CN109913665B - Method for preparing metal aluminum by bauxite vacuum distillation - Google Patents
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Abstract
The invention provides a method for preparing metal aluminum by bauxite vacuum distillation, and belongs to the field of vacuum metallurgy. The method comprises the steps of carrying out first carbothermic reduction under the vacuum condition to volatilize all Si and part of Fe in a pressed blank, then carrying out second carbothermic reduction in nitrogen to obtain a mixture of FeN and AlN, and then carrying out magnetic separation, decarburization and vacuum thermal decomposition to obtain the metal aluminum. The method can be used for directly preparing the metal aluminum from the bauxite, and has the characteristics of low energy consumption, no pollution, high product conversion rate, less aluminum by-products, high purity of the prepared aluminum and the like. The data of the embodiment show that the purity of the metallic aluminum obtained by the preparation method provided by the invention is more than 95%, and the conversion rate is more than 94%.
Description
Technical Field
The invention relates to the technical field of vacuum metallurgy, in particular to a method for preparing metal aluminum by bauxite vacuum distillation.
Background
Aluminum is a light metal with silvery white metallic luster, has the main characteristics of light weight, corrosion resistance, easy conductivity, easy extension, beautiful appearance and the like, has the relative density of 1/3 of steel, and the mechanical strength ratio of some alloys even exceeds that of structural steel. Therefore, the aluminum alloy has a large strength ratio. The alloy is widely applied to the fields of transportation, packaging, construction, electricity, aerospace, military and the like, and is the second largest metal material with the demand next to steel.
The adoption of aluminum ore in China has a long history, and alum is extracted from alunite for medical and industrial application for a long time. The metallic aluminium was originally produced by chemical processes, from Deville, France 1954, by reducing NaCl-AlCl with sodium instead of potassium3The metal aluminum is prepared by the complex salt, and 200t of aluminum is produced in 30 years by the beginning of the production of an electrolytic aluminum plant in 1987. The modern aluminum smelting industry mainly adopts a cryolite-alumina fused salt electrolysis method and an aluminum chloride electrolysis method to smelt aluminum. However, the electrolysis method has the defects of complex process flow, high energy consumption, discharge of greenhouse gases and perfluorocarbons and the like, and causes very serious influence on the environment.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing aluminum metal by vacuum distillation of bauxite. The preparation method provided by the invention has the advantages of low energy consumption and no pollution.
In order to achieve the above object, the present invention provides the following technical solutions:
a method for preparing metal aluminum by bauxite vacuum distillation comprises the following steps:
mixing bauxite, carbon powder and water, and pressing to obtain a pressed blank, wherein the bauxite contains SiO2、FenOxAnd Al2O3；
Carrying out first carbothermic reduction on the pressed compact under a vacuum condition to obtain a first carbothermic product, wherein the temperature of the first carbothermic reduction is 1200-1400 ℃;
performing second carbothermic reduction on the first carbothermic product in a nitrogen atmosphere to obtain a second carbothermic product, wherein the temperature of the second carbothermic reduction is 1500-1700 ℃;
magnetically separating the second carbothermic product to obtain a magnetic separation residue;
decarbonizing the magnetic separation residue to obtain AlN;
and carrying out vacuum thermal decomposition on the AlN to obtain the metal aluminum.
Preferably, the molar ratio of the sum of oxygen and silicon in the bauxite to the carbon powder is 1: 1-1.4.
Preferably, the mass ratio of the sum of the mass of the bauxite and the carbon powder to the mass of the water is 8-10: 1.
preferably, the carbon powder comprises one or more of coke, petroleum coke and coking coal.
Preferably, the particle sizes of the carbon powder and the bauxite are both 200 meshes and below.
Preferably, the pressing pressure is 5-10 MPa.
Preferably, the pressure of the first carbothermic reduction is 10-100 Pa, and the time of the first carbothermic reduction is 60-180 min.
Preferably, the time of the second carbothermic reduction is 60-180 min.
Preferably, the decarbonization temperature is 800-1000 ℃, and the time is 60-180 min.
Preferably, the pressure of the vacuum thermal decomposition is 100-10-3Pa, the temperature is 1550-1700 ℃, and the time is 60-180 min.
