CN109913665A - A kind of method that bauxite vacuum distillation prepares metallic aluminium - Google Patents
A kind of method that bauxite vacuum distillation prepares metallic aluminium Download PDFInfo
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- CN109913665A CN109913665A CN201910288603.9A CN201910288603A CN109913665A CN 109913665 A CN109913665 A CN 109913665A CN 201910288603 A CN201910288603 A CN 201910288603A CN 109913665 A CN109913665 A CN 109913665A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 57
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000004411 aluminium Substances 0.000 title claims abstract description 48
- 229910001570 bauxite Inorganic materials 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000005292 vacuum distillation Methods 0.000 title claims abstract description 12
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 102
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 101
- 238000007885 magnetic separation Methods 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 13
- 238000005261 decarburization Methods 0.000 claims abstract description 10
- 239000000428 dust Substances 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 11
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims description 3
- 239000000571 coke Substances 0.000 claims description 3
- 238000004939 coking Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000002006 petroleum coke Substances 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 27
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 17
- 239000000047 product Substances 0.000 abstract description 15
- 239000000203 mixture Substances 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 description 32
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 27
- 150000001875 compounds Chemical class 0.000 description 12
- 239000007789 gas Substances 0.000 description 11
- 229910052742 iron Inorganic materials 0.000 description 9
- 238000001291 vacuum drying Methods 0.000 description 8
- 238000004321 preservation Methods 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 239000000284 extract Substances 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 238000003763 carbonization Methods 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 238000011946 reduction process Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 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 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000746 Structural steel Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 229910052934 alunite Inorganic materials 0.000 description 1
- 239000010424 alunite Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- OCYSGIYOVXAGKQ-FVGYRXGTSA-N phenylephrine hydrochloride Chemical compound [H+].[Cl-].CNC[C@H](O)C1=CC=CC(O)=C1 OCYSGIYOVXAGKQ-FVGYRXGTSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- KPZTWMNLAFDTGF-UHFFFAOYSA-D trialuminum;potassium;hexahydroxide;disulfate Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Al+3].[Al+3].[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O KPZTWMNLAFDTGF-UHFFFAOYSA-D 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention provides a kind of methods that bauxite vacuum distillation prepares metallic aluminium, belong to vacuum metallurgy field.The present invention makes whole Si and part Fe volatilization in green compact, the second carbon thermal reduction is then carried out in nitrogen, obtains the mixture of FeN and AlN, then by magnetic separation, decarburization and vacuum thermal decomposition, obtain metallic aluminium by carrying out the first carbon thermal reduction under vacuum conditions.Metallic aluminium can be directly prepared from bauxite through the invention, the preparation method have low energy consumption, it is pollution-free, the by-product of the high conversion rate of product, aluminium it is few and preparation aluminium it is with high purity the features such as.Embodiment statistics indicate that, the purity for the metallic aluminium that preparation method provided by the invention obtains is 95% or more, and conversion ratio is 94% or more.
Description
Technical field
The present invention relates to the sides that vacuum metallurgy technology field more particularly to a kind of bauxite vacuum distillation prepare metallic aluminium
Method.
Background technique
Aluminum is a light metal, has argenteous metallic luster, and key property is light-weight, corrosion-resistant, easy conductive, easily
Extension, good appearance etc., relative density only have the 1/3 of steel, and the mechanical strength of certain alloys is than being even more than structural steel.Cause
This, aluminium alloy has very big intensity ratio.It is widely used in communications and transportation, packaging, building, electrical, aerospace and army
The fields such as thing are the second largest metal materials that demand is only second to steel.
