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WO2009113913A1 - Procédé de fabrication de métaux chimiquement actifs - Google Patents

Procédé de fabrication de métaux chimiquement actifs Download PDF

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Publication number
WO2009113913A1
WO2009113913A1 PCT/RU2009/000117 RU2009000117W WO2009113913A1 WO 2009113913 A1 WO2009113913 A1 WO 2009113913A1 RU 2009000117 W RU2009000117 W RU 2009000117W WO 2009113913 A1 WO2009113913 A1 WO 2009113913A1
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WO
WIPO (PCT)
Prior art keywords
nozzle
metal
electrode
arc
gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/RU2009/000117
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English (en)
Russian (ru)
Inventor
Анатолий Евгеньевич ВОЛКОВ
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Individual
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Individual
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Filing date
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Application filed by Individual filed Critical Individual
Publication of WO2009113913A1 publication Critical patent/WO2009113913A1/fr
Anticipated expiration legal-status Critical
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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
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16—Remelting metals
    • C22B9/20—Arc remelting
    • 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
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1295—Refining, melting, remelting, working up of titanium
    • 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
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/16—Remelting metals
    • C22B9/22—Remelting metals with heating by wave energy or particle radiation
    • C22B9/226—Remelting metals with heating by wave energy or particle radiation by electric discharge, e.g. plasma
    • 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
    • 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
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/003—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals by induction
    • 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