The invention provides a method for preparing metal aluminum by bauxite vacuum distillation, which comprises the following steps: mixing bauxite, carbon powder and water, and pressing to obtain a pressed blank, wherein the bauxite contains SiO2、FenOxAnd Al2O3(ii) a Carrying out first carbothermic reduction on the pressed compact under a vacuum condition to obtain a first carbothermic product, wherein the temperature of the first carbothermic reduction is 1200-1400 ℃; performing second carbothermic reduction on the first carbothermic product in a nitrogen atmosphere to obtain a second carbothermic product, wherein the temperature of the second carbothermic reduction is 1500-1700 ℃; magnetically separating the second carbothermic product to obtain a magnetic separation residue; decarbonizing the magnetic separation residue to obtain AlN; and carrying out vacuum thermal decomposition on the AlN to obtain the metal aluminum. The method comprises the steps of performing first carbothermic reduction under a vacuum condition to volatilize all Si and part of Fe in a pressed blank, performing first carbothermic reduction in nitrogen to obtain a mixture of FeN and AlN, and performing magnetic separation, decarburization and vacuum thermal decomposition to obtain the metallic aluminum. The data of the embodiment show that the purity of the metallic aluminum obtained by the preparation method provided by the invention is more than 95%, and the conversion rate is more than 94%.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a flow chart of a process for preparing aluminum metal by vacuum distillation of bauxite in an embodiment of the present invention.
Detailed Description
The invention provides a method for preparing metal aluminum by bauxite vacuum distillation, which comprises the following steps:
mixing bauxite, carbon powder and water, and pressing to obtain a pressed blank, wherein the bauxite contains SiO2、FenOxAnd Al2O3；
Carrying out first carbothermic reduction on the pressed compact under a vacuum condition to obtain a first carbothermic product, wherein the temperature of the first carbothermic reduction is 1200-1400 ℃;
performing second carbothermic reduction on the first carbothermic product in a nitrogen atmosphere to obtain a second carbothermic product, wherein the temperature of the second carbothermic reduction is 1500-1700 ℃;
magnetically separating the second carbothermic product to obtain a magnetic separation residue;
decarbonizing the magnetic separation residue to obtain AlN;
and carrying out vacuum thermal decomposition on the AlN to obtain the metal aluminum.
The invention mixes and presses bauxite, carbon powder and water to obtain pressed compact, wherein the bauxite contains SiO2、FenOxAnd Al2O3. The source of the bauxite and the carbon powder is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
The mixing method of the present invention is not particularly limited, and a mixing method known to those skilled in the art may be used.
In the invention, the mass ratio of the bauxite to the carbon powder to the water is preferably 8-10: 1, more preferably 9: 1. In the present invention, the water is preferably distilled water. In the present invention, the water can be used for a better green compact. .
In the invention, the carbon powder preferably comprises one or more of coke, petroleum coke and coking coal.
In the present invention, the particle sizes of the carbon powder and the bauxite are preferably both 200 mesh and less. In the invention, the carbon powder is used as a reducing agent and can reduce alumina into metallic aluminum under high-temperature conditions.
In the invention, the pressing pressure is preferably 5-10 MPa, more preferably 6-9 MPa, and most preferably 7-8 MPa. In the invention, the pressing can ensure the full contact of the bauxite powder and the carbon powder in the subsequent sintering process, and is convenient for the vacuum carbothermic reaction.
In the invention, the molar ratio of the sum of oxygen and silicon in the bauxite to the carbon powder is preferably 1: 1-1.4, and more preferably 1: 1.2-1.3. In the invention, the mass ratio of the bauxite powder to the carbon powder is within the range, so that the bauxite can be fully reduced, and less CO is generated2And the like.
After a pressed compact is obtained, the pressed compact is subjected to first carbothermic reduction under a vacuum condition to obtain a first carbothermic product, wherein the temperature of the first carbothermic reduction is 1200-1400 ℃.
In the invention, the pressure of the first carbothermic reduction is preferably 10-100 Pa, more preferably 20-80 Pa, and most preferably 30-70 Pa, the time of the first carbothermic reduction is preferably 60-180 min, more preferably 80-160 min, and most preferably 100-140 min, and the temperature of the first carbothermic reduction is preferably 1250-1350 ℃, and more preferably 1300 ℃. In the present invention, during the first carbothermic reduction, all Si and part of Fe in the compact volatilize. In the invention, after all Si and part of Fe are volatilized, compounds containing Si and Fe are obtained by vacuum volatilization and condensation
After the first carbothermic product is obtained, carrying out second carbothermic reduction on the first carbothermic product in a nitrogen atmosphere to obtain a second carbothermic product, wherein the temperature of the second carbothermic reduction is 1500-1700 ℃.