There is long history in China using aluminium ore, begins to extract alum from alunite very early for medicine and industry
Upper application.Metallic aluminium is initially produced by chemical method, replaces potassium to restore NaCl-AlCl with sodium from France Deville in 19543Complexing
Salt produces metallic aluminium, starts to put into production to electrolytic aluminium refining factory in 1987, this between 30 years work produce the aluminium of 200t.It is modern
Aluminum smelting industry mainly takes cryolite-alumina fused salt electrolysis process and aluminium chloride electrolytic aluminium refining.But there are techniques for electrolysis method
Process is complicated, energy consumption is high, has the shortcomings that the discharge of greenhouse gases and perfluorinated hydrocarbon, causes influence very serious to environment.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of methods that bauxite vacuum distillation prepares metallic aluminium.This hair
The preparation method low energy consumption of bright offer, it is pollution-free.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
A kind of method that bauxite vacuum distillation prepares metallic aluminium, comprising the following steps:
It is suppressed after bauxite, carbon dust and water are mixed, obtains green compact, contain SiO in the bauxite2、FenOxAnd Al2O3；
Under vacuum conditions, the green compact is subjected to the first carbon thermal reduction, obtains the first carbon hot, the first carbon heat
The temperature of reduction is 1200~1400 DEG C；
In nitrogen atmosphere, the first carbon hot is subjected to the second carbon thermal reduction, obtains the second carbon hot, it is described
The temperature of second carbon thermal reduction is 1500~1700 DEG C；
By the second carbon hot magnetic separation, magnetic separation residue is obtained；
By the magnetic separation residue decarburization, AlN is obtained；
The AlN is subjected to vacuum thermal decomposition, obtains metallic aluminium.
Preferably, the molar ratio of the sum of the oxygen element in the bauxite and element silicon and carbon dust is 1:1~1.4.
Preferably, the bauxite and carbon dust quality and be 8~10:1 with the mass ratio of water.
Preferably, the material of the carbon dust includes one of coke, petroleum coke and coking coal or a variety of.
Preferably, the partial size of the carbon dust and bauxite is 200 mesh and following.
Preferably, the pressure of the compacting is 5~10MPa.
Preferably, the pressure of first carbon thermal reduction is 10~100Pa, time of first carbon thermal reduction is 60~
180min。
Preferably, the time of second carbon thermal reduction is 60~180min.
Preferably, the temperature of the decarburization is 800~1000 DEG C, and the time is 60~180min.
Preferably, the pressure of the vacuum thermal decomposition is 100~10-3Pa, temperature be 1550~1700 DEG C, the time be 60~
180min。
The present invention provides a kind of methods that bauxite vacuum distillation prepares metallic aluminium, comprising the following steps: by bauxite,
It is suppressed after carbon dust and water mixing, obtains green compact, contain SiO in the bauxite2、FenOxAnd Al2O3；Under vacuum conditions, by institute
It states green compact and carries out the first carbon thermal reduction, obtain the first carbon hot, the temperature of first carbon thermal reduction is 1200~1400 DEG C；
In nitrogen atmosphere, the first carbon hot is subjected to the second carbon thermal reduction, obtains the second carbon hot, the second carbon heat
The temperature of reduction is 1500~1700 DEG C；By the second carbon hot magnetic separation, magnetic separation residue is obtained；The magnetic separation is remaining
Object decarburization, obtains AlN；The AlN is subjected to vacuum thermal decomposition, obtains metallic aluminium.The present invention by carrying out under vacuum conditions
First carbon thermal reduction makes whole Si and part Fe volatilization in green compact, the first carbon thermal reduction is then carried out in nitrogen, is obtained
The mixture of FeN and AlN obtains metallic aluminium, preparation method low energy consumption, no dirt then by magnetic separation, decarburization and vacuum thermal decomposition
Dye, directly can directly prepare metallic aluminium from bauxite through the invention, the high conversion rate with product, and the by-product of aluminium is few
The features such as with high purity with the aluminium of preparation.Embodiment statistics indicate that, the metallic aluminium that preparation method provided by the invention obtains it is pure
Degree is 95% or more, and conversion ratio is 94% or more.
Detailed description of the invention
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.
Fig. 1 is the flow chart for the method that bauxite vacuum distillation prepares metallic aluminium in the embodiment of the present invention.
