• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A process for preparing alloyed or non-alloyed, reactive metals by reaction of halides thereof, in particular chlorides, with a reducing agent at a temperature higher than the melting temperature of the metal to be developed, comprises solidifying the developed metal while maintaining in the reaction zone wherein the reduction proceeds, a layer of this metal in the liquid state, at a temperature higher than the boiling or sublimation temperature of the other reaction products at the pressure at which the reduction develops, these other reaction products being substantially continuously discharged in the gaseous state.
    公开号:SU1331435A3
    申请号:SU802946203
    申请日:1980-07-04
    公开日:1987-08-15
    发明作者:Винан Рене
    申请人:Кокерий С.А. Бельгия；
    IPC主号:
    专利说明:

     one
    The invention relates to a method for the continuous production of rare refractory metals selected from the group: titanium, zirconium, tantalum, niobium, as a result of the reaction of their halides, in particular chlorides, with a reducing agent at a temperature higher than the melting point of the metal produced.
     The aim of the invention is to reduce energy costs.
    FIG. 1 and 2 are schematic diagrams of a device for carrying out the proposed method; in fig. 3 - mold, cut; in fig. 4 is a section A-A in FIG. 3
    The device (Fig. 1) includes a closed chamber 1 located above ingot mold 2 and ingot, which is cooled, for example, by a flow of water (not shown), a device 3 for introducing reagents involved in the reaction in the upper part 2 of mold 2, pipe 4 for continuous removal of by-products in the form of gases resulting from reduction.
    A device 3 for introducing reagents into the upper part 2 of the ingot mold 2 for an ingot includes a first tank 5 located inside the heater 6 and connected by means of a metering pump 7 to a second tank 8 located inside another heater 9. The second tank 8 is connected by means of an injection pipe 10 to the upper part 2.
    A container 11 equipped with a heater 12 for storing the recovered metal is connected by means of a metering pump 13 with a container 14 with a heater 9. The container 14 is in turn connected to a closed chamber 1 by means of an injection pipe 13.
    The proposed device (Fig. 1) is most suitable for reducing metal halides in a liquid state at a pressure close to atmospheric, in a fairly wide range of temperatures.
    In this case, the halide is maintained in a liquid state in the tank 5, heated, if necessary, by the heater 6, and pumped through the pump 7 to eiMKocTb 8, heated by the heater 9, in which it is brought to a boil. Gaseous ha
    0
    five
    0
    five
    0
    five
    0
    five
    35
    The metal logide chatem enters the upper part of the mold through the injection pipe 10.
    The reducing metal contained in the vessel 11 is maintained at a temperature which exceeds its melting point by about 50 ° C, as a result of heating by means of a nag - valve.
    The molten metal is transferred by means of a pump 13 into a container 14, where the metal is maintained in a boiling state.
    The metal-reducing agent in the liquid state is then transferred in a controlled manner to the reaction zone of the closed chamber 1 by means of the injection pipe 15.
    The flow rate of the gaseous reducing metal is controlled in accordance with the flow rate of the liquid metal using a metering pump 7 or controlling the energy supply in the evaporation step by a regulator (not shown).
    In the reaction zone located in part 2 of ingot mold 2, the temperature is maintained above the melting point to obtain 1: Migo metal, as well as higher than the boiling point or sublimation temperature of all other substances participating in the reaction.
    The resulting metal is collected into ingot mold 2, which consists of double-walled copper luuniHupa, between which coolant circulates.
    The upper metal layer 16 is in the reaction zone in the molten state, while the metal layer 17 around and below the liquid layer solidifies as a result of cooling and forms a slat that is continuously moved down (in the direction indicated by the arrow 18) using known devices , for example rotating-. videos (not shown).
    All substances other than metal (by-products of the reaction) are removed from the reaction zone through pipe 4. It is also possible to transfer these gases to a refrigerator (not shown) in order to extract unused reagents.
    Due to Tui o. camera 1 of the chakras ga i ermetm -Sh and possibly cos313
    giving an atmosphere of an inert gas, such as argon or gels, in it by means of a device 19 containing a similar gas and connected to Cameron 1 by a pipe 20.
    FIG. 2, in the device 3 for introducing a halide into the upper part 2, only one tank 5 is provided. Such a device is particularly suitable when the halides are not liquids, for example, zirconium halide. Such halides are converted to gaseous state by sublimation by heating them with a heater 6.