In the invention, the second carbothermic reduction time is preferably 60-180 min, more preferably 80-160 min, and most preferably 100-140 min. In the invention, the pressure of the second carbothermic reduction is preferably 100-500 Pa, more preferably 150-450 Pa, and most preferably 200-400 Pa, and the temperature of the second carbothermic reduction is preferably 1550-1650 ℃, and more preferably 1600 ℃.
In the present invention, the carbothermic reduction of the reacted alumina occurs during the second carbothermic reduction process, which is specified by the following equation：Al2O3+N2(g)+3C＝2AlN+3CO(g)。
After the second carbothermic product is obtained, the second carbothermic product is subjected to magnetic separation to obtain magnetic separation residues. In the present invention, the second carbothermic product is preferably naturally cooled to room temperature and then subjected to magnetic separation. In the present invention, the magnetic separation process can separate Fe-containing substances to obtain a mixture of AlN and C, i.e., a magnetic separation residue.
After the magnetic separation residue is obtained, the magnetic separation residue is decarbonized to obtain AlN. In the invention, the decarburization temperature is preferably 800-1000 ℃, more preferably 850-950 ℃, most preferably 900 ℃, and the time is preferably 60-180 min, more preferably 80-160 min, most preferably 100-140 min.
After AlN is obtained, the AlN is subjected to vacuum thermal decomposition to obtain metal aluminum.
In the invention, the pressure of the vacuum thermal decomposition is preferably 100-10-3Pa, more preferably 50 to 10-2Pa, preferably 1Pa, the temperature is preferably 1550-1700 ℃, more preferably 1570-1630 ℃, most preferably 1600 ℃, and the time is preferably 60-180 min, more preferably 80-160 min, most preferably 100-140 min. In the present invention, the specific equation of the reaction occurring in the vacuum thermal decomposition is: 2AlN ═ 2al (g) + N2(g)。
In an embodiment of the present invention, the vacuum thermal decomposition preferably comprises the steps of: placing AlN into a vacuum furnace after tabletting, closing a furnace door to extract vacuum, starting heating when the pressure is lower than 10Pa, heating the material to a certain target temperature in vacuum thermal decomposition, introducing protective gas to control the pressure to be 10-10-3Pa certain target value and keeping the temperature for 60-180 min to obtain gaseous Al and N2And collecting the generated gaseous Al through a volatilization and condensation device to obtain the metallic aluminum.
In the present invention, the nitrogen gas generated by the vacuum thermal decomposition is preferably recycled to the second carbothermic reduction process.
In the present invention, the protective gas is preferably argon or nitrogen.
The vacuum carbothermic reduction device is not particularly limited, and a vacuum heating device well known to those skilled in the art can be used. The temperature rising rate of the reaction temperature is not particularly limited in the present invention, and a temperature rising rate known to those skilled in the art may be used.
The method for preparing aluminum metal by vacuum distillation of bauxite provided by the present invention is described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
FIG. 1 is a flow chart of a method for preparing aluminum metal by bauxite vacuum distillation according to an embodiment of the present invention, wherein bauxite, carbon powder and water are mixed and then pressed to obtain a pressed compact, and the bauxite contains SiO2、FenOxAnd Al2O3(ii) a Carrying out first carbothermic reduction on the pressed compact under the vacuum condition to obtain Si and Fe-containing gas and Fe and Al-containing compounds (first carbothermic products), and volatilizing and condensing the Si and Fe-containing gas in vacuum to obtain Si and Fe-containing compounds; performing second carbothermic reduction on the first carbothermic product in a nitrogen atmosphere to obtain a second carbothermic product; magnetically separating the second carbothermic product to obtain a magnetic separation residue and a Fe-containing compound; and performing vacuum thermal decomposition on the magnetic separation residue after decarburization to obtain gaseous aluminum and nitrogen, volatilizing and condensing the gaseous aluminum to obtain metal aluminum, and reusing the nitrogen in a second carbothermic reduction process.