Specific embodiment
The present invention provides a kind of methods that bauxite vacuum distillation prepares metallic aluminium, comprising the following steps:
It is suppressed after bauxite, carbon dust and water are mixed, obtains green compact, contain SiO in the bauxite2、FenOxAnd Al2O3；
Under vacuum conditions, the green compact is subjected to the first carbon thermal reduction, obtains the first carbon hot, the first carbon heat
The temperature of reduction is 1200~1400 DEG C；
In nitrogen atmosphere, the first carbon hot is subjected to the second carbon thermal reduction, obtains the second carbon hot, it is described
The temperature of second carbon thermal reduction is 1500~1700 DEG C；
By the second carbon hot magnetic separation, magnetic separation residue is obtained；
By the magnetic separation residue decarburization, AlN is obtained；
The AlN is subjected to vacuum thermal decomposition, obtains metallic aluminium.
The present invention suppresses after mixing bauxite, carbon dust and water, obtains green compact, contains SiO in the bauxite2、FenOx
And Al2O3.The present invention does not have special restriction to the source of the bauxite and carbon dust, and use is well known to those skilled in the art
Commercial goods.
The present invention does not have special restriction to the hybrid mode, is using hybrid mode well known to those skilled in the art
It can.
In the present invention, the bauxite and carbon dust quality and be preferably 8~10:1 with the mass ratio of water, more preferably 9:
1.In the present invention, the water is preferably distilled water.In the present invention, the water can be used to better green compact.
In the present invention, the material of the carbon dust preferably includes one of coke, petroleum coke and coking coal or a variety of.
In the present invention, the partial size of the carbon dust and bauxite is preferably all 200 mesh and following.In the present invention, described
Aluminium oxide can be reduced to metallic aluminium under the high temperature conditions as reducing agent by carbon dust.
In the present invention, the pressure of the compacting is preferably 5~10MPa, more preferably 6~9MPa, most preferably 7~
8MPa.In the present invention, the compacting can guarantee coming into full contact with for bauxite powder and carbon dust during follow-up sintering, convenient for true
The progress of empty carbon-thermal reduction.
In the present invention, the molar ratio of the sum of the oxygen element in the bauxite and element silicon and carbon dust be preferably 1:1~
1.4, more preferably 1:1.2~1.3.In the present invention, the mass ratio of the bauxite powder and carbon dust within the above range can
It is further ensured that bauxite is reduced sufficiently, and generates less CO2Isothermal chamber gas.
After obtaining green compact, the present invention carries out the first carbon thermal reduction under vacuum conditions, by the green compact, obtains the first carbon heat
Product, the temperature of first carbon thermal reduction are 1200~1400 DEG C.
In the present invention, the pressure of first carbon thermal reduction is preferably 10~100Pa, more preferably 20~80Pa, most
The time of preferably 30~70Pa, first carbon thermal reduction are preferably 60~180min, and more preferably 80~160min is optimal
It is selected as 100~140min, the temperature of first carbon thermal reduction is preferably 1250~1350 DEG C, and more preferably 1300 DEG C.At this
Whole Si and part Fe volatilization in invention, during first carbon thermal reduction, in green compact.In the present invention, described complete
It condenses to obtain the compound containing Si, Fe through vacuum volatilization after portion Si and part Fe volatilization
After obtaining the first carbon hot, the present invention carries out the second carbon heat in nitrogen atmosphere, by the first carbon hot
Reduction, obtains the second carbon hot, and the temperature of second carbon thermal reduction is 1500~1700 DEG C.
In the present invention, the time of second carbon thermal reduction is preferably 60~180min, more preferably 80~160min,
Most preferably 100~140min.In the present invention, the pressure of second carbon thermal reduction is preferably 100~500Pa, more preferably
For 150~450Pa, most preferably 200~400Pa, the temperature of second carbon thermal reduction is preferably 1550~1650 DEG C, more excellent
It is selected as 1600 DEG C.
In the present invention, the carbothermic reduction reaction for the aluminium oxide that reacts in second carbothermic reduction process, it is specific
Equation is as follows: Al2O3+N2(g)+3C=2AlN+3CO (g).
