CN104745816A - Method for preparing metallic aluminum by means of chlorination reduction of aluminum nitride - Google Patents
Method for preparing metallic aluminum by means of chlorination reduction of aluminum nitride Download PDFInfo
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- CN104745816A CN104745816A CN201510128262.0A CN201510128262A CN104745816A CN 104745816 A CN104745816 A CN 104745816A CN 201510128262 A CN201510128262 A CN 201510128262A CN 104745816 A CN104745816 A CN 104745816A
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 26
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title abstract 3
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 79
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 23
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000007323 disproportionation reaction Methods 0.000 claims abstract description 10
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 7
- 239000004411 aluminium Substances 0.000 claims description 60
- 229910017083 AlN Inorganic materials 0.000 claims description 31
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 31
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- 239000000428 dust Substances 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005272 metallurgy Methods 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 239000003245 coal Substances 0.000 abstract description 2
- 239000000446 fuel Substances 0.000 abstract description 2
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 3
- 238000003825 pressing Methods 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 description 21
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 3
- 238000012850 discrimination method Methods 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- TWHBEKGYWPPYQL-UHFFFAOYSA-N aluminium carbide Chemical compound [C-4].[C-4].[C-4].[Al+3].[Al+3].[Al+3].[Al+3] TWHBEKGYWPPYQL-UHFFFAOYSA-N 0.000 description 2
- 229910001570 bauxite Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005658 halogenation reaction Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- CSJDCSCTVDEHRN-UHFFFAOYSA-N methane;molecular oxygen Chemical compound C.O=O CSJDCSCTVDEHRN-UHFFFAOYSA-N 0.000 description 2
- 230000002829 reductive effect Effects 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 238000009866 aluminium metallurgy Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 sodium aluminum fluoride Chemical compound 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for preparing metallic aluminum by means of chlorination reduction of aluminum nitride, belonging to the field of vacuum metallurgy. The method comprises the following steps: firstly adding carbon to aluminum oxide and uniformly mixing to obtain a mixture; pressing the mixture into a block; introducing nitrogen gas and reducing under the pressure of 10<-2>-50Pa at 1300-1700 DEG C to obtain aluminum nitride; stopping introducing nitrogen gas and further introducing aluminum subchloride vapor for chlorination and disproportionation reaction; finally controlling the temperature of a condenser to be 700-900 DEG C to obtain metallic aluminum easy to separate and well crystallized on the condenser. The method is simple in process flow, easy to operate and adopts low-price and easily available raw materials; no other additives or coal fuel or the like is added in the process; moreover, aluminum trichloride and nitrogen gas can be recycled.
Description
Technical field
The present invention relates to the method that metallic aluminium is prepared in a kind of aluminium nitride chlorination reduction, belong to vacuum metallurgy technology field.
Background technology
Aluminium is the metallic element that in the earth's crust, content is the abundantest, content 8.3%.The content of aluminium element in the earth's crust is only second to oxygen and silicon, and occupy the 3rd, its standing stock occupy the 2nd in a metal.Aluminium is active metal, and in dry air, the surface of aluminium forms the dense oxidation film of thick about 50 dusts (1 dust=0.1 nanometer) immediately, and aluminium can not be oxidized further also can be water-fast; The purposes of material depends on the character of material to a great extent.Because aluminium has multiple premium properties, so aluminium has purposes very widely.
Al and Alalloy be current applications very widely, one of most economical applicable material.World aluminum output occupies first of non-ferrous metal within 1956, beginning to exceed copper output always.The output of current aluminium and consumption (calculating by ton) are only second to steel, become the second largest metal of mankind's application; And the resource of aluminium is very abundant, according to predesigne, the mineral reserve storage capacity of aluminium accounts for more than 8% of earth's crust constitute.Aluminium alloy is widely used in the process industries such as aircraft, automobile, train, boats and ships.In addition, cosmic rocket, space shuttle, man-made satellite also use a large amount of aluminium and aluminium alloy thereof.Aluminium has been widely used in electrical equipment process industry, electric wire industry and radio industry.Aluminium foil is widely used in containers of cigarettes, candy etc., also can be made into aluminium wire, aluminum strip, and can the various aluminum products of rolling.The surface of aluminium, because there being fine and close oxide film, being not easily corroded, being often used to manufacturing chemistry reactor, medicine equipment, freezing plant, petroleum refining device, oil and natural gas pipeline etc.Aluminium powder has silvery white gloss and is commonly used to do coating etc.
