CN109055753A - A kind of method that alumina carbon thermal reduction prepares metallic aluminium - Google Patents

A kind of method that alumina carbon thermal reduction prepares metallic aluminium Download PDF

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Publication number
CN109055753A
CN109055753A CN201810852461.XA CN201810852461A CN109055753A CN 109055753 A CN109055753 A CN 109055753A CN 201810852461 A CN201810852461 A CN 201810852461A CN 109055753 A CN109055753 A CN 109055753A
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China
Prior art keywords
sintering
metallic aluminium
carbon dust
present
alumina powder
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CN201810852461.XA
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Inventor
陈秀敏
周志强
胥有利
韩晨琛
杨斌
徐宝强
蒋文龙
郁青春
刘大春
马文会
戴永年
邓勇
熊恒
吴鉴
王飞
田阳
杨佳
曲涛
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Priority to CN201810852461.XA priority Critical patent/CN109055753A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00General methods of reducing to metals
    • C22B5/02Dry methods smelting of sulfides or formation of mattes
    • C22B5/10Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B21/00Obtaining aluminium
    • C22B21/02Obtaining aluminium with reducing

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The present invention provides a kind of methods that alumina carbon thermal reduction prepares metallic aluminium, it is suppressed after alumina powder, carbon dust and water are mixed, then the first sintering is carried out at 800~1000 DEG C, finally 1400~1600 DEG C of second sintering of progress under vacuum conditions, obtain metallic aluminium.The present invention is using alumina powder as silicon source, and using carbon dust as reducing agent, the first sintering is carried out at 800~1000 DEG C, and then 1400~1600 DEG C of second sintering of progress, reduction obtain metallic aluminium under vacuum conditions.The present invention reduces the temperature of carbothermic reduction reaction, obtains metallic aluminium at a lower temperature, reduce energy consumption, and without the generation of PFCs gas in preparation process by the second sintering under multi-steps sintering and vacuum condition.The experimental results showed that method provided by the invention is simple, low energy consumption, does not generate perfluorinated hydrocarbon, does not generate the substances such as red mud.

