CN104988335B - A kind of method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition - Google Patents
A kind of method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition Download PDFInfo
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Abstract
The present invention relates to a kind of method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition, belong to vacuum metallurgy technology field.Carbon will be added into aluminum oxide first, is then well mixed and obtains mixed material, mixed material is pressed into bulk, aluminium nitride is obtained being passed through nitrogen, pressure is 10Pa~50Pa, being reduced under conditions of 1300~1700 DEG C of temperature；Obtained aluminium nitride is subjected to 20~60min of pyrolysis under conditions of pressure is 5~60Pa, temperature is 1850~2050K, is subsequently cooled to room temperature, is collected on condenser and obtains the metallic aluminium of well-crystallized.Flow of the present invention is simple, easy to operation, low in raw material price, is easy to get.
Description
Technical field
The present invention relates to a kind of method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition, belong to vacuum metallurgy
Technical field.
Background technology
Aluminium is the metallic element that content is most in the earth's crust, and content is about 8.0%.Content of the aluminium element in the earth's crust occupies the 3rd
Position, its usage amount occupy second, are only second to steel in a metal.And present in nature it is the compound of aluminium, pure aluminum exists
It is not present in nature.Because aluminium easily forms dense oxidation film in dry air with oxygen, formation aluminum oxide makes interior
Layer is not continued oxidation；The purposes of material depends greatly on the property of material.Because aluminium has a variety of premium properties, institute
There is relatively broad purposes with aluminium.
Aluminium and aluminium alloy are that current applications are relatively broad, one of most economical applicable material.Aluminium has low intensity, plasticity good
The advantages of, aluminium is widely used in conducting material, electric wire industry and radio industry.Aluminium alloy be widely used in aircraft,
Process industries such as automobile, train, ship etc..Aluminium also easily forms various aluminum products simultaneously, and is widely used in packaging cigarette, candy
Deng.The surface of aluminium is not easily susceptible to corrode, is often used to manufacture chemical reactor, Medical treatment device because there is the oxide film of densification
Tool, refrigerating plant, petroleum refining device, oil and natural gas pipeline etc..
At present, all aluminium is all extracted by electrolysis from aluminum oxide in the world.Aluminium electrolytic industry is using suddenly
Er-Ai Lu cryolite-alumina molten salt electrolysis, i.e., for the fluoride salt based on ice crystal as flux, aluminum oxide is molten matter group
Into multiphase electrolyte system.And the aluminium electrolysis process needs to consume ample resources, substantial amounts of greenhouse gases and perfluor carbonization is discharged
Thing toxic gas (PFCs).
In the research of aluminum smelting technology new method, both at home and abroad mainly around blast furnace aluminium metallurgy method, ionic liquid electrolysis, direct carbon
Thermal reduction and indirect carbothermic method（Chloridising, nitriding）Etc. carry out the work.By aluminium nitride extraction metallic aluminium
Research focuses primarily upon electrolysis, and in theory, at 700 DEG C, aluminium nitride is decomposed into aluminium and nitrogen, the theoretical decomposition voltage of aluminium nitride
For 0.75V.This decomposition voltage compares AlCl3(l), Al2S3And Al (s)2O3(s) decomposition voltage is low at that same temperature.From heat
From the viewpoint of mechanics, electrolysis has good potentiality, available for extracting aluminium from aluminium nitride.But one of significant challenge faced
It is difficult to find a kind of highly stable AlN (s) of appropriate electrolyte dissolution to be.Bonomi et al. is to 660-700 DEG C of (Li3N-
LiCl) solubility of electrolyte and AlN molten-salt electrolysis have carried out limited research.The current efficiency of this system is 83%, cloudy
Electrode current density about 1.5A/cm2.Final result shows that this process does not succeed.Goto et al. uses LiCl-KCl-Li3N fused salts
System depositing Al N thin film on aluminium base.Yan et al. CaCl at a temperature of 1133k2-Direct Electrochemistry has been carried out in NaCl melts
Reduction nitridation aluminium is tested, and fine aluminium drop is finally observed on minus plate, but this experimentation only has 3-5% yield.West
Pacify technology physicses institute of University of Electronic Science and Technology and superhigh temperature structural composite material science and techniques of defence key lab of Northwestern Polytechnical University
Based on the stability study of aluminium nitride material under high-temperature vacuum, thermodynamic behavior analysis is carried out to AlN and is drawn in standard state
Lower AlN decomposition temperature is 2708K, is in vacuumPa、Pa、During Pa, AlN heat decomposition temperature is respectively
1556K, 1454K, 1365K, AlN stability decline with the rising of vacuum.Dewan et al. is obtained by calculation of thermodynamics
Go out when pressure drops to 0.1KPa, the pyrolysis temperature of aluminium nitride can drop to 1700 DEG C.
