CN103233122A - Method for preparing metal magnesium by carbothermic reduction of magnesium ores - Google Patents
Method for preparing metal magnesium by carbothermic reduction of magnesium ores Download PDFInfo
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- CN103233122A CN103233122A CN2013101627580A CN201310162758A CN103233122A CN 103233122 A CN103233122 A CN 103233122A CN 2013101627580 A CN2013101627580 A CN 2013101627580A CN 201310162758 A CN201310162758 A CN 201310162758A CN 103233122 A CN103233122 A CN 103233122A
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Abstract
The invention discloses a method for preparing metal magnesium by carbothermic reduction of magnesium ores and belongs to the smelting field of nonferrous metals. The technical process comprises the following steps of: metering, crushing and uniformly mixing magnesium ores, elementary magnesium, carbon-containing alloy and auxiliaries in a certain proportion; filling the mixture to a reaction tank for carrying out thermal decomposition under the conditions that the vacuum degree is 100Pa-101325Pa and temperature is 800 DEG C to 1250 DEG C; and carrying out thermal reduction under the conditions that the vacuum degree is 1Pa-20Pa and temperature is 1000 DEG C to 1250 DEG C, collecting the generated magnesium steam and condensing the magnesium steam onto condensed metal magnesium. The method has the advantages of short process flow, high production efficiency, high resource utilization rate and the like.
Description
Technical field
The present invention relates to the method that a kind of vacuum carbothermal reduction magnesium ore deposit prepares MAGNESIUM METAL, belong to smelting field of nonferrous metal.
Background technology
The preparation of former magnesium has electrolytic process and vacuum-thermal method, and commonly used is vacuum-thermal method.According to the difference of reductive agent, vacuum-thermal method can be divided into silicothermic process, carbide reduction process and carbothermic method etc. again.Silicothermic process adopts ferrosilicon reduction-oxidation magnesium, and common technology has Pidgeon process, mug(unit of measure) Nei Mufa and bohr Zha Nuofa, based on Pidgeon process.
The technical process that existing vacuum-thermal reduction prepares MAGNESIUM METAL is generally: the ore of (1) calcining containing metal element, preparation metal oxide; (2) metal oxide is refined as particle; (3) will mix and briquetting after metal oxide and reductive agent, the auxiliary agent metering; (4) lumpy material is put into the vacuum reducing jar and reacted, obtain metal vapors and be condensed into the condensed state metal.
The subject matter that existing vacuum-thermal reduction prepares the technology of MAGNESIUM METAL has: reactant is the block that solid granulates is formed, the heat transmission, the mass transport that reach between the particle between the block are not smooth, the block central part is difficult to be heated, be difficult to participate in reaction, resource, the energy are difficult to obtain good utilization; Calcining, thermal reduction are carried out in distinct device in the technical process, long flow path, and Btu utilization is difficult for fully, and production efficiency is low.The invention provides the novel method that a kind of vacuum-thermal reduction that effectively addresses these problems prepares MAGNESIUM METAL.
Summary of the invention
The present invention is directed to existing thermal reduction and prepare in the method for MAGNESIUM METAL, the preparation process complexity, the production cycle is long, and problems such as efficient is low, energy consumption height provide a kind of novel method that can significantly simplify preparation process, improve the Energy resources utilization ratio.
For achieving the above object, present method by the following technical solutions:
(1) ready reaction material: the mixture, auxiliary agent Calcium Fluoride (Fluorspan) etc. of alloy that comprises magnesium ore, reductive agent simple substance carbon and the carbon containing of reduction to be decomposed in the raw material.Wherein magnesium ore is rhombspar or magnesite; In the reductive agent alloy of carbon containing consist of carbon 1.5-6.7%wt, iron 93.3-98.5%wt, and in the tin, manganese, cerium one or more, the solidus temperature of this alloy is 500-1250 ℃.In the raw material volume of the alloy of carbon containing be other component cumulative volumes 1-20 doubly; In the alloy of carbon containing and the mixture of simple substance carbon the total amount of carbon be the thermal reduction reaction stoichiometric point 1.05-10 doubly; The consumption of Calcium Fluoride (Fluorspan) is the 0.5-5%wt of nonmetallic ingredient total amount in the raw material.