    The flow rate of gaseous halides to the reaction zone is regulated by the supply of energy to the specified heater.
    If non-refractory metals are produced, it is convenient to carry out the reduction reaction under such conditions that the heat required to maintain the reaction zone at a temperature above the melting point of the metal produced, as well as the boiling point or sublimation temperature of all other substances participating in the reaction, would only result as a result of the exothermic reaction between the halide of the metal to be produced and the metal restorer, such as an alkali metal or alkaline earth metal.
    More refractory metals can be obtained by simultaneously reducing the corresponding halide with a reducing metal and hydrogen.
    Refractory metals, such as vanadium, niobium, molybdenum, tungsten and hafnium, are obtained by reducing their halides with hydrogen.
    An additional arc, plasma arc or inductive plasma torch, as well as a parabolic mirror heater or laser can be used to generate additional heat (in the case when the heat produced by the reduction reaction is not enough).
    The proposed method is carried out as follows.
    The reactants are introduced in the gaseous state into the reaction zone located in the upper part 2 of the ingot mold 2 for the ingot in the form of a circular funnel. This achieves
    435
    merging small droplets of metal formed in this stream into larger droplets. The latter are ejected from the flow by centrifugal forces, assembled on the side walls of the mold for the ingot, flow down through them under the force of gravity and fall into the metal layer 16, the pickling ingot 17.
    0 The proposed method provides faster, uninterrupted and deep separation of the formed metal from the reactants and gaseous reaction products.
    5 Entering gaseous reagents into the specified zone at an angle to the vertical ensures the formation, for example, of a circular or ordinary flow. Each of the two reagents is injected
    0 in the upper part 2 of the ingot mold 2 for the ingot at the same time on several levels, thus achieving a high flow rate of the reactants, shortening the mixing time and contacting 5 different reactants, and the contacting is the most complete.
    To create a circular or spiral flow, each of the injection pipes 10 and 15 is introduced into the reaction zone in the view .; nozzles (e.g., double), equipped with injection outlets 10, 10, 15, 13, which are located in planes tangential to cylinders aligned coaxially with ingot mold 2, the horizontal components of which are oriented in a circumferential direction.
    0 These injection outlets are located somewhat below the lid 21, which seals the upper part 2 of the ingot mold. The lid 21 is equipped with a pipe 4, which is intended to release the reaction by-products.
    Example 1. Preparation of titanium by reduction of titanium chloride with sodium.
    Q The metal reducing agent (in this case, sodium) is in the container 11 at a temperature of about, namely, at a temperature exceeding by about 50 ° C the temperature of the melt, which is achieved as a result
    using a heater 12, which preferably is a resistor-type electric heater.
    five
    51
    The temperature inside the entire volume of the upper part 2 is maintained at a level exceeding the boiling point of the reagents, specifically 1100 C.
    Sodium and titanium chloride are introduced in the desired ratio into the specified upper part 2 of the ingot mold; their feed rate is controlled by metering pumps 7 and 13.
    Since titanium chloride is a liquid at room temperature, there is no need to heat tank 5, so heater 6 may not be used.
    Before entering the reagents, chamber 1 is initially degassed several times as a result of successive vacuuming and purging with argon through line 20 at atmospheric pressure or at a pressure slightly higher than atmospheric.
    The total flow rate of the reagents is controlled so that in the reaction zone in the upper part 2 of the ingot mold 2, the ingot temperature is higher than the melting point of the metal (1688 ° C), i.e. temperature of about 1750 C.
    The flow rate at the supply of titanium chloride is 2.6, and the feed rate of sodium is 2.7 t / h. Such a ratio of reagents provides a 25% excess of sodium, which improves the reaction.
    The amount of heat released by the reaction is sufficient to maintain the temperature in the reaction zone at 1750 ° C.
    The cooling of the ingot mold 2 for the ingot is regulated so that in the upper part of the ingot mold the liquid metal layer is kept at all times. The temperature of the liquid metal layer is maintained at a level that exceeds the melting point of the metal by 15-.
    Thus, it is possible to obtain titanium with a yield of 1 t / h in the form of a homogeneous bulk ingot, which can be directly subjected to forging and rolling.
    In the reduction process, gaseous substances in the form of smoke containing sodium chloride and, by-products of titanium processing, as well as an excess of sodium, are continuously removed from the reaction zone. These gases enter the refrigerator, where complete metal recovery is completed at low
    356
    temperature with the formation of dendrites which are then again replaced in the liquid metal layer above the ingot.