Example 1
Step 1, bauxite and carbon powder are mixed according to a molar ratio (n)(O)+n(Si)):n(C)1:1.3, adding water with the total mass of the bauxite and the carbon powder of 1/8, uniformly mixing, and tabletting under the pressure of 5 MPa;
and 2, putting the material obtained in the step 1 into a graphite crucible, covering a condenser on the top of the crucible, closing the vacuum furnace, covering the condenser, extracting vacuum to control the pressure at 10Pa, heating the material to 1300 ℃, preserving the heat for 80 minutes, and volatilizing part of iron and all silicon in the material.
And 3, heating the residual product (the compound of the residual iron and the aluminum) in the step 2 to 1700 ℃, introducing nitrogen to control the pressure at 100Pa, and keeping the temperature for 60 minutes to obtain the product of FeN and AlN.
And 4, when the product obtained in the step 3 is cooled to room temperature, separating the Fe-containing compound by a magnetic separation method to obtain a mixture of AlN and C, heating the mixture containing AlN and C in the air to 800 ℃, and keeping the temperature for 90 minutes for decarburization treatment to finally obtain AlN.
Step 5, placing the obtained AlN pressed sheet into a vacuum furnace, closing a furnace door to extract vacuum, starting heating when the pressure is lower than 10Pa, introducing protective gas when the material is heated to a certain target temperature of 1650 ℃ and controlling the pressure to be 10-3Pa and keeping the temperature for 80 minutes to obtain gaseous Al and gaseous N2And volatilizing, condensing and collecting to obtain metal aluminum, and recycling the nitrogen in the step 3.
The purity of the metallic aluminum prepared by the embodiment is 97% and the yield is 96%.
Example 2
Step 1, bauxite and carbon powder are mixed according to a molar ratio (n)(O)+n(Si)):n(C)1:1.2, adding water with the mass of 1/10 of the total mass of the bauxite and the carbon powder, uniformly mixing, and tabletting under the pressure of 7 MPa;
and 2, putting the material obtained in the step 1 into a graphite crucible, covering a condenser on the top of the crucible, closing the vacuum furnace, covering the condenser, extracting vacuum to control the pressure at 20Pa, heating the material to 1400 ℃, preserving the temperature for 180 minutes, and volatilizing part of iron and all silicon in the material.
And 3, heating the residual product (the compound of the residual iron and the aluminum) in the step 2 to 1500 ℃, introducing nitrogen to control the pressure at 400Pa, and keeping the temperature for 160 minutes to obtain the product of FeN and AlN.
And 4, when the product obtained in the step 3 is cooled to room temperature, separating the Fe-containing compound by a magnetic separation method to obtain a mixture of AlN and C, heating the mixture containing AlN and C in the air to 900 ℃, preserving the heat for 100 minutes and carrying out decarburization treatment to finally obtain AlN.
Step 5, placing the obtained AlN tablets into a vacuum furnace, closing a furnace door to extract vacuum, starting heating when the pressure is lower than 10Pa, and heating the materials to a certain target temperature of 1700 DEG CIntroducing protective gas to control the pressure at 10Pa and keeping the temperature for 100 minutes to obtain gaseous Al and N2And volatilizing, condensing and collecting to obtain metal aluminum, and recycling the nitrogen in the step 3.
The purity of the metallic aluminum prepared by the embodiment is 96 percent and the yield is 95 percent.
Example 3
Step 1, bauxite and carbon powder are mixed according to a molar ratio (n)(O)+n(Si)):n(C)1:1.1, adding water with the total mass of the bauxite and the carbon powder of 1/9, uniformly mixing, and tabletting under the pressure of 10 MPa;
and 2, putting the material obtained in the step 1 into a graphite crucible, covering a condenser on the top of the crucible, closing the vacuum furnace, covering the condenser, extracting vacuum to control the pressure at 50Pa, heating the material to 1200 ℃, preserving the temperature for 60 minutes, and volatilizing part of iron and all silicon in the material.
And 3, heating the residual product (the compound of the residual iron and the aluminum) in the step 2 to 1500 ℃, introducing nitrogen to control the pressure at 500Pa, and keeping the temperature for 160 minutes to obtain the product of FeN and AlN.
And 4, when the product obtained in the step 3 is cooled to room temperature, separating the Fe-containing compound by a magnetic separation method to obtain a mixture of AlN and C, heating the mixture containing AlN and C in the air to 1000 ℃, and keeping the temperature for 180 minutes for decarburization treatment to finally obtain AlN.
