WO2005103309A1 - Processus metallothermique pour la production de magnesium et four a induction sous vide approprie - Google Patents

Processus metallothermique pour la production de magnesium et four a induction sous vide approprie Download PDF

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Publication number
WO2005103309A1
WO2005103309A1 PCT/UA2004/000047 UA2004000047W WO2005103309A1 WO 2005103309 A1 WO2005103309 A1 WO 2005103309A1 UA 2004000047 W UA2004000047 W UA 2004000047W WO 2005103309 A1 WO2005103309 A1 WO 2005103309A1
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WIPO (PCT)
Prior art keywords
magnesium
furnace
mixture
crucible
batch mixture
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PCT/UA2004/000047
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English (en)
Inventor
Oleksandr Dmitriyevich Podoltsev
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Fos International S.A.
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Publication date
Application filed by Fos International S.A. filed Critical Fos International S.A.
Publication of WO2005103309A1 publication Critical patent/WO2005103309A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • C22B26/22—Obtaining magnesium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/02—Light metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00—General methods of reducing to metals
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes
    • C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/06—Crucible or pot furnaces heated electrically, e.g. induction crucible furnaces with or without any other source of heat
    • F27B14/061—Induction furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details peculiar to crucible or pot furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details peculiar to crucible or pot furnaces
    • F27B14/14—Arrangements of heating devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
    • F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B14/00—Crucible or pot furnaces
    • F27B14/08—Details peculiar to crucible or pot furnaces
    • F27B2014/0837—Cooling arrangements
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Definitions

  • This invention relates: to metallothermic process for magnesium production from dispersed calcined dolomite raw using silicon-containing reducing agent, and to vacuum-induction furnace for realization of this process.
  • Background Art It is well known that industrial consumption of magnesium constantly increases, and substantial share of its global market is supplied by metallothermic processes.
  • any metallothermic processing of the calcined dolomite has ecological advantages in comparison with electrochemical production of magnesium from practically waterless magnesium chloride.
  • An available to all Internet-review of « Metallothermic Reduction). http:/www. magnesium.com/w3/data-bank discloses that usual metallothermic process for magnesium production from dolomite raw includes following basic steps: (1 ) preparation of a mixture of dispersed calcined dolomite and dispersed silicon- containing reducing agent (preferably ferrosilicon and, seldom, aluminum-silicon); (2) pressing the mixture to obtain briquettes; (3) loading said briquettes into reactor which comprises an area for heating the briquettes and cooling area for magnesium vapor condensation; (4) heating said briquettes, reducing and sublimation of magnesium at temperature of about 1200°C and under residual pressure less than 670 Pa (preferably less than 400 Pa) with condensation of magnesium vapor in cooling area at temperature in the range of 400°C to 500°C; (5) emptying and new-loading the reactor
  • the heating the mixture at temperature of about 1200°C is needed because the reaction of magnesium oxide reduction with silicon is highly endothermic, and vacuum is needed to lessen of the evaporation of magnesium from a nascent slag.
  • three modifications of metallothermic processes for the industrial magnesium production namely: Pidgeon Process, Bolzano Process, and Magnetherm Process are well known.
  • the above-mentioned step (1) is included into all these processes, and Pidgeon and Bolzano Processes have practically identical all steps of the magnesium production.
  • Pidgeon Process was developed in the forties of XX century. It is carried out in such batch mode reactors as retorts which, after loading the briquettes immediately, must be closed and vacuumed. At the time of processing, at least two such retorts are placed vertically into heating furnace roof. This furnace is heated by liquid and/or gas hydrocarbon fuel.
  • each retort must be located within the furnace space, and the cooling area for magnesium vapor condensation must be located over the said furnace roof. It is well known that even briquetted batch mixture has low thermal conductivity. Therefore, diameter of the retort opening is not more 300 mm usually, and is equal to 275 mm practically. It is well known also that even deep vacuum cannot provide magnesium vapor exhausting out of the lower layers of the batch mixture briquettes. Therefore, extreme height of the retort is usually not more 3.0 m, and their load doesn't reach the half volume. Unfortunately, either of these limitations is insufficient for uniform heating the full mass of the batch mixture with an external heat source. Correspondingly, 24 hours' magnesium yield to one retort averages about 70 kg.