Description

A kind of method that alumina carbon thermal reduction prepares metallic aluminium
Technical field
The present invention relates to technical field of metal material preparation, in particular to a kind of alumina carbon thermal reduction prepares metallic aluminium Method.
Background technique
Aluminium is a kind of metal of the silvery white with thermal conductive resin, electric conductivity and chemical property wave very living, aluminium element Content in the earth's crust accounts for about 8.8%.Metallic aluminium is with density is low, corrosion resistance is excellent, thermal conductivity is good, elasticity modulus The advantages that high.Aluminium alloy has many advantages, such as light-weight, corrosion-resistant, easy conductive, easily extends, and is widely used in communications and transportation, packet The every field such as dress, building, electrical, aerospace and military affairs.In the metal material that the mankind use, the consumption figure of aluminium is only second to Steel, it has also become the second largest metal.
The metallurgy of aluminium it is with a long history, France in 1845 begin to chemical method produce aluminium, by many years to aluminum electrolysis technology Continuous research, electrolytic aluminium have become the world produce the most important method of aluminium.Currently, the method for aluminium metallurgy is broadly divided into two major classes: Electrolysis method and thermal reduction.The former mainly includes that aluminium oxide-cryolite fused salt electrolysis method and chlorination aluminium reduction process, the latter mainly wrap Include electrothermal way and carbothermic method.
But that there are process flows is various, building equipment investment is big, energy consumption is high, has greenhouse gases and perfluorocarbon for electrolysis method The disadvantages of discharge of compound (PFCs), generation red mud, and pollutant is very serious for the harm of human body and environment.Electrothermal way Also although primary aluminum is able to solve the problem of pollution, but cost is higher compared with electrolysis method, causes it in fine aluminium industrially without big prospect. The mode of carbothermic method is mainly blast furnace aluminium metallurgy, and principle is to be reduced directly aluminium oxide with carbon, and the technology of blast furnace aluminium metallurgy is similar In blast furnace ironmaking, but higher temperature (2000~2200 DEG C) is needed relative to blast furnace ironmaking, energy consumption is still higher.
Summary of the invention
The purpose of the present invention is to provide a kind of methods that alumina carbon thermal reduction prepares metallic aluminium.Side provided by the invention Low energy consumption for method, and does not generate PFCs gas.
The present invention provides a kind of methods that alumina carbon thermal reduction prepares metallic aluminium, comprising the following steps:
(1) it is suppressed after mixing alumina powder, carbon dust and water, obtains green compact;
(2) green compact for obtaining the step (1) carries out the first sintering, obtains dry body;It is described first sintering temperature be 800~1000 DEG C;
(3) dry body that the step (2) obtains is subjected to the second sintering under vacuum conditions, obtains metallic aluminium;Described The temperature of two sintering is 1400~1600 DEG C.
Preferably, the mass ratio of alumina powder and carbon dust is 7:(3~5 in the step (1)).
Preferably, in the step (1) water quality be alumina powder and carbon dust gross mass 1/ (8~10).
Preferably, the material of the carbon dust is one of coke, petroleum coke and coking coal or a variety of.
Preferably, the partial size of the coke is 200 mesh or less.
Preferably, the partial size of the alumina powder is 200 mesh or less.
Preferably, the time of the first sintering is 30~60min in the step (2).
Preferably, the time of the first sintering is 30~90min in the step (3).
Preferably, the pressure of vacuum condition is 0.05~1Pa in the step (3).
Preferably, the pressure suppressed in the step (1) is 5~10MPa.
The present invention provides a kind of methods that alumina carbon thermal reduction prepares metallic aluminium, comprising the following steps: by aluminium oxide It is suppressed after powder, carbon dust and water mixing, the first sintering is then carried out at 800~1000 DEG C, finally under vacuum conditions 1400 ~1600 DEG C carry out the second sintering, obtain metallic aluminium.The present invention is using alumina powder as silicon source, using carbon dust as reducing agent, 800~ 1000 DEG C carry out the first sintering, and then 1400~1600 DEG C of second sintering of progress, reduction obtain metallic aluminium under vacuum conditions.This Invention reduces the temperature of carbothermic reduction reaction, in lower temperature by the second sintering under multi-steps sintering and vacuum condition Metallic aluminium is obtained under degree, reduces energy consumption, and without the generation of PFCs gas in preparation process.The experimental result of embodiment Show that method provided by the invention is simple, low energy consumption, does not generate perfluorinated hydrocarbon, does not generate the substances such as red mud, the dirt to environment Dye is substantially reduced.
Detailed description of the invention
Fig. 1 is the process flow chart for the method that alumina carbon thermal reduction prepares metallic aluminium in the present invention.
Specific embodiment
The present invention provides a kind of methods that alumina carbon thermal reduction prepares metallic aluminium, comprising the following steps:
(1) it is suppressed after mixing alumina powder, carbon dust and water, obtains green compact;
(2) green compact for obtaining the step (1) carries out the first sintering, obtains dry body;It is described first sintering temperature be 800~1000 DEG C;
(3) dry body that the step (2) obtains is subjected to the second sintering under vacuum conditions, obtains metallic aluminium;Described The temperature of two sintering is 1400~1600 DEG C.
Alumina carbon thermal reduction provided by the invention prepares the process flow chart of the method for metallic aluminium as shown in Figure 1, by oxygen Tabletting obtains metallic aluminium through vacuum carbothermal reduction after change aluminium, carbon source and distilled water mixing.
The present invention suppresses after mixing alumina powder, carbon dust and water, obtains green compact.The present invention is to the aluminium oxide The not special restriction of operation of the mixing of powder, carbon dust and water, using the mixed material well known to those skilled in the art for preparing Technical solution.
In the present invention, the mass ratio of the alumina powder and carbon dust is preferably 7:(3~5), more preferably 7:4.At this In invention, the mass ratio of the alumina powder and carbon dust can be further ensured that alumina powder by sufficiently also within the above range Original, and generate less CO2Isothermal chamber gas.
In the present invention, the partial size of the alumina powder is preferably 200 mesh hereinafter, more preferably 50~150 mesh, most preferably For 100 mesh.The present invention does not have special restriction to the source of the alumina powder, using well known to those skilled in the art commercially available Product.