And 5, putting the obtained AlN pressed sheet into a vacuum furnace, closing a furnace door to extract vacuum, starting heating when the pressure is lower than 10Pa, heating the material to a certain target temperature of 1500 ℃, introducing protective gas to control the pressure to be 0.1Pa, and preserving the temperature for 80 minutes to obtain gaseous Al and N2And volatilizing, condensing and collecting to obtain metal aluminum, and recycling the nitrogen in the step 3.
The purity of the metallic aluminum prepared by the embodiment is 96% and the yield is 96%.
Example 4
Step 1, bauxite and carbon powder are mixed according to a molar ratio (n)(O)+n(Si)):n(C)The ratio is 1:1.4, the bauxite and the additive are addedMixing water of 1/10 carbon powder total mass, tabletting under 9 MPa;
and 2, putting the material obtained in the step 1 into a graphite crucible, covering a condenser on the top of the crucible, closing the vacuum furnace, covering the condenser, extracting vacuum to control the pressure at 40Pa, heating the material to 1350 ℃, preserving the heat for 140 minutes, and volatilizing part of iron and all silicon in the material.
And 3, heating the residual product (the compound of the residual iron and the aluminum) in the step 2 to 1600 ℃, introducing nitrogen to control the pressure at 450Pa, and preserving the heat for 140 minutes to obtain the product of FeN and AlN.
And 4, when the product obtained in the step 3 is cooled to room temperature, separating the Fe-containing compound by a magnetic separation method to obtain a mixture of AlN and C, heating the mixture containing AlN and C in the air to 850 ℃, preserving the heat for 140 minutes and carrying out decarburization treatment to finally obtain AlN.
Step 5, putting the obtained AlN tablets into a vacuum furnace, closing a furnace door to extract vacuum, starting heating when the pressure is lower than 10Pa, heating the materials to a certain target temperature of 1630 ℃, introducing protective gas to control the pressure to be 0.01Pa, and preserving the temperature for 140 minutes to obtain gaseous Al and N2And volatilizing, condensing and collecting to obtain metal aluminum, and recycling the nitrogen in the step 3.
The purity of the metallic aluminum prepared by the embodiment is 98 percent, and the yield is 97 percent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A method for preparing metal aluminum by bauxite vacuum distillation is characterized by comprising the following steps:
mixing bauxite, carbon powder and water, and pressing to obtain a pressed blank, wherein the bauxite contains SiO2、FenOxAnd Al2O3；
Carrying out first carbothermic reduction on the pressed compact under a vacuum condition to obtain a first carbothermic product, wherein the temperature of the first carbothermic reduction is 1200-1400 ℃; the pressure of the first carbothermic reduction is 10-100 Pa, and the time of the first carbothermic reduction is 60-180 min;
performing second carbothermic reduction on the first carbothermic product in a nitrogen atmosphere to obtain a second carbothermic product, wherein the temperature of the second carbothermic reduction is 1500-1700 ℃; magnetically separating the second carbothermic product to obtain a magnetic separation residue;
decarbonizing the magnetic separation residue to obtain AlN;
and carrying out vacuum thermal decomposition on the AlN to obtain the metal aluminum.
2. The preparation method according to claim 1, wherein the molar ratio of the sum of oxygen and silicon in the bauxite to the carbon powder is 1:1 to 1.4.
3. The preparation method according to claim 1, wherein the mass ratio of the sum of the bauxite and the carbon powder to the water is 8-10: 1.
4. the preparation method according to claim 1, wherein the carbon powder comprises one or more of coke, petroleum coke and coking coal.
5. The production method according to claim 1 or 4, wherein the particle sizes of the carbon powder and the bauxite are both 100 mesh and less.
6. The method according to claim 1, wherein the pressure for pressing is 5 to 10 MPa.
7. The method according to claim 1, wherein the second carbothermic reduction time is 60 to 180 min.
8. The method according to claim 1, wherein the decarburization temperature is 800 to 1000 ℃ for 60 to 180 minutes.
9. The method according to claim 1, wherein the pressure of the vacuum thermal decomposition is 10 to 10%-3Pa, the temperature is 1550-1700 ℃, and the time is 60-180 min.
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