Aluminium all in the world is all produced by electrolytic process.Aluminium electrolytic industry is produced and is adopted Hall-Ai Lu cryolite-alumina molten salt electrolysis, and the fluoride salt namely based on sodium aluminum fluoride is as flux, and aluminum oxide forms heterogeneous electrolyte system for melting matter.Wherein Na
2alF
6-Al
2o
3two component system and Na
3alF
6-AlF
3-Al
2o
3three component system is the basis of industrial electrolysis matter.Aluminium Industry has greater environmental impacts, and belongs to highly energy-consuming, high pollution industry.The waste gas of discharging in Aluminum Electrolysis Production mainly CO
2, and based on the gas-solid fluorochemical etc. of HF gas.CO
2being a kind of greenhouse gases, is the major cause causing global warming.And the CF in fluorochemical
4and C
2f
6its greenhouse effect effect be the 6500-10000 of carbonic acid gas doubly, and impact in various degree can be caused on ozonosphere.
In the research of aluminum smelting technology novel method, mainly both at home and abroad to carry out the work around electric heating process, blast furnace aluminium metallurgy method, ionic liquid electrolytic process, the directly aspect such as carbothermic method and alumina carbon thermal reduction halogenation discrimination method, in addition, some investigators are also had just to adopt hydrogen reducing aluminum oxide or AlCl
3prepare metallic aluminium and carry out some researchs.Carbothermic method receives publicity because its flow process is short, energy-conservation always, Alcoa Inc of the U.S. and Swiss Zurich Federal Institute of Technology carry out continuing research to the method in recent years always, but in the direct carbothermic reduction reaction of aluminum oxide, the material such as aluminium carbide, carbon oxygen aluminium of metallic aluminium and the impurity in bauxite that reaction generates and generation mixes and is difficult to be separated this problem and governs applying of the method always.And alumina carbon thermal reduction chlorination discrimination method is that vacuum metallurgy national engineering laboratory of Kunming University of Science and Technology is on the basis of the long-term vacuum reducing research work to non-ferrous metal, for the feature of aluminum subchloride disproportionation reaction, under the aluminum oxide low pressure proposed, carbothermic reduction-halogenation discrimination method prepares the thinking of metallic aluminium, and achieves interim progress.The party's ratio juris is: under high-temperature low-pressure aluminum oxide under the existence of carbon can with AlCl
3react, generate volatile AlCl, AlCl about 700 DEG C, be decomposed into metallic aluminium and AlCl under 60Pa
3, obtain metallic aluminium, wherein AlCl
3recyclable rear recycling, react as follows:
(1-1)
(1-2)
The method efficiently solves in the direct carbothermic reduction reaction of aluminum oxide, and the material such as aluminium carbide, carbon oxygen aluminium of metallic aluminium and the impurity in bauxite that reaction generates and generation mixes the problem being difficult to be separated.
The present invention with wear that to study Yongnian etc. identical be all adopt carbon as reductive agent, but the many crucial difference existed, one, when the present invention adopts reduction with carbon, with the addition of nitrogen, changes aluminum oxide into aluminium nitride; Its two, operational condition also has bigger difference, carbon tropical resources reaction have employed relatively high temperature of reaction; Its three, in the present invention, the object of chlorination process is aluminium nitride, finally obtains the metallic aluminium of well-crystallized.In a word, the present invention has raw materials for production cheapness, is easy to get, the features such as technical process is short, simple to operate.
