EP0134780A2 - Procédé et installation pour l'élaboration de métaux ou d'alliages - Google Patents

Procédé et installation pour l'élaboration de métaux ou d'alliages Download PDF

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Publication number
EP0134780A2
EP0134780A2 EP84890155A EP84890155A EP0134780A2 EP 0134780 A2 EP0134780 A2 EP 0134780A2 EP 84890155 A EP84890155 A EP 84890155A EP 84890155 A EP84890155 A EP 84890155A EP 0134780 A2 EP0134780 A2 EP 0134780A2
Authority
EP
European Patent Office
Prior art keywords
metal
plasma
reaction
hydrogen
reaction vessel
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.)
Withdrawn
Application number
EP84890155A
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German (de)
English (en)
Other versions
EP0134780A3 (fr
Inventor
Paul Muellner
Bernhard Enkner
Gerhard Hubweber
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Voestalpine AG
Original Assignee
Voestalpine AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Voestalpine AG filed Critical Voestalpine AG
Publication of EP0134780A2 publication Critical patent/EP0134780A2/fr
Publication of EP0134780A3 publication Critical patent/EP0134780A3/fr
Withdrawn legal-status Critical Current

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    • 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
    • C22B5/12—Dry methods smelting of sulfides or formation of mattes by gases
    • 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
    • C22B34/1263—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 obtaining metallic titanium from titanium compounds, e.g. by reduction
    • C22B34/1286—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 obtaining metallic titanium from titanium compounds, e.g. by reduction using hydrogen containing agents, e.g. H2, CaH2, hydrocarbons
    • 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
    • C22B4/005—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys using plasma jets