The present patent application is the vacuum of vacuum metallurgy national engineering laboratory of Kunming University of Science and Technology long campaigns non-ferrous metal
Emtallurgy research works, and the characteristics of for aluminium nitride pyrolysis, the alumina high temperature vacuum carbon tropical resources of proposition prepare nitridation
Aluminium（1850-2050K、5-60Pa）Thermal decomposition prepares the thinking of metallic aluminium, and metallic aluminium has been prepared.This method effectively overcomes
Electrolysis prepare the Process Energy consumption of aluminium greatly and be not easy to find suitable electrode material the shortcomings that, to prepare aluminium propose one
The new method of kind.The principle of this method is：Under elevated temperature in vacuo aluminium nitride, Jin Eryou are prepared by alumina carbon tropical resources
Aluminium nitride high-temperature vacuum pyrolysis prepares metallic aluminium, and AlN is decomposed into metallic aluminium and N2 under about 1850 ~ 2050K, 5-60Pa
(g), react as follows：
（1850~2050K、5~60Pa）
The present invention has the features such as raw materials for production are cheap, are easy to get, and technological process is short, simple to operate.
The content of the invention
For the above-mentioned problems of the prior art and deficiency, the present invention provides one kind and uses alumina carbon tropical resources Vacuum Heat
The method that decomposition prepares metallic aluminium.Raw material of the present invention using aluminum oxide as extraction metallic aluminium, carbon is reducing agent, is passed through nitrogen, is led to
Crossing addition on reduction nitridation process makes aluminum oxide be transformed into aluminium nitride, the vacuum that aluminium nitride is 5~60Pa in the pressure of vacuum system
In stove, the solid metal aluminium that well-crystallized is made is thermally decomposed under conditions of temperature is 1850-2050K, reduces the life of metallic aluminium
Cost is produced, the present invention is achieved through the following technical solutions.
A kind of method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition, it is comprised the following steps that：
Step 1, the carbon that will add 3 ~ 6 times of alumina molar amount into aluminum oxide first, are then mixed
Material, mixed material is pressed into bulk with 10MPa~50MPa pressure, be passed through nitrogen, pressure be 10Pa~50Pa, temperature
Reduction obtains aluminium nitride under conditions of 1300~1700 DEG C（Such as（a）It is shown）；
Al2O3(s)+3C(s)+N2(g)=2AlN(s)+3CO(g) （a）
Step 2, the aluminium nitride that step 1 obtains entered under conditions of pressure is 5~60Pa, temperature is 1850~2050K
20~60min of row pyrolysis（Such as（b）It is shown）, room temperature is subsequently cooled to, is collected on condenser and obtains well-crystallized's
Metallic aluminium.
（b）
Carbon is the carbon dust that granularity is less than 0.5mm in the step 1.
The beneficial effects of the invention are as follows：Flow of the present invention is simple, easy to operation, low in raw material price, is easy to get, during nothing
Any other additive and coal fuel etc. need to be added.