In the present invention, the material of the carbon dust is one of coke, petroleum coke and coking coal or a variety of.In the present invention In, 200 mesh is hereinafter, more preferably 50~150 mesh, most preferably 100 mesh.The present invention is to the source of the carbon dust without spy Different restriction, using commercial product well known to those skilled in the art.In the present invention, the carbon dust is as reducing agent, Aluminium oxide can be reduced to metallic aluminium under the high temperature conditions.
In the present invention, the quality of the water is preferably 1/ (8~10) of alumina powder and carbon dust gross mass, more preferably 1/9.In the present invention, the water is preferably distilled water.In the present invention, the water energy enough mixes alumina powder and carbon dust equal It is even, it is used to better green compact.
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 alumina powder and carbon dust during follow-up sintering, convenient for also The progress of original reaction.
After obtaining green compact, the green compact is carried out the first sintering by the present invention, obtains dry body.In the present invention, described first The temperature of sintering is 800~1000 DEG C, preferably 850~950 DEG C, more preferably 900 DEG C.In the present invention, described first burns The time of knot is preferably 30~60min, more preferably 40~50min, most preferably 45min.In the present invention, described first burns During knot, water evaporation in green compact, while making the green compact of sintering that there is better performance using the carbonization of coke, with solution Thorax phenomenon is certainly sprayed under vacuum.
The present invention does not have special restriction to the device of first sintering, using vacuum well known to those skilled in the art Heating device.The present invention does not have special restriction to the heating rate for being warming up to first sintering temperature, using ability Heating rate known to field technique personnel.
After obtaining dry body, the dry body is carried out the second sintering by the present invention under vacuum conditions, obtains metallic aluminium.In this hair In bright, the temperature of second sintering is 1400~1600 DEG C, preferably 1500~1550 DEG C, more preferably 1600 DEG C.At this In invention, the time of second sintering is preferably 30~90min, more preferably 40~80min, most preferably 50~70min. In the present invention, the carbothermic reduction reaction for the aluminium oxide that reacts in second sintering process, specific equation are as follows: Al2O3+3C→2Al(g)+3CO。
The present invention does not have special restriction to the heating rate for being warming up to second sintering temperature, using art technology Heating rate known to personnel.The present invention does not have special restriction to the device of second sintering, using this field skill Vacuum heater known to art personnel.The present invention is not special to the heating rate for being warming up to second sintering temperature Restriction, using heating rate well known to those skilled in the art.
In the present invention, the pressure of the vacuum condition is preferably 0.05~1Pa, more preferably 0.06~0.09Pa, most Preferably 0.07~0.08Pa.In the present invention, the vacuum condition is low vacuum, since alumina carbon thermal reduction prepares metal The reaction of aluminium is the reaction that gas volume increases, and the reaction can be effectively facilitated and carry out to the right by reducing vacuum degree, so as to Carbothermic reduction reaction is realized at lower temperature.
The gaseous metal of generation is preferably carried out condensation collection after the completion of the second sintering by the present invention, obtains metallic aluminium. The present invention operates not special restriction by condensation to described, is using condensing unit well known to those skilled in the art It can.
The present invention reduces the temperature of carbothermic reduction reaction by the second sintering under the first sintering and vacuum condition, Metallic aluminium is obtained at a lower temperature, reduces energy consumption, and without the generation of PFCs gas in preparation process.
In order to further illustrate the present invention, preparation gold is heat-treated to alumina carbon provided by the invention below with reference to embodiment The method for belonging to aluminium is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1:
Step 1 matches aluminium oxide and carbon dust according to mass ratio for 7:3, and it is that aluminium oxide and carbon dust are total that quality, which is added, The water of quality 1/8 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 The material is heated to 800 DEG C of sintering 60min first by upper condenser, is extracted vacuum and is controlled pressure in 0.05Pa or so, in temperature Degree arrives the metallic aluminium with metallic luster after keeping the temperature 90min under conditions of being 1400 DEG C.
Embodiment 2:
Step 1 matches aluminium oxide and carbon dust according to mass ratio for 7:4, and it is that aluminium oxide and carbon dust are total that quality, which is added, The water of quality 1/9 is uniformly mixed, tabletting is carried out under the pressure of 6MPa;
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 The material is heated to 900 DEG C of sintering 50min first by upper condenser, is extracted vacuum and is controlled pressure in 0.1Pa or so, in temperature Degree arrives the metallic aluminium with metallic luster after keeping the temperature 75min under conditions of being 1450 DEG C.
Embodiment 3:
Step 1 matches aluminium oxide and carbon dust according to mass ratio for 7:5, and it is that aluminium oxide and carbon dust are total that quality, which is added, The water of quality 1/10 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 The material is heated to 900 DEG C of sintering 50min first by upper condenser, and extraction vacuum controls pressure in 1Pa or so when pressure, To the metallic aluminium with metallic luster after heat preservation 40min under conditions of temperature is 1500 DEG C.
Embodiment 4:
Step 1 matches aluminium oxide and carbon dust according to mass ratio for 7:3, and it is that aluminium oxide and carbon dust are total that quality, which is added, The water of quality 1/10 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 The material is heated to 1000 DEG C of sintering 30min first by upper condenser, is extracted vacuum and is controlled pressure in 0.05Pa, in temperature The metallic aluminium with metallic luster is arrived after keeping the temperature 30min under conditions of being 1600 DEG C.
As can be seen from the above embodiments, method provided by the invention is simple, and low energy consumption, and the CO generated2Isothermal chamber gas Body substantially reduces and does not generate perfluorinated hydrocarbon, does not generate the substances such as red mud, is substantially reduced to the pollution of environment.
The above is only a preferred embodiment of the present invention, it is not intended to limit the present invention in any form.It should It points out, for those skilled in the art, without departing from the principle of the present invention, if can also make Dry improvements and modifications, these modifications and embellishments should also be considered as the scope of protection of the present invention.