After obtaining the second carbon hot, the second carbon hot magnetic separation is obtained magnetic separation residue by the present invention.In this hair
In bright, magnetic separation is carried out again after the preferred cooled to room temperature of the second carbon hot.In the present invention, the magnetic separation process energy
It is enough to separate the substance containing Fe, obtain the mixture of AlN and C, i.e. magnetic separation residue.
After obtaining magnetic separation residue, the magnetic separation residue decarburization is obtained AlN by the present invention.In the present invention, described de-
The temperature of carbon is preferably 800~1000 DEG C, more preferably 850~950 DEG C, most preferably 900 DEG C, and the time is preferably 60~
180min, more preferably 80~160min, most preferably 100~140min.
After obtaining AlN, the AlN is carried out vacuum thermal decomposition by the present invention, obtains metallic aluminium.
In the present invention, the pressure of the vacuum thermal decomposition is preferably 100~10-3Pa, more preferably 50~10-2Pa, most
Preferably 1Pa, temperature are preferably 1550~1700 DEG C, and more preferably 1570~1630 DEG C, most preferably 1600 DEG C, the time is excellent
It is selected as 60~180min, more preferably 80~160min, most preferably 100~140min.In the present invention, the Vacuum Heat point
The specific equation of the reaction occurred in solution are as follows: 2AlN=2Al (g)+N2(g)。
In an embodiment of the present invention, the vacuum thermal decomposition preferably includes following steps: AlN being put into after tabletting true
Empty furnace closes fire door and extracts vacuum, begins to warm up when pressure is lower than 10Pa, and material is heated to a certain mesh in vacuum thermal decomposition
Protective gas is passed through when marking temperature to control pressure 10~10-3The a certain target value of Pa simultaneously keeps the temperature 60~180min, obtains gas
State Al and N2, collect the gaseous state Al of generation to obtain metallic aluminium by volatilization condensing unit.
In the present invention, the nitrogen that the vacuum thermal decomposition generates preferably is back in the second carbothermic reduction process.
In the present invention, the protective gas is preferably argon gas or nitrogen.
The present invention does not have special restriction to the device of the vacuum carbothermal reduction, and use is well known to those skilled in the art
Vacuum heater.The present invention does not have special restriction to the heating rate for being warming up to the reaction temperature, using ability
Heating rate known to field technique personnel.
It is detailed to a kind of method progress that bauxite vacuum distillation prepares metallic aluminium provided by the invention below with reference to embodiment
Thin explanation, but they cannot be interpreted as limiting the scope of the present invention.
Fig. 1 is the flow chart for the method that the vacuum distillation of bauxite of the embodiment of the present invention prepares metallic aluminium, by bauxite, carbon dust
It is suppressed with after water mixing, obtains green compact, contain SiO in the bauxite2、FenOxAnd Al2O3；Under vacuum conditions, by the pressure
Base carries out the first carbon thermal reduction, obtains containing Si, Fe gas and (the first carbon hot) containing Fe, Al compound, the gas containing Si, Fe
It condenses to obtain the compound containing Si, Fe through vacuum volatilization；In nitrogen atmosphere, the first carbon hot is subjected to the second carbon heat also
Original obtains the second carbon hot；By the second carbon hot magnetic separation, magnetic separation residue and compound containing Fe are obtained；By institute
Vacuum Heat decomposition is carried out after stating magnetic separation residue decarburization, obtains gaseous aluminum and nitrogen, gaseous aluminum volatilization condensation obtains metallic aluminium, nitrogen
Gas is back in the second carbothermic reduction process.
Embodiment 1
Step 1, by bauxite and carbon dust according to molar ratio (n(O)+n(Si)):n(C)=1:1.3 is matched, and quality is added
For the water of bauxite and carbon dust gross mass 1/8, it is uniformly mixed, tabletting is carried out under the pressure of 5MPa；
The material of step 1 is put into graphite crucible by step 2, is covered condenser in crucible top, is closed vacuum drying oven, lid
Upper condenser extracts vacuum and controls pressure in 10Pa, material is then heated to 1300 DEG C and keeps the temperature 80 minutes, will be in material
Part iron and whole silicon volatilize.