  • mixture must be primarily dried and prepared on base of such dolomite that contains no less than 99,5% calcium and magnesium carbonates and such high-silica ferrosilicon that contains no less than 65%, preferably to 90%, silicon and is taken in amount that exceeds somewhat the stoichiometric relationships. Only fulfillment all these requirements allows to extract no less than 90% magnesium that was contained initially in batch mixture and to provide for its purity no less than 99.95%.
  • More efficient Bolzano Process provides an internal batch mixture heating at temperature about 1200°C and under residual pressure less than 400 Pa.
  • Compact vacuum bell-type furnaces are used thereto. Each such furnace comprises steel housing that includes a cylindrical heating lower section and a removable cylindrical-spheroidal cooling upper section.
  • the lower housing section is lined on the inside by refractory brick and equipped with a support for mixture briquettes and such contactors for connection to a current source that being adjacent tightly to ends of a set of said briquettes when the furnace operates.
  • the upper housing section is equipped with a water jacket and has at least one (as a rule central) opening for connection of the furnace space to a vacuum source and to atmosphere.
  • magnesium vapor permeability of the briquettes set decreases when height and consistence of said set increase. Further, current density and, correspondingly, heat development do not be equal in different cross-sections of said set in principle. Therefore, magnesium wastes with slag is increased in accordance with enhancement of height and volume temperature inhomogeneity of said set.
  • Magnetherm Process includes: (1) preparation of a mixture of dispersed calcined dolomite raw, dispersed silicon- containing reducing agent, and aluminum oxide (that is taken, especially, as alumina); (2) loading a batch mixture into reactor having an area for electrical heating the mixture and nascent slag and cooling area for magnesium vapor condensation; (3) vacuuming the reactor at residual pressure in the range of 400 Pa to 670 Pa, electrical heating the mixture within the reactor at temperature no more than 1200°C sufficient for reduction and sublimation of magnesium, and nascent slag melting at temperature in the range of 1550 to 1600°C; (4) precipitation of magnesium vapor within the cooling area (where temperature is usually no more than 500°C); (5) removal of the slag from the reactor and repeating the production cycle starting with step ( 1 ) when process carrying out in batch mode, or replenishment of the heating area with make-up mixture and at least repeatable slag discharge when process carrying out continuously.
  • a reactor for Magnetherm Process has two parts.
  • a first axisymmetric heated part comprises: a heat-resistant housing that is lined near-bottom by refractory body, a first practically vertical copper nonconsumable electrode rigidly fixed into the housing roof in such a way that its geometrical axis is practically coincident with axis of symmetry of said first part; a graphite lining supported by said refractory body and served as a second practically nonconsumable electrode; a bypass channel for passing the magnesium vapor from underroof space of the said first part into second (condensation) part of the reactor; a tap hole for slag removal from the graphite lining.
  • Second (not necessarily axisymmetric) part has a sectional housing.
  • Upper cone- shaped cooling section of this housing serves as a condenser of the magnesium vapor.
  • This section is connected with said first part by above-mentioned bypass channel and equipped with at least one vertical nipple for connection to a vacuum source and to atmosphere.
  • Lower section of this housing serves as a downtank of base product.