Claims (10)

1. a kind of method that alumina carbon thermal reduction prepares metallic aluminium, comprising the following steps:
(1) it is suppressed after mixing alumina powder, carbon dust and water, obtains green compact;
(2) green compact for obtaining the step (1) carries out the first sintering, obtains dry body;It is described first sintering temperature be 800~ 1000℃;
(3) dry body that the step (2) obtains is subjected to the second sintering under vacuum conditions, obtains metallic aluminium;Described second burns The temperature of knot is 1400~1600 DEG C.
2. the method according to claim 1, wherein in the step (1) alumina powder and carbon dust mass ratio For 7:(3~5).
3. method according to claim 1 or 2, which is characterized in that in the step (1) quality of water be alumina powder and 1/ (8~10) of carbon dust gross mass.
4. the method according to claim 1, wherein the material of the carbon dust is in coke, petroleum coke and coking coal It is one or more.
5. method according to claim 1 or 4, which is characterized in that the partial size of the carbon dust is 200 mesh or less.
6. the method according to claim 1, wherein the partial size of the alumina powder is 200 mesh or less.
7. the method according to claim 1, wherein in the step (2) first sintering time be 30~ 60min。
8. the method according to claim 1, wherein in the step (3) first sintering time be 30~ 90min。
9. method according to claim 1 or 8, which is characterized in that the pressure of vacuum condition is 0.05 in the step (3) ~1Pa.
10. the method according to claim 1, wherein the pressure suppressed in the step (1) is 5~10MPa.
CN201810852461.XA 2018-07-27 2018-07-27 A kind of method that alumina carbon thermal reduction prepares metallic aluminium Pending CN109055753A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109797285A (en) * 2019-04-02 2019-05-24 昆明理工大学 A kind of method that the indirect carbon thermal reduction of aluminium oxide prepares metallic aluminium
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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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109797285A (en) * 2019-04-02 2019-05-24 昆明理工大学 A kind of method that the indirect carbon thermal reduction of aluminium oxide prepares metallic aluminium
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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Application publication date: 20181221