Step 3 is passed through nitrogen for pressure when step 2 resultant product (compound of Yu Tie and aluminium) is warming up in 1700 DEG C
Control is in 100Pa and keeps the temperature 60 minutes, obtains the product of FeN, AlN.
Step 4, when the product of step 3 is cooled to room temperature, by magnetic method separate compound containing Fe obtain AlN's and C
Mixture containing AlN and C is heated to 800 DEG C of heat preservations, 90 minutes progress carbonization treatments in air, finally obtained by mixture
AlN。
Step 5 by obtained AlN tabletting and is put into vacuum drying oven, is closed fire door and is extracted vacuum, when pressure is lower than 10Pa
It begins to warm up, protective gas is passed through when material is heated to a certain target temperature in 1650 DEG C and controls pressure 10-3Pa is simultaneously
Heat preservation is to obtaining gaseous state Al and N after 80 minutes2, collected through volatilization condensation and obtain metallic aluminium, nitrogen is back in step 3.
Through detecting, the purity of metallic aluminium made from the present embodiment is 97%, yield 96%.
Embodiment 2
Step 1, by bauxite and carbon dust according to molar ratio (n(O)+n(Si)):n(C)=1:1.2 is matched, and quality is added
For the water of bauxite and carbon dust gross mass 1/10, it is uniformly mixed, tabletting is carried out under the pressure of 7MPa；
The material of step 1 is put into graphite crucible by step 2, is covered condenser in crucible top, is closed vacuum drying oven, lid
Upper condenser extracts vacuum and controls pressure in 20Pa, material is then heated to 1400 DEG C and keeps the temperature 180 minutes, by material
In part iron and whole silicon volatilize.
Step 3 is passed through nitrogen for pressure when step 2 resultant product (compound of Yu Tie and aluminium) is warming up in 1500 DEG C
Control is in 400Pa and keeps the temperature 160 minutes, obtains the product of FeN, AlN.
Step 4, when the product of step 3 is cooled to room temperature, by magnetic method separate compound containing Fe obtain AlN's and C
Mixture containing AlN and C is heated to 900 DEG C of heat preservations, 100 minutes progress carbonization treatments in air, finally obtained by mixture
AlN。
Step 5 by obtained AlN tabletting and is put into vacuum drying oven, is closed fire door and is extracted vacuum, when pressure is lower than 10Pa
It begins to warm up, protective gas is passed through when material is heated to a certain target temperature in 1700 DEG C, pressure is controlled in 10Pa and protected
Temperature is to obtaining gaseous state Al and N after 100 minutes2, collected through volatilization condensation and obtain metallic aluminium, nitrogen is back in step 3.
Through detecting, the purity of metallic aluminium made from the present embodiment is 96%, yield 95%.
Embodiment 3
Step 1, by bauxite and carbon dust according to molar ratio (n(O)+n(Si)):n(C)=1:1.1 is matched, and quality is added
For the water of bauxite and carbon dust gross mass 1/9, it is uniformly mixed, tabletting is carried out under the pressure of 10MPa；
The material of step 1 is put into graphite crucible by step 2, is covered condenser in crucible top, is closed vacuum drying oven, lid
Upper condenser extracts vacuum and controls pressure in 50Pa, material is then heated to 1200 DEG C and keeps the temperature 60 minutes, will be in material
Part iron and whole silicon volatilize.
Step 3 is passed through nitrogen for pressure when step 2 resultant product (compound of Yu Tie and aluminium) is warming up in 1500 DEG C
Control is in 500Pa and keeps the temperature 160 minutes, obtains the product of FeN, AlN.
Step 4, when the product of step 3 is cooled to room temperature, by magnetic method separate compound containing Fe obtain AlN's and C
Mixture containing AlN and C is heated to 1000 DEG C of heat preservations, 180 minutes progress carbonization treatments in air, finally obtained by mixture
AlN。
Step 5 by obtained AlN tabletting and is put into vacuum drying oven, is closed fire door and is extracted vacuum, when pressure is lower than 10Pa
Begin to warm up, be passed through when material is heated to a certain target temperature in 1500 DEG C protective gas by pressure control 0.1Pa simultaneously
Heat preservation is to obtaining gaseous state Al and N after 80 minutes2, collected through volatilization condensation and obtain metallic aluminium, nitrogen is back in step 3.