  • the present invention relates to the production of chemically active metals from ore raw materials and other compounds and can be used for refining any metals, including chemically active and refractory metals from non-metallic impurities and metals.
  • plasmatrons as heating elements are the stability of the discharge in the gas stream, good power control, the ability to obtain high temperatures, a large concentration of energy.
  • the closest technical solution is a carbothermal reduction method in an arc plasmatron [2], in which cylindrical billets pressed from a charge consisting of Nb 2 O 5 + 5C or Nb 2 O 5 + 5NbC are placed in a water-cooled copper anode crucible.
  • the cathode is graphite.
  • the mixture is heated in argon-hydrogen plasma (5% H 2 in a mixture of Ar).
  • argon-hydrogen plasma 5% H 2 in a mixture of Ar.
  • Liquid phase carbothermal reduction can be carried out by pulling an ingot of ferrous metal from the mold and periodically loading the compressed tablets of the charge.
  • the disadvantages of the analogue is low productivity, since it is necessary to briquet the mixture.
  • the closest technical solution selected as a prototype of a device for implementing the proposed method, is a high-frequency plasma torch described in [2], which contains a discharge chamber in the form of a quartz tube in which a carbon or tungsten rod is placed, which serves as an electrode for igniting a discharge, which is removed after the occurrence of an annular discharge, a gas supply unit, an inductor located in the region of plasma formation.
  • the technical task is to develop a method and device for its implementation, providing increased productivity by reducing the process time, increasing yield, lack of additional cleaning processes, and for the device, in addition, by shielding the nozzle with the melt from the electrode or the melt to be added separately ( charge), due to the use of a remelted electrode as an electrode.
  • This object is achieved by the fact that in the known method for the production of chemically active metals, including the burning of an arc on an electrode, the formation of a plasma jet due to gas and the concentration of the arc in the nozzle and the electromagnetic field that heats the formed metal, drawing an ingot from the mold, according to the invention, protect the nozzle due to the melt of reduced or unreduced metal flowing down it from a consumable electrode or added separately to the nozzle, and its thickness is regulated by the modes and melting, by reversing the current on the electrode, the nozzle, and the metal being formed, while the plasma gas is organized in the arc burning zone above the nozzle by vacuum pumping through the metal ingot formation zone located under the nozzle.
  • a vacuum-stationary plasmatron containing a discharge chamber with an electrode placed in it, a gas supply unit, an inductor, and a mold, according to the invention the electrode is made expendable, the lower part of the upper part of the chamber is made in the form of a funnel-shaped tray forms with a hole in its central part that performs the function of a nozzle, while a solenoid is located on the outside of the chamber in the region of the arc heating zone, in addition, at the bottom of the chamber
  • an inductor can be located under the nozzle, additionally heating the plasma, preventing the molten metal from freezing on the nozzle and concentrating its flow, and the cooled crystallizer can be made sliding, allowing the melt bath mirror to be kept at the same distance from the nozzle exit, that is, without disrupting the technological work plasmatron;
  • a vertically stationary plasmatron can operate on the principle of indirect, direct and variable action, while the electrode is an anode on which oxygen and other gases are released, and a metal ingot is a cathode, where metal is restored electrochemically, plasmochemically and metallothermally.
  • Figure l shows a VSP device that implements the proposed method
  • figure 2 - implementing the proposed method the device VSP, in which carbon is used as an electrode
  • Fig. 3 the main technological zones of metal reduction and crystallization are indicated (enlarged central part of the VSP device shown in Fig. 2);
  • figure 4 is a graph of the melting temperature of the oxide from the temperature of the onset of the reaction.
  • the proposed method is implemented using a device - vertically - a stationary plasma torch - VSP, shown in Fig.l.
  • the device includes a melting chamber 1, in which a consumable electrode 2 is melted due to arc b on a cooled tray 3, which has a funnel-shaped shape and a central hole 24, which serves as a plasma torch nozzle.
  • a melting chamber 1 in which a consumable electrode 2 is melted due to arc b on a cooled tray 3, which has a funnel-shaped shape and a central hole 24, which serves as a plasma torch nozzle.
  • the melt on the pan is mixed due to the solenoid 23, covering the zone of arc heating.
  • the ingot 5 can be drawn simultaneously with the rotation, transmitted also through rod 16.
  • the consumable electrode 2 is moved using the holder 14, which connects the positive pole.
  • the holder 14 is installed in the sliding seals 18.
  • the insulating gaskets 19 separate the upper chamber 1, the pallet 3 and the lower chamber And, to which the pipe 15 is connected, through which it is pumped gas accumulating in the upper chamber, creating a plasma jet.
  • An ingot 5 with a rod 16 is connected to the negative pole or neutral.
  • Arc stabilization is provided by a solenoid 10, as well as an inductor 22, which can additionally heat the plasma and center its direction.
  • Figure l shows a VSP device where a consumable electrode is used as a source of metal to be reduced. It may consist of crude metal contaminated with non-metallic impurities or low boiling metals that pollute the base metal.