Definitions

  • the invention relates to a process for the production of metals or metal alloys by reducing their halides and to an apparatus for carrying out the process.
  • the extraction of metals from their halides is primarily known for titanium, zirconium, hafnium, niobium and tantalum, but can also be used for other metals, such as for chrome and uranium.
  • the so-called Kroll process according to US Pat. No. 2,205,854 is known for the production of titanium, titanium tetrachloride and a reducing metal, namely magnesium or sodium, being used as starting materials, and the titanium tetrachloride in gaseous or liquid form in one with a liquid reduction metal filled reaction crucible is introduced. The temperature is kept at about 1100 ° K. Disadvantages of this process are that the reducing metal is expensive, the recovery of the metal from the metal halide is complex and the titanium is obtained in sponge form, which requires several post-treatment steps.
  • the invention aims at avoiding the difficulties described and has as its object to be able to produce metals or metal alloys in liquid form by reducing their halides using hydrogen as reducing agent, but without using reducing metals such as sodium or magnesium, the molten metal can be shed immediately afterwards.
  • a plasma jet reaction zone is formed from metal halides contained in vapor form in the plasma gas, from which the resulting molten metal passes into a mold arranged below the reaction zone and is optionally continuously extracted therefrom.
  • reaction zone As a plasma jet reaction zone, a very high temperature is achieved compared to the known method, namely up to 10,000 ° K, a thermodynamic effect advantageously being used becomes:
  • the reducing power of hydrogen for metal halides increases with increasing temperature, so that the halides can be reduced without the aid of additional reducing metals.
  • Hydrogen alone but preferably a mixture of hydrogen and noble gas, in particular argon, can be used as the plasma gas, the temperature of the plasma jet (the plasma column) being able to be regulated by the mixing ratio.
  • the temperature can be increased by adding argon.
  • the metal halide can be introduced into the plasma jet in a solid, liquid or preferably gaseous state.
  • additional hydrogen streams surrounding the plasma jet reaction zone are introduced in order to remove the HCl and unreacted metal halides formed from the reaction space.
  • the exhaust gas generated in the reaction contains unreacted metal halides and HCl.
  • the unreacted metal halides can be separated by cooling and returned to the plasma jet reaction zone in the circuit.
  • the metal halides to be reacted are converted into vapor form before introduction into the plasma jet reaction zone; they are preferably pre-reduced.
  • titanium tetrachloride can be pre-reduced to titanium dichloride in an upstream reaction chamber.
  • the invention further comprises a device for performing the described method with a cooled reaction vessel, in the upper part of which a reaction chamber is formed, into which the metal halide and hydrogen to be reduced are introduced and means for heating the reaction chamber are provided, and in the latter lower part of the metal formed is collected.
  • the device according to the invention is characterized in that a plasma lance is arranged centrally in the reaction vessel, through which a mixture of hydrogen-containing plasma gas and the vaporous metal halide to be reduced is passed, a plasma jet serving as the counter electrode between the mouth of the plasma lance and the metal sump located in the reaction vessel is formed in which the reaction between hydrogen and metal halide takes place.
  • the reaction vessel consists of an upper part of the reactor containing the plasma lance and a lower part of the mold which accommodates the metal sump and is telescopically displaceable relative thereto.
  • the plasma lance is concentrically surrounded by hydrogen supply tubes; that the upper part and the lower part of the reaction vessel are double-walled and have coolant flowing through them; that the displaceable parts of the reaction vessel are sealed against one another by a sealing gas, such as argon; and that the lower part of the reaction vessel is designed as an oscillating continuous mold.
  • FIG. 1 showing a diagram of the process according to the invention
  • FIGS. 2 and 3 showing vertical sections, partially side views, of a reactor with attached mold part in two working positions
  • Figure 4 illustrates a modified embodiment of an oscillating continuous mold reactor.
  • the reaction vessel is generally designated 1. It consists of an upper reactor part 2 and a lower mold part 3. Central in the reactor part 2 is one Plasma lance 4 arranged, which is fed via the line 5 gaseous titanium tetrachloride.
  • the gaseous titanium tetrachloride is formed in a gasification chamber 6, which chamber is supplied by a metering pump 7.
  • the gasification or evaporation of liquid titanium tetrachloride takes place by injection into the chamber 6 via a nozzle 8 and simultaneous heating from the outside.