Through detecting, the purity of metallic aluminium made from the present embodiment is 96%, yield 96%.
Embodiment 4
Step 1, by bauxite and carbon dust according to molar ratio (n(O)+n(Si)):n(C)=1:1.4 is matched, and quality is added
For the water of bauxite and carbon dust gross mass 1/10, it is uniformly mixed, tabletting is carried out under the pressure of 9MPa；
The material of step 1 is put into graphite crucible by step 2, is covered condenser in crucible top, is closed vacuum drying oven, lid
Upper condenser extracts vacuum and controls pressure in 40Pa, material is then heated to 1350 DEG C and keeps the temperature 140 minutes, by material
In part iron and whole silicon volatilize.
Step 3 is passed through nitrogen for pressure when step 2 resultant product (compound of Yu Tie and aluminium) is warming up in 1600 DEG C
Control is in 450Pa and keeps the temperature 140 minutes, obtains the product of FeN, AlN.
Step 4, when the product of step 3 is cooled to room temperature, by magnetic method separate compound containing Fe obtain AlN's and C
Mixture containing AlN and C is heated to 850 DEG C of heat preservations, 140 minutes progress carbonization treatments in air, finally obtained by mixture
AlN。
Step 5 by obtained AlN tabletting and is put into vacuum drying oven, is closed fire door and is extracted vacuum, when pressure is lower than 10Pa
Begin to warm up, be passed through when material is heated to a certain target temperature in 1630 DEG C protective gas by pressure control 0.01Pa simultaneously
Heat preservation is to obtaining gaseous state Al and N after 140 minutes2, collected through volatilization condensation and obtain metallic aluminium, nitrogen is back in step 3.
Through detecting, the purity of metallic aluminium made from the present embodiment is 98%, yield 97%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of method that bauxite vacuum distillation prepares metallic aluminium, which comprises the following steps:
It is suppressed after bauxite, carbon dust and water are mixed, obtains green compact, contain SiO in the bauxite2、FenOxAnd Al2O3；
Under vacuum conditions, the green compact is subjected to the first carbon thermal reduction, obtains the first carbon hot, first carbon thermal reduction
Temperature be 1200~1400 DEG C；
In nitrogen atmosphere, the first carbon hot is subjected to the second carbon thermal reduction, obtains the second carbon hot, described second
The temperature of carbon thermal reduction is 1500~1700 DEG C；
By the second carbon hot magnetic separation, magnetic separation residue is obtained；
By the magnetic separation residue decarburization, AlN is obtained；
The AlN is subjected to vacuum thermal decomposition, obtains metallic aluminium.
2. preparation method according to claim 1, which is characterized in that the sum of oxygen element and element silicon in the bauxite
Molar ratio with carbon dust is 1:1~1.4.
3. preparation method according to claim 1, which is characterized in that the bauxite and carbon dust quality and the quality with water
Than for 8~10:1.
4. preparation method according to claim 1, which is characterized in that the material of the carbon dust include coke, petroleum coke and
One of coking coal is a variety of.
5. preparation method according to claim 1 or 4, which is characterized in that the partial size of the carbon dust and bauxite is 100
Mesh and following.
6. preparation method according to claim 1, which is characterized in that the pressure of the compacting is 5~10MPa.
7. preparation method according to claim 1, which is characterized in that the pressure of first carbon thermal reduction be 10~
100Pa, the time of first carbon thermal reduction are 60~180min.
8. preparation method according to claim 1, which is characterized in that the time of second carbon thermal reduction be 60~
180min。
9. preparation method according to claim 1, which is characterized in that the temperature of the decarburization is 800~1000 DEG C, the time
For 60~180min.
10. preparation method according to claim 1, which is characterized in that the pressure of the vacuum thermal decomposition is 10~10- 3Pa, temperature are 1550~1700 DEG C, and the time is 60~180min.
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