  • the electrode can be formed from oxides of the reduced metal and the metal of the reducing agent.
  • the electrode melting under the action of an arc and a metallothermal reaction, will protect the copper cooled nozzle with metal reduction products.
  • the electrode being an anode, on its surface will oxidize oxygen to a gas state, removing it from TiO 2 .
  • the melt formed by titanium and Al 2 O 3 falling into the narrow part of the nozzle, is additionally heated to high temperatures, and, passing through the inductor, can be ionized.
  • titanium, falling into the sliding mold cools and passes into the melt, being further freed from oxygen, due to the fact that the melt and then the formed ingot are the cathode where the electrochemical reduction of the metal proceeds.
  • the compound Al 2 O 3 (CaO, MgO, etc.) under the influence of high temperature can ionize, while oxygen can removed in the form of gas, and aluminum, being a more boiling metal, can evaporate from the metal bath of the ingot.
  • the TiO 2 reduction process if an electrode is formed from it (similar to the Cambridge process) can proceed without the addition of reducing metals due to high temperatures and electrochemical reactions. Draft ingots are also refined from gas and metal impurities according to the above scheme.
  • the circuit of the VSP device depicted in FIG. 2 can also be used for refining metal ingots, which will melt as electrode 2, contaminated with oxygen, for example.
  • metal ingots which will melt as electrode 2, contaminated with oxygen, for example.
  • powdered carbon will be added to the drip tray.
  • the oxygen present in it will combine with carbon to a gas state, thereby the process of metal refining will occur.
  • FIG. 3 The general scheme of the implementation of the method is shown in FIG. 3, where the main technological zones of metal reduction and crystallization are indicated, as well as one of the possible temperature fields that can pass through the substance in these zones, shown in the graph (figure 4). That is, electrode 2, heating due to arc 6 to temperatures from 1000 to 2000 0 C in zone I, starts to oxidize oxygen on its surface to gas compounds, this also applies to chlorine, fluorine, etc. connections. Due to the melting of the solid phase of the substance, a protective layer from the reaction mixture is formed in zone II on the upper part of the nozzle, in which the metal reduction process continues.
  • the ongoing heating of the substance in zone II leads to the fact that when the temperature of the charge heating exceeds the melting temperature of the reduced oxide by a certain amount, a spontaneous metallothermal reduction reaction begins. Due to the reaction in this zone, the metal begins to recover, while additional heat is released. If the reduced and unreduced metal enters the IH zone, i.e., when it leaves the plasmatron nozzle and enters the section of the inductor heating the plasma, the metal will additionally heat up and its temperature will increase even further, while its increase can reach 3500 ⁇ 7000 ° C. That is, plasmochemical processes begin to occur in this zone, where the substance will be almost completely ionized, which will significantly accelerate the course of metal reduction reactions.
  • oxygen begins to be removed in the form of gas, due to the vacuum pumping system.
  • the plasma upon exiting the inductor, heats the molten metal mirror with its torch, where the reduced metal enters, forming a molten bath 8.
  • the temperature begins to drop and all processes begin to slow down.
  • a metal bath forms and crystallizes due to cooling by a crystallizer, while the reduction product in the form of a metal exits the reaction, shifting it to the right.
  • the metal reduction process consists of the following chain: arc heating of the electrode, which is the anode during which the melting of the mixture and the oxidation reaction with gas evolution occur, the metal thermal reduction of the metal inside the plasmatron, the metal thermal, plasma chemical and electrochemical metal reduction in the plasma combustion zone, the formation of the metal bath and its cooling on the mold.
  • the proposed device can carry out the process of metal recovery from oxide, fluoride, carbide, chloride compounds, as well as purify a metal ingot from oxygen, nitrogen, hydrogen, carbon, chlorine, fluorine and other impurity metals.
  • the process of metal reduction and purification is based on a complex of processes, the main of which are the plasma-chemical and electrochemical processes, in addition, metallothermal reduction of the base metal can take part in the process.
  • the entire installation serves as a plasma torch, where the consumable electrode simultaneously serves as the anode and source of melt production, on which an arc is formed for its subsequent compression.
  • a skull is formed of the metal or its compounds on the cooled tray, the layer of which protects the copper tray from heat load, which will increase as the arc contracts and moves to the hole in the tray.
  • the melt on the pallet rises partially due to its rotation under the action of the electromagnetic field of the solenoid. As it accumulates, due to the angle of inclination of the pallet, the melt flows to the central hole. Further, the melt, passing through the central hole, which is a plasma torch nozzle, receives significant thermal energy, being heated by a plasma stream formed from a compressed arc discharge formed on the anode.
  • the thickness of the skull layer formed on the pallet depends on the thermal power of the arc, while the skull layer can reach different sizes.
  • the skull has the smallest thickness.
  • the negative pole switches to the rod, which pulls the ingot from the sliding mold, thereby the electrode-pallet-ingot system will be a direct-acting plasmatron [3], (p.407).
