EP0053566A1 - Verfahren zur elektrolytischen Herstellung von Titan - Google Patents

Verfahren zur elektrolytischen Herstellung von Titan Download PDF

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Publication number
EP0053566A1
EP0053566A1 EP81420174A EP81420174A EP0053566A1 EP 0053566 A1 EP0053566 A1 EP 0053566A1 EP 81420174 A EP81420174 A EP 81420174A EP 81420174 A EP81420174 A EP 81420174A EP 0053566 A1 EP0053566 A1 EP 0053566A1
Authority
EP
European Patent Office
Prior art keywords
titanium
ticl
halide
electrolyte
electrolysis
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Withdrawn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
EP81420174A
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English (en)
French (fr)
Inventor
Marcel Armand
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.)
Pechiney SA
Original Assignee
Pechiney SA
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 Pechiney SA filed Critical Pechiney SA
Publication of EP0053566A1 publication Critical patent/EP0053566A1/de
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
    • C25C3/26—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium
    • C25C3/28—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium of titanium

Definitions

  • the process which is the subject of the invention relates to the preparation of titanium by electrolysis of molten halides. It relates more particularly to the electrolysis of titanium dissolved in an electrolyte based on chlorides using, as starting material, titanium tetrachloride.
  • the electrolysis cell shown in Figure 1 has a container (1) heated from the outside to 520 ° C which contains a molten electrolyte (2), based on a LiCl KCl mixture, in which 8 to 12 are dissolved. % of TiCl 2 .
  • An anode (3) surrounded by a porous diaphragm (4) is connected to the positive pole and a deposition cathode (5) to the negative pole.
  • a porous diaphragm (4) is connected to the positive pole and a deposition cathode (5) to the negative pole.
  • a supply cathode (6) which comprises a supply tube of TiCl 4 (7) whose perforated end (8) is immersed in the electrolyte.
  • the electrolysis current 1 which passes through the electrolyte from the anode, is divided into two parts: a current I 1 which passes through the feed cathode (6) and a current I 2 which passes through the deposition cathode.
  • the titanium must be present in the electrolyte in the bivalent form. It is therefore necessary to reduce to a valence close to 2 the titanium which is introduced at valence 4 in the form of TiCl 4 .
  • reaction (1) and reaction (3) can very well take place at different points of the electrolyte, in particular if the latter is strongly agitated by the introduction of TiCl 4 .
  • reaction (1) and reaction (3) can very well take place at different points of the electrolyte, in particular if the latter is strongly agitated by the introduction of TiCl 4 .
  • the process according to the invention relates to the preparation by electrolysis of titanium dissolved in the form of halide in an electrolyte based on at least one alkali or alkaline earth halide. It is characterized by the use of a supply device which allows titanium to be introduced into the cathode zone of the electrolysis cell in the form of a halide or a mixture of halides of lower average valence to 3.
  • the titanium halides are titanium chlorides obtained by partial reduction of TiCl 4 .
  • An alkali or alkaline earth metal, or alloys of these metals, or titanium or a titanium alloy can be used as reducing agent.
  • This reduction of TiCl 4 to the desired valence level is carried out by means of the reducing agent chosen in a separate installation.
  • the titanium chloride (s) with an average valence of less than 3 are most often obtained in solution in a halide or mixture of molten alkali or alkaline earth halides.
  • This molten mixture thus produced is gradually introduced into the cathode compartment of the electrolyser as and when required. Simultaneously a corresponding quantity of electrolyte depleted in titanium halides is extracted from the anode compartment.
  • FIG. 2 schematically represents an electrolysis cell (10) for the production of titanium, in which the method according to the invention is implemented.
  • This cell is heated from the outside by means not shown.
  • the complex relativizing feed cathode device described above is here replaced by a simple feed tube (11) which makes it possible to introduce the mixture of molten halides containing titanium, in the form of valence ions average less than 3, in the cathode compartment.
  • This tube is connected to an installation, not shown, in which the partial reduction of TiCl 4 is carried out.
  • the cell also comprises a deposition cathode (12) on which the titanium is deposited.
  • a withdrawal tube (15) which makes it possible to extract from the cell amounts of electrolyte equivalent to those which are introduced by the tube ( 11).
  • a tube (16) allows the release of chlorine formed at the anode.
  • the electrolyte thus withdrawn contains very little titanium in solution.
  • a first method of reducing titanium tetrachloride is to carry out this using metallic titanium. Such an operation is particularly justified in the case where there is waste of titanium or titanium-based alloys, in the divided state, such as turnings, falling sheets, etc.
  • electrolytic titanium can also be used, to which its crystalline structure, generally quite loose, confers great reactivity.
  • a second method consists in carrying out this reduction with sodium. It is known, in fact, that TiCl 4 can be reduced by Na according to the following reactions: either in total
  • reducers can be envisaged for the preparation of titanium subchlorides.
  • use may be made of other alkali or alkaline earth metals.
  • alloys of alkali or alkaline earth metals such as NaK or LiK or other alloys.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)
EP81420174A 1980-11-27 1981-11-25 Verfahren zur elektrolytischen Herstellung von Titan Withdrawn EP0053566A1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8025506 1980-11-27
FR8025506A FR2494726A1 (fr) 1980-11-27 1980-11-27 Procede ameliore de preparation de titane par electrolyse