  • each of the known reactors cannot be supplied with easily accessible low-grade row materials such as: above-mentioned fine-dispersed calcined dolomite wastes (because they must be dried thoroughly and at least pelleted before magnesium reduction), and reducing agents contained less than 50% of silicon (because their reduction potential is too small for Magnetherm Process)
  • low-grade row materials such as: above-mentioned fine-dispersed calcined dolomite wastes (because they must be dried thoroughly and at least pelleted before magnesium reduction), and reducing agents contained less than 50% of silicon (because their reduction potential is too small for Magnetherm Process)
  • metallothermic process for magnesium production includes the following steps: preparation of mixture of dispersed at least partially calcined dolomite raw and dispersed silicon-containing reducing agent, loading the batch mixture into a reactor that has an area for heating the batch mixture and a cooling area for magnesium vapor condensation, vacuuming the reactor at residual pressure no more than 670 Pa and heating the batch mixture within the reactor up to temperature no more than 1200°C sufficient for the metallothermic process of magnesium reduction and sublimation, precipitation of magnesium vapor in said cooling area, depressuhzing the reactor, evacuation of the base product from the cooling area and the slag from the heating area to preparation for repeating the production cycle, and, according to the invention, the process further provides use, as reactor, a vacuum induction furnace that has an electroconductive crucible equipped, within the located near the bottom heating area, with at least one additional electroconductive heating element, and, on the upper part, with a cooler on the outside and with a magnesium vapor trap inside, preparation of the mixture from fine-dispersed
  • Synchronous heating of the mixture based on fine-dispersed dolomite raw material, from crucible wall and from at least one additional electroconductive element within furnace space allows: firstly, to reduce magnesium efficiently even if ferrosilicon contains about 45% of silicon, and secondly, to decrease substantially magnesium wastes with slag (up to 4.5% of its basic amount).
  • First and second additional features are consisted, correspondingly, in that partially calcined dolomite powder that is waste of industrial dolomite calcination as fine-dispersed dolomite raw is used, and waste of ferrosilicon production that consists of no less 45% of silicon by weight as reducing agent is used.
  • each loaded into furnace batch mixture is preliminary calcined in contact with atmosphere at temperature in the range of 885°C to 920°C. This temperature interval is the most useful for practically completed dewatering the raw material, destroying the magnesium and calcium hydroxides and carbonates of these metals residue with evacuation of the nascent water vapor and carbon dioxide into atmosphere during usually no more one hour.
  • the problem is also solved in that in the vacuum-induction furnace comprising: a produced from electroconductive material crucible intended for placing and processing of the batch mixture, a removable cover for hermetic seal of the crucible, a heat-insulating mantle and an inductor, which are surrounded the lower part of the crucible, and means for alternate connection the furnace space to a vacuum source or atmosphere, according to the invention the crucible is equipped, within the heating area that meant for placing and processing the metallurgical raw mixture, with at least one additional electroconductive heating element, and, on the upper part, with a cooler on the outside and with a metal vapor trap inside.
  • First additional feature consists in that said additional electroconductive heating elements are selected from group consisting of at least one lateral rod, at least one membrane having at least one through-hole, at least one plate, a spiral insert which has a lead angle that exceeds the angle of free-flowing raw and/or slag friction and is formed as unbroken vane or consequently arranged separate vanes, and an arbitrary set of these component parts.
  • This list includes the most preferable shapes of the additional electroconductive heating elements that can provide for temperature homogenizing within batch mixture and nascent slag mass.
  • Second additional feature consists in that said trap is formed as plug-in shell.
  • Fig.1 shows schematic longitudinal section of a vacuum-induction furnace equipped with an inductor having a single-phase winding
  • Fig.2 shows schematic longitudinal section of a vacuum-induction furnace equipped with an inductor having three-phase winding
  • Fig.3 shows cross-section of a crucible at rod additional electroconductive heating elements level
  • Fig.4 shows cross-section of a crucible at additional electroconductive heating element level (this element is shaped as membrane having a central through-hole)
  • Fig.5 shows cross-section of a crucible at additional electroconductive heating element level (this element is shaped as a membrane having several through-holes)
  • Fig.6 shows schematic longitudinal section of the crucible that equipped with such additional electroconductive heating elements, which are shaped as stepwise mounted plates.