    Mold for ingot have a diameter of 80 - 160 mm, 1 to 200 - 400 mm
    Ingots with a diameter of 150 mm are output at a speed of 210 mm / min, and ingots with a diameter of 100 mm are output at a speed of 470 mm / min (in both cases at the above flow rates).
    II p m m e p 2. Production of titanium as a result of the simultaneous reduction of titanium chloride by sodium and hydrogen.
    A device (Figs. 1, 3 and 4) is used to generate an additional amount of heat using a hydrogen plasma torch (not shown).
    4.4 kg / h of gaseous titanium chloride 2.7 kg / h of gaseous sodium and 1.2 m / h of hydrogen are introduced into the reaction zone, in which the temperature is maintained at 2450 - 3570 K, preferably 3000 K. The excess hydrogen is recycled.
    The temperature conditions for the feed reagents and for the reaction zone, as well as the injection method, are identical to those described in step 1.
    The amount of titanium produced is 1 kg / h.
    Additional heating can also be carried out using an electric arc, a mirror heater, a laser, or another device, but the use of a hydrogen plasma torch is most effective.
    Plasma-forming gas is a reducing agent for reducing titanium chloride in this way, it becomes possible to simultaneously reduce titanium chloride with sodium and hydrogen.
    Sodium reduction is an exothermic process, and hydrogen reduction is endothermic, therefore, while carrying out both reactions, the following effect is observed: in the case when the temperature of the reaction varies, one of the two reactions takes precedence, and the overall metallurgical cost will be higher than the output of each of the separately occurring reactions.
    Example 3. Production of zirconium by reduction of zirconium tetrachloride with sodium.
    Since the zirconium tetraphorum is not a liquid, the device shown in FIG. 2
    Zirconium tetrachloride sublumine freezes at atmospheric pressure and
    gws.
    Sodium is brought to a boil in tank 14, heated by heater 9, before being introduced through an injection tube 15, upper part 2 of ingot mold 2 and ingot, and four zirconium chloride is submerged in tank 5, heated by heater 6.
    The flow rate of the gaseous halogen is dictated by the energy imparted by the heater 6.
    9 kg / h of zirconium are obtained by reducing 23 kg / h of zirconium tetrachloride to 5 kg / h of sodium.
    The reagent ratio used corresponds to a 25% excess of sodium.
    The remaining conditions are identical to those described in the previous examples, except that the flow rate of the reactants is maintained at a level sufficient to ensure that the temperature in the reaction zone is higher than the melting point of zirconium (), i.e. about 1900 ° C
    Example 4. Production of tantalum by reducing tantalum chloride with hydrogen.
    Since tantalum is a very refractory metal, obtaining it in a liquid state requires the use of temperatures higher.
    In general, the metallothermic reduction does not provide enough heat to reach this temperature; In addition, the exothermic reaction has a very low metallurgical yield at very high temperatures, therefore, in this case, the hydrogen plasma torch is used to obtain heat.
    It has been established that the high temperatures required by the melting of the metal are easily achievable and contribute to the reduction of the metal with hydrogen, since the reduction reaction is endothermic.
    Tantalum is a liquid at a temperature of 3000 to 5000 ° C, and the temperature in the reaction zone maintains
    c at about 4000 ° C. In addition, since tantalum chloride melts at a temperature of about 220 ° C, it is of principle possible to vary the flow rate by means of a metering pump.
    Since the temperature range in which perchloride tantalum is a liquid is limited (about 220 ° C), it is preferable to adjust the gas flow rate of this chloride by changing the energy reported by heater 6, similarly to that described in example 3.
    As a result of the reaction, 1 kg / h of tantalum is obtained when reducing
    2.1kg / h p-tantalum chloride
    1.2 m / h of hydrogen, which corresponds to a significant excess of the reducing agent (molar ratio N gTaSTs is 10).
    Excess hydrogen is recycled to further carry out the reduction process.
    The metal hardens in a cooled copper ingot mold for an ingot in the same way as in the previous examples.
    In carrying out the proposed process, the reactants are introduced in the gaseous state directly into the upper part of the ingot mold, and not into a separate reaction chamber.