  • the plasma lance which consists of a mixture of hydrogen and argon, is fed to the plasma lance via lines 9 and 10.
  • the plasma column or plasma jet 11 forms at the mouth of the plasma lance, which reaches a high temperature of up to 10,000 ° K and in which the reduction takes place.
  • the molten metal is collected in the mold part 3.
  • the plasma jet burns between the formed metal sump 12, which forms the anode, and the lance mouth.
  • the mold part 3 is telescopically displaceable relative to the reactor part 2.
  • the gap is sealed by a gas curtain 13, preferably made of argon.
  • Further supply lines for hydrogen gas, which are designated by 14, are arranged around the plasma lance.
  • the process scheme shown in Fig. 1 can be according to a modified embodiment can be supplemented by introducing hydrogen into the gasification chamber 6 through a line (not shown), the titanium tetrachloride being reduced beforehand to titanium dichloride.
  • a cooling chamber can also be provided in line 5 between the gasification chamber and the plasma lance, from which the HC1 formed during the pre-reduction is derived.
  • the structural design of the reaction vessel according to the invention is explained in more detail. It can be seen from this that the plasma lance 4 is cooled by having a cooling jacket 20 in which a guide tube 21 is provided for diverting the coolant. Furthermore, the formation of the supply pipes 14 surrounding the plasma lance for additional hydrogen can be seen from FIG. 2. These are also provided with a cooling jacket 22. Furthermore, the mold part 3 of the reaction vessel is also equipped with a cooling system which consists of a double jacket 23, 24 and a ring of tubes 25 arranged in the jacket space. The coolant is supplied to the cooling jacket through line 26, discharged through the ring-shaped tubes 25 and discharged through line 27.
  • the mold part 3 is telescopically displaceable relative to the reactor part 2, that is to say it can be pulled in and pulled out, FIG. 2 showing the inserted position at the beginning or shortly after the start of the reduction process and FIG. 3 the position after filling the mold part with liquid metal 28 Illustrated end of process.
  • the electrical connection of the mold part of the reaction vessel which forms the anode takes place via line 29 to the positive pole of a current source.
  • the plasma lance itself is the cathode on the negative pole Power source connected.
  • the mold part 3 is shifted relative to the reactor part 2 by means of an actuator 30 engaging the mold part.
  • the gap between the reactor part 2 and the mold part 3 is sealed by a sleeve 31 into which argon is introduced through line 32.
  • the reactor part is formed by a continuous mold 34 which oscillates in the direction of the double arrow 33 and which has a cooling jacket 35, into which the cooling water enters at 36 and exits at 37.
  • the plasma lance 4 and the pipes 14 arranged around it for the supply of additional hydrogen are configured in the same way as described in connection with FIG. 2.
  • the continuous mold 34 is connected to a fixed support part 38 connected to the casting platform 39 by means of a bellows 40.
  • argon is blown through the line 41 into the gap between the support part 38 and the strand 42 formed in the reduction zone 11 (plasma wire) in a similar manner as described earlier.
  • the strand 43 is continuously drawn out by the rollers 43.
  • the entire device is first flushed with noble gases, in particular argon. Afterwards the plasma lance is ignited and the noble gas is largely replaced by hydrogen and then the metal halide is switched on.
  • a plate made of the metal to be melted is expediently placed on the bottom of the mold part, on which the molten metal attaches and continues to grow as the reduction process progresses.
  • a starting strand made of the metal to be melted is inserted into the mold from below, which is pulled down as the process progresses.
  • the continuous mold is sealed off from the fixed plasma lance by a further bellows 44 made of electrically insulating material.
  • the start-up line is connected to the positive, the plasma lance to the negative pole of a power source.
  • the energy consumption was 56 kWh, composed of: 46 kWh for heating the hydrogen, 7 kWh for heating the titanium tetrachloride and 3 kWh reaction energy.
  • the energy consumption was 46.4 kWh, composed of: 35.8 kWh for heating the hydrogen, 7.6 kWh for heating the titanium tetrachloride and 3 kWh of reaction energy.
  • the energy consumption was 35.2 kWh, composed of: 23 kWh for heating the hydrogen, 9 kWh for heating the titanium tetrachloride and 3.2 kWh of reaction energy.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
EP84890155A 1983-08-18 1984-08-13 Procédé et installation pour l'élaboration de métaux ou d'alliages Withdrawn EP0134780A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AT2954/83 1983-08-18
AT0295483A AT378539B (de) 1983-08-18 1983-08-18 Verfahren zur herstellung von metallen oder metallegierungen sowie vorrichtung zur durchfuehrung des verfahrens