  • a simplest vacuum-induction furnace according to the invention has: a produced from electroconductive (usually ferromagnetic) material preferably plug-in crucible 1 for placing and processing of a batch mixture, a removable cover 2 for hermetic seal of the crucible 1 , a heat-insulating mantle 3 and a having single-phase winding inductor 4, which are surrounded consequently the lower part of the crucible 1 , means for alternate connection the furnace space to a vacuum source or atmosphere, namely: at least one nipple 5 that is connected, as a rule, to the cover 2, and at least one locking and regulating element (e.g., a three-way tap or valve) 6, at least one additional electroconductive (preferably ferromagnetic) heating element 7 that is rigidly connected inside to the wall of lower part of the crucible 1 , a cooler 8 that, at least when operates, surrounded tightly the upper part of the crucible 1 from the outside and formed, as
  • Shapes of cross-section of the crucible 1 may be very various.
  • the crucible 1 is axisymmetric but most preferably, if it would be produced as such piece of an annular cylindrical pipe that equipped with a hermetically welded bottom from below and a flange for fastening the cover 2 at upper end.
  • the inductor 4 having single-phase winding may be connected to an arbitrary alternating (commercial or high frequency) current source. Nevertheless, it is advisable that the furnaces, equipped with such inductors 4, are taken in a divisible by three numbers and combined as tri-furnaces' units.
  • each single-phase winding of each this unit may be connected to a single phase of three-phase alternating current industrial network at a frequency of 50 or 60 hertz.
  • Fig.2 shows vacuum-induction furnace equipped with such inductor 4, the three- phase winding of which meant for connecting to the above-mentioned three-phase industrial network.
  • the heat-insulating mantle 3 is made of a material permeable to electromagnetic field and is fixed between the outside crucible 1 wall and the inductor 4 winding(s).
  • the additional electroconductive heating elements 7 may be various in geometric form and dimensions and may be selected from group consisting of: at least one rod but preferably as a grate composed from transverse or crossing and tight interlocked rods which, in aggregate, are comprise the closed circuit for circular movement of induced eddy currents (see. Fig.3 wherein the curved arrow indicates one of two possibles closed current path), at least one membrane having at least one preferably central through-hole
  • Fig.4 or several through-holes (Fig.5) for batch mixture loading and free-flowing slag removal these membrane, irrespective of shape, number and arrangement of the through-holes, must be providing the such closed circuits for circular movement of induced eddy currents which are indicated by the curved arrows
  • at least one plate but preferably a set arranged stepwise entire or perforated plates see Fig.6
  • a spiral insert not showed apart which has always a lead angle that exceeds the angle of free-flowing raw and/or slag friction and may be formed as unbroken (and perforated usually) vane or preferably as consequently arranged separate (entire or perforated) vanes, and an arbitrary set of these component parts.
  • Metallothermic process for magnesium production using the described furnace includes the following steps: (1 ) preparation of a mixture: a) of a fine-dispersed at least partially calcined dolomite raw material that mainly contains particles with diameter less than 0.1 mm (i.e.
  • tail-end steps namely: (7a) switching off the feed of the inductor 4 for stopping the slag heating that is originated as a result of the chemical reactions between batch mixture ingredients and magnesium sublimation, (7b) depressuhzing the crucible 1 (by switching the locking and regulating element 6 to atmosphere), (7c) pulling-off the cover 2 when pressure in the crucible 1 puts on a par with a barometric pressure current value, (7d) removal of the plug-in shell 9, which contains a bootleg (in this case, magnesium), from the crucible 1, (7e) removal of the slag from the crucible 1 ; and repeating the production cycle as described above.
  • (7a) switching off the feed of the inductor 4 for stopping the slag heating that is originated as a result of the chemical reactions between batch mixture ingredients and magnesium sublimation (7b) depressuhzing the crucible 1 (by switching the locking and regulating element 6 to atmosphere), (7c) pulling-off the cover 2 when pressure in the crucible 1 puts on a par with
  • the total moisture values of the calcined dolomite wastes must be taken into account in the course of usual technical chemical calculations of supply rates of the magnesium oxide containing raw and the silicon-containing raw before preparation of prescribed batch mixture portions. It is preferable to use (and were used) low-silicon wastes of blast-furnace production of ferrosilicon as silicon-containing reducing agent (see Table 2). These wastes are retained today at dumping places of ferrosilicon works in abundance.