    The proposed method allows to obtain reactive metals in a pure state or in the form of alloys with other reactive or non-reactive elements, for example, in the form of a titanium alloy with vanadium and aluminum, while saving energy by performing a process with a minimum supply or without the supply of external heat and by reducing the reaction zone.
    权利要求:
    Claims (6)
    [1]
    1. A method for producing a rare refractory metal selected from the groups Qpu: titanium, zirconium, tantalum, niobium, including the reduction of their halides at a temperature above the melting point of the metal, with the supply of gaseous halide of the metal to be obtained and the reducing agent in the form of inclined vortex flows to produce metal in the form of liquid droplets forming a molten layer on top of the ingot of the resulting
    9gzz
    metal in 1e in the reaction zone near the pacn.naBju HHoro layer above the boiling point or sublimation of unreacted reaction products, and their removal, characterized in that, in order to reduce energy costs, HcxoAHi.ie reagents are restored) 1 in a circular or spiral flow over the molten layer of the obtained metal to form a reaction zone in the upper part of the mold.
    [2]
    2. The method according to p.
    This is due to the fact that, before reduction, at least one of the initial reagents is melted in the first stage, followed by heating it in the second stage to the boiling point and continuous transportation.
    [3]
    3. Method according to paragraphs. 1 and 2, that is, one of the starting reagents is sublimated at atmospheric pressure before being reduced, and its sublimation is controlled and its reaction zone is controlled by controlling the temperature,
    [4]
    4. Spssob on PP. 1-3, the casting is used sodium.
    [5]
    5.Ciu: co6 110 pp. 1 to 3, about tl and the fact that hydrogen is used as a reducing agent.
    [6]
    6. SposooO on PP. 1-3, characterized in that in quality
    O
    50
    five
    0
    five
    5 5I O
    I1; gstlnont Olya isp (endless mixture of sodium and hydrogen.
    U.Superity to obtain a rare, spongy metal sputtering metal: titanium, lyipicoHurt, tantalum, niobium, reduction of their halides, including sealed camlo with a cooled cylindrical mold located in it, separate chambers; 1) evaporation of source reagents, supply pipes argon and removal of reaction by-products, ingestion of pipes for supplying initial HPTFj reagents and means of hypanate cjuiTKH of obtained metal from outlines1, characterized in that, in order to reduce energy consumption, it has a lid To seal the mold, and the lower parts of the injection tubes are placed in the lid directly at the side of the mold in the directions, Hhix is located in the planes tangent to the ijj-linderx mold, and the pressure directions have horizontal fittings, and the pipe for ny ;, and by-products are placed on the top of the chamber.
    8, The device according to claim 7, about tl and - h: i n. Shche e with IKM, that it is supplied with the iiii (mksst; viH transfer the original rt.ich itonon liquid state, connected by metering pumps with chambers l: 1 and made with nlgrsnaty.
    /
    srig2
    J5 L
    ten
    fig.Z
    fO
    21
    Editor L. Veselovska
    Order 3595/58 Draw 604
    VNIIPI USSR State Committee
    for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., d. A / 5
    Production and printing company, Uzhgorod, st. Project, 4
    figl
    Compiled by G. Melnikova
    Tehred M. Khodanich Proofreader E. Roshko
    Subscription
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    同族专利:
    公开号 | 公开日
    DE3024697C2|1990-01-18|
    LU81469A1|1981-02-03|
    DE3024697A1|1981-01-29|
    GB2057016B|1984-01-18|
    AT374502B|1984-05-10|
    NO156495B|1987-06-22|
    IT1131902B|1986-06-25|
    BR8004185A|1981-01-21|
    NL8003899A|1981-01-07|
    NO801998L|1981-01-06|
    BE884188A|1980-11-03|
    SE8004897L|1981-01-06|
    CH648062A5|1985-02-28|
    JPS5635733A|1981-04-08|
    GB2057016A|1981-03-25|
    ATA347680A|1983-09-15|
    US4830665A|1989-05-16|
    FR2461014B1|1986-03-21|
    IT8023224D0|1980-07-03|
    NO156495C|1987-09-30|
    CA1153210A|1983-09-06|
    JPS6121290B2|1986-05-26|
    FR2461014A1|1981-01-30|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    LU81469A|LU81469A1|1979-07-05|1979-07-05|PROCESS AND PLANT FOR THE PRODUCTION OF REACTIVE METALS BY REDUCTION OF THEIR HALIDES|
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