Publications (2)

Publication Number Publication Date
EP0134780A2 true EP0134780A2 (fr) 1985-03-20
EP0134780A3 EP0134780A3 (fr) 1986-08-13

Family

ID=3543002

Family Applications (1)

Application Number Title Priority Date Filing Date
EP84890155A Withdrawn EP0134780A3 (fr) 1983-08-18 1984-08-13 Procédé et installation pour l'élaboration de métaux ou d'alliages

Country Status (6)

Country Link
US (1) US4561883A (fr)
EP (1) EP0134780A3 (fr)
JP (1) JPS6070135A (fr)
AT (1) AT378539B (fr)
AU (1) AU3165984A (fr)
CA (1) CA1215677A (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11643704B2 (en) 2017-06-02 2023-05-09 Se Corporation Producing method for producing magnesium hydride, power generation system using magnesium hydride, and producing apparatus for producing magnesium hydride

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5201939A (en) * 1989-12-04 1993-04-13 General Electric Company Method of modifying titanium aluminide composition
US7576296B2 (en) * 1995-03-14 2009-08-18 Battelle Energy Alliance, Llc Thermal synthesis apparatus
US5749937A (en) * 1995-03-14 1998-05-12 Lockheed Idaho Technologies Company Fast quench reactor and method
US6821500B2 (en) 1995-03-14 2004-11-23 Bechtel Bwxt Idaho, Llc Thermal synthesis apparatus and process
US6096109A (en) * 1996-01-18 2000-08-01 Molten Metal Technology, Inc. Chemical component recovery from ligated-metals
WO2001046067A1 (fr) * 1999-12-21 2001-06-28 Bechtel Bwxt Idaho, Llc Production d'hydrogene et de carbone elementaire a partir de gaz naturel et d'autres hydrocarbures
WO2005035807A1 (fr) * 2003-09-19 2005-04-21 Sri International Methodes et appareils de production de compositions metalliques par reduction d'halogenures metallises
US7354561B2 (en) * 2004-11-17 2008-04-08 Battelle Energy Alliance, Llc Chemical reactor and method for chemically converting a first material into a second material
CN101432453B (zh) * 2006-04-28 2011-12-28 Sri国际公司 用于生产固结的和纯化的材料的方法
US8591821B2 (en) * 2009-04-23 2013-11-26 Battelle Energy Alliance, Llc Combustion flame-plasma hybrid reactor systems, and chemical reactant sources
CA3169637A1 (fr) * 2011-03-14 2012-09-20 Pyrogenesis Canada Inc. Procede pour rendre au maximal une recuperation d'energie dans des procedes dechets-en-energie
CN103137857B (zh) * 2011-12-02 2016-01-06 中芯国际集成电路制造(上海)有限公司 隧道绝缘材料层的形成方法及形成装置
JP6487087B2 (ja) * 2018-03-13 2019-03-20 株式会社エスイー 金属マグネシウムの製造方法とその製造装置
KR102247338B1 (ko) * 2018-12-14 2021-05-04 재단법인 포항산업과학연구원 입상 물질 제조 방법 및 제조 장치

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2760857A (en) * 1951-09-05 1956-08-28 Fulmer Res Inst Ltd Production and purification of titanium
US3211548A (en) * 1961-11-23 1965-10-12 Ciba Ltd Process for the production of tantalum or niobium in a hydrogen plasma jet
FR1441152A (fr) * 1965-07-22 1966-06-03 Rio Algom Mines Ltd Fabrication de métaux directement à partir de leurs halogénures
FR2341389A1 (fr) * 1976-02-17 1977-09-16 Montedison Spa Procede de production de poudres de produits ceramiques, metalliques ou similaires par arc au plasma

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3380904A (en) * 1965-04-20 1968-04-30 Dev Corp Confining the reaction zone in a plasma arc by solidifying a confining shell around the zone
US3429691A (en) * 1966-08-19 1969-02-25 Aerojet General Co Plasma reduction of titanium dioxide
GB1278495A (en) * 1969-08-08 1972-06-21 Ian George Sayce Production of flourine or volatile fluorine compounds by melt electrolysis
GB1462056A (en) * 1973-09-07 1977-01-19 Electricity Council Process and apparatus for chemical reactions in the presence of electric discharge

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2760857A (en) * 1951-09-05 1956-08-28 Fulmer Res Inst Ltd Production and purification of titanium
US3211548A (en) * 1961-11-23 1965-10-12 Ciba Ltd Process for the production of tantalum or niobium in a hydrogen plasma jet
FR1441152A (fr) * 1965-07-22 1966-06-03 Rio Algom Mines Ltd Fabrication de métaux directement à partir de leurs halogénures
FR2341389A1 (fr) * 1976-02-17 1977-09-16 Montedison Spa Procede de production de poudres de produits ceramiques, metalliques ou similaires par arc au plasma

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11643704B2 (en) 2017-06-02 2023-05-09 Se Corporation Producing method for producing magnesium hydride, power generation system using magnesium hydride, and producing apparatus for producing magnesium hydride

Also Published As

Publication number Publication date
AU3165984A (en) 1985-02-21
EP0134780A3 (fr) 1986-08-13
AT378539B (de) 1985-08-26
ATA295483A (de) 1985-01-15
CA1215677A (fr) 1986-12-23
US4561883A (en) 1985-12-31
JPS6070135A (ja) 1985-04-20

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