Publications (1)

Publication Number Publication Date
EP0053566A1 true EP0053566A1 (de) 1982-06-09

Family

ID=9248546

Family Applications (1)

Application Number Title Priority Date Filing Date
EP81420174A Withdrawn EP0053566A1 (de) 1980-11-27 1981-11-25 Verfahren zur elektrolytischen Herstellung von Titan

Country Status (5)

Country Link
US (1) US4381976A (de)
EP (1) EP0053566A1 (de)
JP (1) JPS57116791A (de)
FR (1) FR2494726A1 (de)
NO (1) NO814030L (de)

Families Citing this family (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4521281A (en) * 1983-10-03 1985-06-04 Olin Corporation Process and apparatus for continuously producing multivalent metals
EP0148122B1 (de) * 1983-12-23 1988-04-27 Eltech Systems Corporation Verfahren zum Elektroplattieren, elektroplattierter Überzug und Verwendung des Überzuges
US5204057A (en) * 1989-07-14 1993-04-20 Kabushiki Kaisha Toshiba Highly purified titanium material and its named article, a sputtering target
US6210634B1 (en) 1989-07-14 2001-04-03 Kabushiki Kaisha Toshiba Highly purified titanium material, method for preparation of it and sputtering target using it
US6024847A (en) * 1997-04-30 2000-02-15 The Alta Group, Inc. Apparatus for producing titanium crystal and titanium
US6309595B1 (en) 1997-04-30 2001-10-30 The Altalgroup, Inc Titanium crystal and titanium
US6063254A (en) * 1997-04-30 2000-05-16 The Alta Group, Inc. Method for producing titanium crystal and titanium
AUPR602901A0 (en) * 2001-06-29 2001-07-26 Bhp Innovation Pty Ltd Removal of oxygen from metals oxides and solid metal solutions
JP2003129268A (ja) * 2001-10-17 2003-05-08 Katsutoshi Ono 金属チタンの精錬方法及び精錬装置
US7504017B2 (en) * 2001-11-22 2009-03-17 Qit-Fer Et Titane Inc. Method for electrowinning of titanium metal or alloy from titanium oxide containing compound in the liquid state
CN101649472B (zh) * 2008-08-15 2012-06-06 攀钢集团钢铁钒钛股份有限公司 一种制备金属钛的方法
CN101519789A (zh) * 2009-03-30 2009-09-02 攀钢集团研究院有限公司 一种钛循环熔盐电解制取金属钛的方法
CN103882476B (zh) * 2012-12-21 2017-02-15 攀钢集团攀枝花钢铁研究院有限公司 一种含有低价氯化钛的电解质及金属钛的制备方法
CN105088283B (zh) * 2015-09-29 2018-05-11 攀钢集团攀枝花钢铁研究院有限公司 一种提取金属钛的方法
CN107164781A (zh) * 2017-06-05 2017-09-15 攀钢集团研究院有限公司 一种制备超细钛粉的方法
CN107059067A (zh) * 2017-06-05 2017-08-18 攀钢集团研究院有限公司 一种制备超细钛合金粉的方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR1126457A (fr) * 1954-03-23 1956-11-23 Titan Gmbh Procédé de production de titane métallique
US3137641A (en) * 1949-08-10 1964-06-16 Timax Associates Electrolytic process for the production of titanium metal
FR2359221A1 (fr) * 1976-07-23 1978-02-17 Anvar Procede de fabrication de titane par reduction electrolytique dans un bain de sels fondus d'halogenures de titane

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2975111A (en) * 1958-03-19 1961-03-14 New Jersey Zinc Co Production of titanium

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3137641A (en) * 1949-08-10 1964-06-16 Timax Associates Electrolytic process for the production of titanium metal
FR1126457A (fr) * 1954-03-23 1956-11-23 Titan Gmbh Procédé de production de titane métallique
FR2359221A1 (fr) * 1976-07-23 1978-02-17 Anvar Procede de fabrication de titane par reduction electrolytique dans un bain de sels fondus d'halogenures de titane

Also Published As

Publication number Publication date
FR2494726B1 (de) 1984-09-14
JPS57116791A (en) 1982-07-20
US4381976A (en) 1983-05-03
FR2494726A1 (fr) 1982-05-28
NO814030L (no) 1982-05-28

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PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

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Effective date: 19820622

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Inventor name: ARMAND, MARCEL