(2) pack into after metering reduction jar of reaction mass is that 100-101325Pa, temperature are thermolysis under 800-1250 ℃ the condition in vacuum tightness; Adjust vacuum tightness afterwards and be 1-20Pa, temperature and be 1000-1250 ℃ and carry out thermal reduction, obtain metal vapors.
(3) collect metal vapors and condensation and obtain the condensed state metal.
(4) after reaction was finished, remaining metalliferous material also was used for thermal reduction again and prepares the non-ferrous metal flow process in the collection reduction jar, perhaps makes his usefulness in addition.
Simultaneously, in the reduction reaction process, can be by measures such as stirring reaction material or rotation reduction jars, the forced disturbance reaction mass promotes reaction to carry out.
Compared with prior art, present invention can be implemented in the same retort high-level efficiency and finish magnesium ore and decompose and reduction process, technology, economy, resource, source benefit are good.
Embodiment
Further specify the specific embodiment of the present invention below in conjunction with embodiment.
Embodiment 1
(1) ready reaction material, reaction mass contains alloy and the CaF that MgO is 21.7% ground dolomite, simple substance carbon, carbon containing by theory
2Form, the ratio of batching quality is rhombspar: simple substance carbon: CaF
2=100:36:5, the ratio of the quality of each component of the alloy of carbon containing is: iron: carbon: tin=94:5:1, volume are rhombspar, simple substance carbon and CaF
25 times of volume sum are with rhombspar, simple substance carbon and CaF
2Grind into powder.
(2) with alloy and the CaF of rhombspar, simple substance carbon, carbon containing
2Put into the vacuum reaction jar, be evacuated to 10000Pa, be heated to 1000 ℃, be incubated 0.5 hour, carry out pyrolysis.
(3) adjusting vacuum tightness afterwards is 1Pa, and temperature is 1150 ℃, carries out thermal reduction reaction 0.5 hour, obtains magnesium vapor and the cool condensed state MAGNESIUM METAL that obtains with fixed attention.
Embodiment 2
(1) ready reaction material, reaction mass contains the alloy composition that MgO is 47.8% magnesite breeze, simple substance carbon, carbon containing by theory, the ratio of batching quality is magnesite: simple substance carbon=100:36, the ratio of the quality of each component of the alloy of carbon containing is iron: carbon: manganese=94:5:1, volume is magnesite, simple substance carbon volume sum 20 times, and magnesite, simple substance carbon are made powder.
(2) alloy of magnesite, simple substance carbon, carbon containing is put into the vacuum reaction jar, be evacuated to 1500Pa, be heated to 1000 ℃, be incubated 0.5 hour, carry out pyrolysis.
(3) adjusting vacuum tightness afterwards is 10Pa, and temperature is 1150 ℃, carries out thermal reduction reaction 0.5 hour, obtains magnesium vapor and the cool condensed state MAGNESIUM METAL that obtains with fixed attention.
(4) reclaim alloy and the recycle of reacting the remaining carbon containing in back.
Claims (9)
1. a carbothermic reduction magnesium ore deposit prepares the method for MAGNESIUM METAL, and raw material is made up of magnesium ore deposit, reductive agent and auxiliary agent, it is characterized in that, raw material is that 100-101325Pa, temperature are thermolysis in 800-1250 ℃ the retort in vacuum tightness; Adjust vacuum tightness afterwards and be 1-20Pa, temperature and be 1000-1250 ℃ and carry out thermal reduction that the metal vapors that restores obtains the condensed state MAGNESIUM METAL after condensation.