Summary of the invention
For above-mentioned prior art Problems existing and deficiency, the invention provides the method that metallic aluminium is prepared in a kind of aluminium nitride chlorination reduction.The present invention take aluminum oxide as the raw material extracting metallic aluminium, and carbon is reductive agent, passes into nitrogen, makes aluminum oxide be transformed into aluminium nitride by addition on reduction nitridation process, and aluminium nitride is at pressure 10
-2after the condensation of chlorination disproportionation, obtain the solid metal aluminium of well-crystallized under Pa ~ 30Pa, 1300 DEG C ~ 1700 DEG C conditions, reduce the production cost of metallic aluminium, the present invention is achieved through the following technical solutions.
A method for metallic aluminium is prepared in aluminium nitride chlorination reduction, and its concrete steps are as follows:
Step 1, first will add the carbon of alumina molar amount 3 ~ 6 times in aluminum oxide, and then mix and obtain mixture, mixture is pressed into bulk with 10MPa ~ 50MPa pressure, passing into nitrogen, pressure is 10
-2under the condition of Pa ~ 50Pa, temperature 1300 ~ 1700 DEG C, reduction obtains aluminium nitride (as Suo Shi (a));
Al
2O
3(s)+3C(s)+N
2(g)=2AlN(s)+3CO(g) （a）
The aluminium nitride that step 2, step 1 obtain passing into aluminum subchloride steam, the pressure of vacuum system is 10
-2chlorination disproportionation reaction under the condition of Pa ~ 50Pa, temperature 1300 ~ 1700 DEG C (as shown in (b), (c)), the temperature finally controlling condenser is 700 ~ 900 DEG C and on condenser, obtains the easily separated and metallic aluminium of complete crystallization;
2AlN(s)+AlCl
3(g)=3AlCl(g)+N
2(g) （b）
3AlCl(g)=AlCl
3(g)+2Al(s) （c）
Carbon in described step 1 is the carbon dust that granularity is less than 0.5mm.
The intake of the nitrogen in described step 1 is 15g/h ~ 25g/h.
The intake of described step 2 middle or low price aluminum chloride steam is 200g/h ~ 300g/h.
The invention has the beneficial effects as follows: flow process of the present invention is simple, convenient operation, low in raw material price, to be easy to get, without the need to adding any other additive and coal fuel etc. in process, and aluminum chloride and nitrogen reusable edible.
Accompanying drawing explanation
Fig. 1 is present invention process schema;
Fig. 2 is the XRD figure of the metallic aluminium that the embodiment of the present invention 1 condensation obtains.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
As shown in Figure 1, the method for metallic aluminium is prepared in this aluminium nitride chlorination reduction, and its concrete steps are as follows:
Step 1, first will add the carbon (60g) of 5 moles in 1 moles aluminium (102g), then mix and obtain mixture, mixture is pressed into bulk with 30MPa pressure, passing into nitrogen, pressure is 50Pa, under the condition of temperature 1700 DEG C reduction within 5 hours, obtain aluminium nitride (as Suo Shi (a)); Wherein carbon is the carbon dust that granularity is less than 0.5mm, and the intake of nitrogen is 25g/h;
Al
2O
3(s)+3C(s)+N
2(g)=2AlN(s)+3CO(g) （a）
Step 2, stopping pass into nitrogen, the aluminium nitride that step 1 obtains passing into aluminum subchloride steam, the pressure of vacuum system is 50Pa, chlorination disproportionation reaction 1 hour (as shown in (b), (c)) under the condition of temperature 1700 DEG C, the temperature finally controlling condenser is 700 DEG C and on condenser, obtains the easily separated and metallic aluminium of complete crystallization, and aluminum subchloride steam intake is 300g/h;
2AlN(s)+AlCl
3(g)=3AlCl(g)+N
2(g) （b）
3AlCl(g)=AlCl
3(g)+2Al(s) （c）
The metallic aluminium XRD figure prepared is composed as shown in Figure 2, its purity >95wt.%.
