterised in that: step 5. in, online
Filtering uses foam ceramic filter, and the mesh diameter of foam ceramic filter is 0.2~0.8mm.
8. a kind of production technology of high-quality aluminium ingot according to claim 1, it is characterised in that: step 7. in, online
In such a way that cool water shower is cooling, the flow of cooling water is 100~150m for cooling3/min。
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