2. carbothermic reduction magnesium according to claim 1 ore deposit prepares the method for MAGNESIUM METAL, it is characterized in that, described reductive agent is the mixture of the alloy of simple substance carbon and carbon containing, wherein the alloy of carbon containing consists of carbon 1.5-6.7%wt, iron 93.3-98.5%wt, and in the tin, manganese, cerium one or more, the solidus temperature of this alloy is 500-1250 ℃.
3. carbothermic reduction magnesium according to claim 1 ore deposit prepares the method for MAGNESIUM METAL, it is characterized in that, in the alloy of described carbon containing and the mixture of simple substance carbon the total amount of carbon for the 1.05-10 of the stoichiometric point of carbothermic reduction magnesium oxide reaction carbon doubly.
4. carbothermic reduction magnesium according to claim 1 ore deposit prepares the method for MAGNESIUM METAL, it is characterized in that, in the raw material volume of the alloy of carbon containing be other component cumulative volumes 1-20 doubly.
5. carbothermic reduction magnesium according to claim 1 ore deposit prepares the method for MAGNESIUM METAL, it is characterized in that described magnesium ore deposit is rhombspar or magnesite, and its particle size is 0.01-100mm.
6. carbothermic reduction magnesium according to claim 1 ore deposit prepares the method for MAGNESIUM METAL, it is characterized in that described simple substance carbon is coke, coal, graphite or the material that at high temperature can generate carbon, and its particle size is 0.005-2mm.
7. carbothermic reduction magnesium according to claim 1 ore deposit prepares the method for MAGNESIUM METAL, it is characterized in that the material in the forced disturbance retort.
8. carbothermic reduction magnesium according to claim 1 ore deposit prepares the method for MAGNESIUM METAL, it is characterized in that, after reaction is finished, collects the metalliferous material in the retort and is used for thermal reduction again and prepare the flow process of MAGNESIUM METAL or do his in addition and use.
9. carbothermic reduction magnesium according to claim 1 ore deposit prepares the method for MAGNESIUM METAL, it is characterized in that CO, CO that reaction produces
2For decomposing and thermal reduction provides heat energy in the magnesium ore deposit.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110055409A (en) * | 2019-04-29 | 2019-07-26 | 安徽工业大学 | A kind of Smelting magnesium technique of exhaust gas waste residue recoverable |
CN113073211A (en) * | 2021-03-17 | 2021-07-06 | 西安交通大学 | Method for directly reducing powder into magnesium metal under inert gas carrying |
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CN1152032A (en) * | 1995-12-14 | 1997-06-18 | 高翔铎 | Fast vacuum-producing method in magnesium smelting |
CN101397609A (en) * | 2008-09-18 | 2009-04-01 | 昆明理工大学 | Method for preparing magnesium metal by giobertite vacuum carbon thermal reduction |
CN101560603A (en) * | 2009-05-21 | 2009-10-21 | 北京华夏建龙矿业科技有限公司 | Method for preparing magnesium metal and by-product by vacuum carbothermic reduction with serpentine minerals |
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CN102277506A (en) * | 2011-08-01 | 2011-12-14 | 开泰镁业有限公司 | Process of smelting magnesium by use of heating method |
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CN1152032A (en) * | 1995-12-14 | 1997-06-18 | 高翔铎 | Fast vacuum-producing method in magnesium smelting |
CN101397609A (en) * | 2008-09-18 | 2009-04-01 | 昆明理工大学 | Method for preparing magnesium metal by giobertite vacuum carbon thermal reduction |
CN101560603A (en) * | 2009-05-21 | 2009-10-21 | 北京华夏建龙矿业科技有限公司 | Method for preparing magnesium metal and by-product by vacuum carbothermic reduction with serpentine minerals |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110055409A (en) * | 2019-04-29 | 2019-07-26 | 安徽工业大学 | A kind of Smelting magnesium technique of exhaust gas waste residue recoverable |
CN113073211A (en) * | 2021-03-17 | 2021-07-06 | 西安交通大学 | Method for directly reducing powder into magnesium metal under inert gas carrying |
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Application publication date: 20130807 |