Embodiment 2
As shown in Figure 1, the method for metallic aluminium is prepared in this aluminium nitride chlorination reduction, and its concrete steps are as follows:
Step 1, first will add the carbon (48g) of 4 moles in 1 moles aluminium (102g), and then mix and obtain mixture, mixture is pressed into bulk with 20MPa pressure, passing into nitrogen, pressure is 10
-2under the condition of Pa, temperature 1600 DEG C, reduction obtains aluminium nitride (as Suo Shi (a)) for 5 hours; Wherein carbon is the carbon dust that granularity is less than 0.5mm, and the intake of nitrogen is 15g/h;
Al
2O
3(s)+3C(s)+N
2(g)=2AlN(s)+3CO(g) （a）
Step 2, stop passing into nitrogen, the aluminium nitride that step 1 obtains passing into aluminum subchloride steam, the pressure of vacuum system is 10
-2chlorination disproportionation reaction 1 hour (as shown in (b), (c)) under the condition of Pa, temperature 1600 DEG C, the temperature finally controlling condenser is 900 DEG C and on condenser, obtains the easily separated and metallic aluminium of complete crystallization, and aluminum subchloride steam intake is 200g/h;
2AlN(s)+AlCl
3(g)=3AlCl(g)+N
2(g) （b）
3AlCl(g)=AlCl
3(g)+2Al(s) （c）
Its purity >94wt.% of the metallic aluminium prepared.
Embodiment 3
As shown in Figure 1, the method for metallic aluminium is prepared in this aluminium nitride chlorination reduction, and its concrete steps are as follows:
Step 1, first will add the carbon (72g) of 6 moles in 1 moles aluminium (102g), then mix and obtain mixture, mixture is pressed into bulk with 40MPa pressure, passing into nitrogen, pressure is 30Pa, under the condition of temperature 1600 DEG C reduction within 5 hours, obtain aluminium nitride (as Suo Shi (a)); Wherein carbon is the carbon dust that granularity is less than 0.5mm, and the intake of nitrogen is 20g/h;
Al
2O
3(s)+3C(s)+N
2(g)=2AlN(s)+3CO(g) （a）
Step 2, stopping pass into nitrogen, the aluminium nitride that step 1 obtains passing into aluminum subchloride steam, the pressure of vacuum system is 30Pa, chlorination disproportionation reaction 1 hour (as shown in (b), (c)) under the condition of temperature 1600 DEG C, the temperature finally controlling condenser is 700 DEG C and on condenser, obtains the easily separated and metallic aluminium of complete crystallization; Aluminum subchloride steam intake is 250g/h;
2AlN(s)+AlCl
3(g)=3AlCl(g)+N
2(g) （b）
3AlCl(g)=AlCl
3(g)+2Al(s) （c）
Its purity >94wt.% of the metallic aluminium prepared.
Embodiment 4
As shown in Figure 1, the method for metallic aluminium is prepared in this aluminium nitride chlorination reduction, and its concrete steps are as follows:
Step 1, first will add the carbon (48g) of 3 moles in 1 moles aluminium (102g), then mix and obtain mixture, mixture is pressed into bulk with 50MPa pressure, passing into nitrogen, pressure is 20Pa, under the condition of temperature 1300 DEG C reduction within 5 hours, obtain aluminium nitride (as Suo Shi (a)); Wherein carbon is the carbon dust that granularity is less than 0.5mm, and the intake of nitrogen is 20g/h;
Al
2O
3(s)+3C(s)+N
2(g)=2AlN(s)+3CO(g) （a）
Step 2, stopping pass into nitrogen, the aluminium nitride that step 1 obtains passing into aluminum subchloride steam, the pressure of vacuum system is 20Pa, chlorination disproportionation reaction 1 hour (as shown in (b), (c)) under the condition of temperature 1300 DEG C, the temperature finally controlling condenser is 750 DEG C and on condenser, obtains the easily separated and metallic aluminium of complete crystallization; Aluminum subchloride steam intake is 250g/h;
2AlN(s)+AlCl
3(g)=3AlCl(g)+N
2(g) （b）
3AlCl(g)=AlCl
3(g)+2Al(s) （c）
Its purity >92wt.% of the metallic aluminium prepared.