  • Table 2 AVERAGED COMPOSITION OF THE FERROSILICON WASTES BEFORE SILICON ENRICHMENT
  • Enrichment of said wastes up to needed no less than 45% silicon concentration may be carried out with any suitable means. More than 100 pilot experiments with metallothermic magnesium production using above-mentioned raw and experimental vacuum-induction furnace were carried out for evaluation of practicability of the invention. Cylindrical crucible 1 of said experimental furnace was produced from heat- resistant chromium-nickel steel.
  • the inductor 4 was equipped with single-phase winding and designed for peak active power consumption at 50 kWh.
  • Each additional heating element 7 was formed as welded grate (lattice) composed of the ferromagnetic heat-resistant steel rods.
  • said elements 7 are able, during metallothermic process, to prevent the magnetism stratification of the free- flowing mass of the batch mixture residue and the nascent slag under the influence of inductor's 4 magnetic field.
  • conditions of chemical interaction of the non- ferromagnetic magnesium oxide particles and ferromagnetic ferrosilicon particles were ameliorated substantially so as to use the reduction potential of the low-silicon ferrosilicon.
  • Fine- dispersed mixture ingredients were mixed by rotary mixing machine to practically homogeneous mass, then obtained mixture was divided into equal parts (up about 100 kg by weight) for sequential loading into crucible 1. Average duration of the single processing steps were as follows: preliminary calcination of each loaded batch mixture (at temperature of about

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  • General Life Sciences & Earth Sciences (AREA)
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  • Crucibles And Fluidized-Bed Furnaces (AREA)

Abstract

L'invention concerne un processus métallothermique pour produire du magnésium, consistant à chauffer un mélange discontinu de dolomite calcinée et de ferrosilicium, pour le porter à une température d'approximativement 1.200 °C, à une pression résiduelle inférieure à 670 Par et à condenser la vapeur de magnésium. Afin d'augmenter l'extraction de magnésium, un mélange discontinu de dolomite calcinée au moins en partie est finement dispersé, ladite dolomite comprenant des particules ne dépassant pas 0,1 mm et du ferrosilicium à faible teneur en silicium. Le mélange est chargé dans un four à induction sous vide présentant un creuset électroconducteur, muni d'au moins un élément chauffant électroconducteur additionnel, dans la zone de chauffage, et d'un condensateur de refroidissement, à l'extrémité supérieure. Chaque mélange discontinu chargé est calciné en temps utile à une température d'approximativement 900 °C, à pression atmosphérique. Ledit four est ensuite fermé et une fois le vide effectué, ledit four est porté à une température suffisante pour débuter le processus métallothermique, qui se déroule à condition que de la chaleur soit alimentée dans le volume de ladite charge.
PCT/UA2004/000047 2004-04-26 2004-07-06 Processus metallothermique pour la production de magnesium et four a induction sous vide approprie WO2005103309A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
UA20040403072A UA74941C2 (en) 2004-04-26 2004-04-26 A metal-thermal process for producing magnesium and vacuum induction furnace for realizing the same
UA20040403072 2004-04-26

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WO2005103309A1 true WO2005103309A1 (fr) 2005-11-03

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CN107523701A (zh) * 2017-08-22 2017-12-29 西安交通大学 一种常压硅热还原金属镁的方法
CN109930023A (zh) * 2019-03-28 2019-06-25 西安交通大学 一种大吨位铬锆铜合金的制造方法
CN111270088A (zh) * 2020-02-10 2020-06-12 中国恩菲工程技术有限公司 感应加热液态搅拌连续炼镁的系统和方法
CN111707100A (zh) * 2020-06-24 2020-09-25 中南大学 还原罐
EP3797765A1 (fr) 2006-06-27 2021-03-31 Novartis AG Modulateurs du récepteur s1p pour traiter la sclérose en plaques
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