  • the arc will be focused from a large area of the consumable electrode acting as an anode and compressed in the hole of the tray serving as a nozzle, while its heat power will be mainly directed to the upper part of the formed ingot acting as a cathode, and therefore the skull , which is distributed around the periphery of the pallet, will increase, protecting the pallet from thermal overheating.
  • Titanium freed from oxygen, flowing down the pallet and falling into the bath of the sliding mold-cathode, will be additionally freed from the oxygen present in it, both due to additional heating by a plasma jet, which will accelerate the plasma-chemical process, and due to electrochemical reactions that take place on the cathode allow the metal to be released from oxygen.
  • Direct reduction of titanium from oxides, as well as other chemical active metals, can be accelerated by the introduction of reducing agents, such as calcium, sodium, magnesium, aluminum, carbon, etc., into the electrode.
  • reducing agents such as calcium, sodium, magnesium, aluminum, carbon, etc.
  • metallothermal reduction reactions will begin to take place, which will be accelerated when the reaction charge gets on the pallet as moving it to the nozzle hole.
  • the reduced metal entering the ingot bath i.e. to the cathode, additionally heated by a jet of plasma, it will begin to get rid of reducing metal metals (which usually refer to low-boiling metals) or carbon, which will be present in it, i.e. these impurities will evaporate.
  • Carbon capturing the remaining oxygen from the metal, in the form of CO or CO 2 , will be removed from the reaction by a vacuum system.
  • Plasma jet heating the ingot bath with its torch, will also evaporate slag formations, which will close this bath, as during metallothermal processes oxidation reactions of reducing metals will occur.
  • VSP vertically stationary plasmatron
  • Chlorine and oxygen are removed from the furnace by a vacuum pumping system and captured by a gas collection system for reuse.
  • a vacuum pumping system In the case of remelting of the contaminated sponge on vacuum-arc furnaces, there is always a real threat of lateral breakdown to the mold, which can lead to the explosion of the furnace. Therefore, the dirty sponge on these furnaces is not remelted and is used mainly for ferrotitanium.
  • Electron beam furnaces also do not melt this mixture, since increased gas generation destroys electron beam guns.
  • Conventional plasmatrons in view of their operation under increased gas pressure, do not allow the metal to be well cleared of gas impurities. Therefore, the cleaning of heavily contaminated metals on a VSP furnace can be one of the most effective today.
  • An additional technological lever affecting the heating parameters is the possibility of supplying additional inert gas to the upper melting chamber through line 12 and valve 13.
  • the supply of additional inert gas will contribute to the increase in the skull on the pallet due to gas cooling, but in the same time the amplification of the plasma jet flow will be to increase the heating of the mirror of the liquid bath 8 in the ingot.
  • the supply of additional inert gas will contribute to the increase of the skull on the periphery of the pallet, but at the same time its fusion closer to the center.
  • the plasma-forming gas generated due to the arc at its end face of a large area becomes quite sufficient for the successful operation of the plasma torch without any additional pumping of gas.
  • the consumable electrode serves both as a source of melt and a source of plasma-forming gas, which enhances its thermal energy due to the narrowing hole in the pan, and the smaller the hole, the higher the temperature of the generated plasma stream and the smaller the diameter you can get an ingot, without fearing that a small hole the nozzle will overgrow with a skull.
  • the presented VSP device allows very compact arrangement of equipment in the workshop room. So, for example, when a titanium electrode is re-melted with a diameter of 1.2 m and a length of 1.5 m, the upper part of the installation above the zero mark will be no more than 3 m, when the ingot is melted with a diameter of 0.5 m, the shaft depth will be 9 m.
  • a high-frequency inductor 22 can be used, which will additionally heat the plasma jet and squeeze it to the center of the vertical axis, thereby facilitating and stabilizing the process of melting and metal reduction.
  • the proposed method has wider possibilities for averaging the chemical composition and allows to obtain ingots of smaller diameter than the original electrode, thereby sharply reducing production costs, increasing yield and reducing time for metal redistribution.
  • the claimed method is more productive, since the efficiency of the heater using the consumable electrode is higher, while the design of the device is much simpler than furnaces with plasma heaters.
  • the process of titanium reduction in the VSP device proceeds at very high speeds, since the substance is restored much faster due to ionization at high temperature. It is also necessary to take into account that in this case an electrolyte consisting of a certain substance in liquid form is not used, and, therefore, there is no limitation on the heating temperature of the reduced metal.
  • the thermal density of the arc can be greater by orders of magnitude, and, consequently, the rates of metal reduction and refining reactions also increase by orders of magnitude.
  • this method and device may be useful for widespread adoption in industry.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Plasma & Fusion (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • General Engineering & Computer Science (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Plasma Technology (AREA)