Embodiment 5
As shown in Figure 1, the method for metallic aluminium is prepared in this aluminium nitride chlorination reduction, and its concrete steps are as follows:
Step 1, first will add the carbon (64g) of 4 moles in 1 moles aluminium (102g), then mix and obtain mixture, mixture is pressed into bulk with 10MPa pressure, passing into nitrogen, pressure is 30Pa, under the condition of temperature 1500 DEG C reduction within 5 hours, obtain aluminium nitride (as Suo Shi (a)); Wherein carbon is the carbon dust that granularity is less than 0.5mm, and the intake of nitrogen is 20g/h;
Al
2O
3(s)+3C(s)+N
2(g)=2AlN(s)+3CO(g) （a）
Step 2, stopping pass into nitrogen, the aluminium nitride that step 1 obtains passing into aluminum subchloride steam, the pressure of vacuum system is 30Pa, chlorination disproportionation reaction 1 hour (as shown in (b), (c)) under the condition of temperature 1500 DEG C, the temperature finally controlling condenser is 800 DEG C and on condenser, obtains the easily separated and metallic aluminium of complete crystallization; Aluminum subchloride steam intake is 250g/h;
2AlN(s)+AlCl
3(g)=3AlCl(g)+N
2(g) （b）
3AlCl(g)=AlCl
3(g)+2Al(s) （c）
Its purity >93wt.% of the metallic aluminium prepared.
By reference to the accompanying drawings the specific embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, various change can also be made under the prerequisite not departing from present inventive concept.
Claims (4)
1. a method for metallic aluminium is prepared in aluminium nitride chlorination reduction, it is characterized in that concrete steps are as follows:
Step 1, first will add the carbon of alumina molar amount 3 ~ 6 times in aluminum oxide, and then mix and obtain mixture, mixture is pressed into bulk with 10MPa ~ 50MPa pressure, passing into nitrogen, pressure is 10
-2under the condition of Pa ~ 50Pa, temperature 1300 ~ 1700 DEG C, reduction obtains aluminium nitride;
The aluminium nitride that step 2, step 1 obtain passing into aluminum subchloride steam, the pressure of vacuum system is 10
-2chlorination disproportionation reaction under the condition of Pa ~ 50Pa, temperature 1300 ~ 1700 DEG C, the temperature finally controlling condenser is 700 ~ 900 DEG C and on condenser, obtains the easily separated and metallic aluminium of complete crystallization.
2. the method for metallic aluminium is prepared in aluminium nitride chlorination reduction according to claim 1, it is characterized in that: the carbon in described step 1 is the carbon dust that granularity is less than 0.5mm.
3. the method for metallic aluminium is prepared in aluminium nitride chlorination reduction according to claim 1, it is characterized in that: the intake of the nitrogen in described step 1 is 15g/h ~ 25g/h.
4. the method for metallic aluminium is prepared in aluminium nitride chlorination reduction according to claim 1, it is characterized in that: the intake of described step 2 middle or low price aluminum chloride steam is 200g/h ~ 300g/h.
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| CN108793101A (en) * | 2018-06-15 | 2018-11-13 | 昆明理工大学 | A kind of method that alumina carbon tropical resources reduction prepares aluminium nitride under vacuum |
| CN109913665A (en) * | 2019-04-11 | 2019-06-21 | 昆明理工大学 | A kind of method that bauxite vacuum distillation prepares metallic aluminium |
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| CN107287423A (en) * | 2017-06-22 | 2017-10-24 | 神雾科技集团股份有限公司 | A kind of continuous aluminium metallurgy device |
| CN107746972A (en) * | 2017-09-19 | 2018-03-02 | 昆明理工大学 | A kind of preparation method of metallic aluminium |
| CN108793101A (en) * | 2018-06-15 | 2018-11-13 | 昆明理工大学 | A kind of method that alumina carbon tropical resources reduction prepares aluminium nitride under vacuum |
| CN109913665A (en) * | 2019-04-11 | 2019-06-21 | 昆明理工大学 | A kind of method that bauxite vacuum distillation prepares metallic aluminium |
| CN109913665B (en) * | 2019-04-11 | 2020-03-10 | 昆明理工大学 | Method for preparing metal aluminum by bauxite vacuum distillation |
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