Brief description of the drawings
Fig. 1 is present invention process flow chart；
Fig. 2 is the XRD for the metallic aluminium that the vacuum of the embodiment of the present invention 1 thermally decomposes to yield.
Embodiment
With reference to the accompanying drawings and detailed description, the invention will be further described.
Embodiment 1
As shown in figure 1, the method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition, its specific steps is such as
Under：
Step 1, first will be to 1mol aluminum oxide（102g）The middle carbon for adding 4 times of alumina molar amount（4mol, 48g）, so
Afterwards be well mixed obtain mixed material, mixed material is pressed into bulk with 30MPa pressure, be passed through 25g/h nitrogen, pressure is
5h is reduced under conditions of 50Pa, 1700 DEG C of temperature and obtains aluminium nitride（Such as（a）It is shown）；Wherein carbon is the carbon that granularity is less than 0.5mm
Powder；
Al2O3(s)+3C(s)+N2(g)=2AlN(s)+3CO(g) （a）
Step 2, the 3mol aluminium nitride for obtaining step 1（123g）Enter under conditions of pressure is 60Pa, temperature is 2050K
Row pyrolysis 20min（Such as（b）It is shown）, room temperature is subsequently cooled to, is collected on condenser and obtains the metal of well-crystallized
Aluminium.
（b）
The metallic aluminium XRD spectrum being prepared is as shown in Fig. 2 its purity>95wt.%.
Embodiment 2
As shown in figure 1, the method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition, its specific steps is such as
Under：
Step 1, first will be to 1mol aluminum oxide（102g）The middle carbon for adding 5 times of alumina molar amount（5mol, 60g）, so
Afterwards be well mixed obtain mixed material, mixed material is pressed into bulk with 20MPa pressure, be passed through 15g/h nitrogen, pressure is
5h is reduced under conditions of 10Pa, 1600 DEG C of temperature and obtains aluminium nitride（Such as（a）It is shown）；Wherein carbon is the carbon that granularity is less than 0.5mm
Powder；
Al2O3(s)+3C(s)+N2(g)=2AlN(s)+3CO(g) （a）
Step 2, the 2mol aluminium nitride for obtaining step 1（82g）Enter under conditions of pressure is 40Pa, temperature is 2000K
Row pyrolysis 30min（Such as（b）It is shown）, room temperature is subsequently cooled to, is collected on condenser and obtains the metal of well-crystallized
Aluminium.
（b）
Its purity of the metallic aluminium being prepared>98wt.%.
Embodiment 3
As shown in figure 1, the method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition, its specific steps is such as
Under：
Step 1, first will be to 1mol aluminum oxide（102g）The middle carbon for adding 6 times of alumina molar amount（6mol, 72g）, so
Afterwards be well mixed obtain mixed material, mixed material is pressed into bulk with 40MPa pressure, be passed through 20g/h nitrogen, pressure is
5h is reduced under conditions of 30Pa, 1600 DEG C of temperature and obtains aluminium nitride（Such as（a）It is shown）；Wherein carbon is the carbon that granularity is less than 0.5mm
Powder；
Al2O3(s)+3C(s)+N2(g)=2AlN(s)+3CO(g) （a）
Step 2, the 0.5mol aluminium nitride for obtaining step 1（20.5g）In the condition that pressure is 20Pa, temperature is 1950K
Lower progress pyrolysis 40min（Such as（b）It is shown）, room temperature is subsequently cooled to, is collected on condenser and obtains well-crystallized's
Metallic aluminium.
（b）
Its purity of the metallic aluminium being prepared>92wt.%.