Abstract

L’invention concerne la fabrication de métaux et peut s’utiliser pour le raffinage de métaux chimiquement actifs et réfractaires visant à éliminer les impuretés non métalliques. Le procédé comprend la création d’un arc électrique sur une électrode, la formation d’un jet de plasma réchauffant le métal à former grâce au gaz et à la concentration de l’arc dans une buse au moyen d’un champ électromagnétique. La protection de la buse est effectuée par la masse fondue de métal partiellement ou entièrement réduit qui s’écoule de l’électrode consommée ou qui est versé sur l’électrode sous la forme d’une poudre. L’épaisseur de la masse fondue est régulée via les modes de fusion, par le changement de polarité sur l’électrode, la buse et le métal formé. Le gaz destiné au plasma est formé dans la zone de l’arc électrique au-dessus de la buse grâce à l’évacuation du vide par pompage via la zone de formation d’un lingot de métal qui est située sous la buse. Un générateur de plasma stationnaire vertical comprend une chambre à décharges dans laquelle est disposée l’électrode consommable (l’anode) ainsi qu’une unité d’amenée de gaz, un inducteur et un cristalliseur. La partie inférieure de la zone supérieure de la chambre se présente comme un bac en forme d’entonnoir possédant un orifice dans sa partie centrale qui fonctionne comme une buse. Du côté extérieur de la chambre on a disposé un solénoïde, et dans la partie inférieure de la chambre on a monté sur le périmètre de l’arc un inducteur et un cristalliseur à l’intérieur duquel on a placé un lingot de métal qui a une fonction de cathode. L’invention permet d’augmenter la productivité.
PCT/RU2009/000117 2008-03-14 2009-03-10 Procédé de fabrication de métaux chimiquement actifs Ceased WO2009113913A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2008109797 2008-03-14
RU2008109797/28A RU2401477C2 (ru) 2008-03-14 2008-03-14 Способ волкова для производства химически активных металлов и использование вертикально-стационарного плазматрона - "всп"

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WO2009113913A1 true WO2009113913A1 (fr) 2009-09-17

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU553842A1 (ru) * 1975-12-15 1986-10-30 Предприятие П/Я Г-4911 Вакуумна плазменно-электрошлакова печь
US4681627A (en) * 1985-06-03 1987-07-21 Mitsubishi Kinzoku Kabushiki Kaisha Process for preparing an ingot from metal scrap
RU1770420C (ru) * 1990-07-31 1992-10-23 Запорожский машиностроительный институт им.В.Я.Чубаря Способ очистки тугоплавких металлов и сплавов от примесей цветных металлов
RU2209841C2 (ru) * 1998-03-30 2003-08-10 Волков Анатолий Евгеньевич Способ литья металла
RU2209842C2 (ru) * 1999-12-20 2003-08-10 Волков Анатолий Евгеньевич Способ плавки и литья металла
RU2295574C2 (ru) * 2004-02-23 2007-03-20 Анатолий Тимофеевич Неклеса Способ получения металла и установка для его осуществления

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2198772C1 (ru) * 2001-05-28 2003-02-20 Пермский государственный технический университет Плазмотрон
RU20871U1 (ru) * 2001-08-22 2001-12-10 Пыкин Юрий Анатольевич Плазмотрон
WO2004010747A1 (fr) * 2002-07-19 2004-01-29 International Association Interm Plasmatron pour la pulverisation de revetements

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU553842A1 (ru) * 1975-12-15 1986-10-30 Предприятие П/Я Г-4911 Вакуумна плазменно-электрошлакова печь
US4681627A (en) * 1985-06-03 1987-07-21 Mitsubishi Kinzoku Kabushiki Kaisha Process for preparing an ingot from metal scrap
RU1770420C (ru) * 1990-07-31 1992-10-23 Запорожский машиностроительный институт им.В.Я.Чубаря Способ очистки тугоплавких металлов и сплавов от примесей цветных металлов
RU2209841C2 (ru) * 1998-03-30 2003-08-10 Волков Анатолий Евгеньевич Способ литья металла
RU2209842C2 (ru) * 1999-12-20 2003-08-10 Волков Анатолий Евгеньевич Способ плавки и литья металла
RU2295574C2 (ru) * 2004-02-23 2007-03-20 Анатолий Тимофеевич Неклеса Способ получения металла и установка для его осуществления

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RU2008109797A (ru) 2009-09-20
RU2401477C2 (ru) 2010-10-10

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