Embodiment 4
As shown in figure 1, the method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition, its specific steps is such as
Under：
Step 1, first will be to 1mol aluminum oxide（102g）The middle carbon for adding 3 times of alumina molar amount（3mol, 48g）, so
Afterwards be well mixed obtain mixed material, mixed material is pressed into bulk with 50MPa pressure, be passed through 20g/h nitrogen, pressure is
5h is reduced under conditions of 20Pa, 1300 DEG C of temperature and obtains aluminium nitride（Such as（a）It is shown）；Wherein carbon is the carbon that granularity is less than 0.5mm
Powder；
Al2O3(s)+3C(s)+N2(g)=2AlN(s)+3CO(g) （a）
Step 2, the 1mol aluminium nitride for obtaining step 1（41g）Enter under conditions of pressure is 10Pa, temperature is 1900K
Row pyrolysis 50min（Such as（b）It is shown）, room temperature is subsequently cooled to, is collected on condenser and obtains the metal of well-crystallized
Aluminium.
（b）
Its purity of the metallic aluminium being prepared>95wt.%.
Embodiment 5
As shown in figure 1, the method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition, its specific steps is such as
Under：
Step 1, first will be to 1mol aluminum oxide（102g）The middle carbon for adding 4 times of alumina molar amount（4mol, 64g）, so
Afterwards be well mixed obtain mixed material, mixed material is pressed into bulk with 10MPa pressure, be passed through 20g/h nitrogen, pressure is
5h is reduced under conditions of 30Pa, 1500 DEG C of temperature and obtains aluminium nitride（Such as（a）It is shown）；Wherein carbon is the carbon that granularity is less than 0.5mm
Powder；
Al2O3(s)+3C(s)+N2(g)=2AlN(s)+3CO(g) （a）
Step 2, the 1.5mol aluminium nitride for obtaining step 1（61.5g）In the condition that pressure is 20Pa, temperature is 1850K
Lower progress pyrolysis 60min（Such as（b）It is shown）, room temperature is subsequently cooled to, is collected on condenser and obtains well-crystallized's
Metallic aluminium.
（b）
Its purity of the metallic aluminium being prepared>92wt.%.
Above in association with accompanying drawing to the present invention embodiment be explained in detail, but the present invention be not limited to it is above-mentioned
Embodiment, can also be before present inventive concept not be departed from those of ordinary skill in the art's possessed knowledge
Put that various changes can be made.
Claims (2)
- A kind of 1. method for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition, it is characterised in that comprise the following steps that：Step 1, the carbon that 3 ~ 6 times of alumina molar amount will be added into aluminum oxide first, then it is well mixed and obtains mixed material, Mixed material is pressed into bulk with 10MPa~50MPa pressure, be passed through nitrogen, pressure be 10Pa~50Pa, 1300 DEG C of temperature Under conditions of reduction obtain aluminium nitride；Step 2, the aluminium nitride that step 1 obtains is carried out to heat under conditions of pressure is 5~20Pa, temperature is 1850~2050K 20~60min of decomposition reaction, is subsequently cooled to room temperature, is collected on condenser and obtains the metallic aluminium of well-crystallized.
- 2. the method according to claim 1 for preparing metallic aluminium with alumina carbon tropical resources vacuum thermal decomposition, its feature exist In：Carbon is the carbon dust that granularity is less than 0.5mm in the step 1.
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| CN106392099B (en) * | 2016-06-08 | 2018-08-31 | 昆明理工大学 | A kind of preparation method of aluminium oxide/aluminium composite superfine powder |
| CN107746972A (en) * | 2017-09-19 | 2018-03-02 | 昆明理工大学 | A kind of preparation method of metallic aluminium |
| WO2019077970A1 (en) * | 2017-10-18 | 2019-04-25 | 株式会社アルバック | Ion source and ion injection device |
| 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 |
| CN109518004B (en) * | 2018-11-26 | 2019-10-29 | 昆明理工大学 | A kind of method that carbon thermal reduction prepares metallic aluminium |
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| CN1304613C (en) * | 2005-10-18 | 2007-03-14 | 昆明理工大学 | Vacuum carbon heat reduction aluminium smelting method |
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