EP0202174B1 - Procédé et dispositif de purification du lithium - Google Patents

Procédé et dispositif de purification du lithium Download PDF

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Publication number
EP0202174B1
EP0202174B1 EP86420106A EP86420106A EP0202174B1 EP 0202174 B1 EP0202174 B1 EP 0202174B1 EP 86420106 A EP86420106 A EP 86420106A EP 86420106 A EP86420106 A EP 86420106A EP 0202174 B1 EP0202174 B1 EP 0202174B1
Authority
EP
European Patent Office
Prior art keywords
lithium
temperature
process according
enclosure
condensation
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.)
Expired
Application number
EP86420106A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0202174A1 (fr
Inventor
Raymond Roumieu
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.)
Metaux Speciaux SA
Original Assignee
Metaux Speciaux 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
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=9318850&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP0202174(B1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Metaux Speciaux SA filed Critical Metaux Speciaux SA
Priority to AT86420106T priority Critical patent/ATE35293T1/de
Publication of EP0202174A1 publication Critical patent/EP0202174A1/fr
Application granted granted Critical
Publication of EP0202174B1 publication Critical patent/EP0202174B1/fr
Expired legal-status Critical Current

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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
    • C22B26/10—Obtaining alkali metals
    • C22B26/12—Obtaining lithium
    • 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
    • C22B9/04—Refining by applying a vacuum

Definitions

  • the present invention relates to a method and a device for purifying lithium, in particular sodium and potassium.
  • the lithium used for this purpose must have a suitable purity, in particular it must contain very few alkali metals such as sodium and potassium because these elements significantly degrade the mechanical characteristics of aluminum alloys.
  • the lithium obtained by chemical or electrochemical route generally contains sodium coming from the raw material and potassium in particular when it is manufactured electrolytically because this technique implements most often baths of molten salts containing chloride of potassium and that this compound dissociates partially during electrolysis, giving rise to a deposit of potassium simultaneously with lithium.
  • lithium can be purified from potassium by distilling the hydride at around 700 ° C. or else simultaneously lowering the sodium and potassium content by distilling the lithium at around 400-450 ° C. under a very low pressure of the order from 1.10- 3 Pascal approximately.
  • This process therefore consists in having melted the mass of lithium to be purified away from air in order to avoid its oxidation, in subjecting the bath thus formed to stirring so as to permanently renew the free surface which it presents. in the container where it was originally placed.
  • This agitation can be obtained for any mechanical means such as agitator or electric such as electromagnetic coils supplied with alternating current, which induce in the bath of the electric forces which by interaction with the magnetic field which they create, develop forces of Laplace own to the commotion.
  • the metal is maintained at a temperature between 400 and 700 ° C and reduced atmospheric pressure on the free surface of the bath to a value less than 10 Pascal, so as to cause evaporation.
  • Maintaining the indicated temperature can be achieved by means of heating elements placed at the end of the bath so as to prevent their corrosion by lithium.
  • this is obtained by any suitable pumping device, such as for example the combination of a vane pump and a diffusion pump.
  • the chosen temperature range results from the fact that a higher temperature increases the lithium losses while a lower temperature reduces the rate of evaporation. In this range, a pressure below 10 Pascal must be maintained to have sufficient evaporation. But these conditions most favorable to the implementation of the method correspond to a temperature between 530 and 570 ° C and at a pressure between 1 and 1.10- 1.10- 3 Pascal.
  • the process also includes a condensation phase which makes it possible to collect, in the liquid or solid state, the impurities which have evaporated.
  • This condensation takes place at a temperature below 100 ° C and preferably below 50 ° C. It is indeed desirable to condense at the lowest possible temperature in order to be able to promote evaporation and to maintain a speed compatible with the desired productivity.
  • the invention also includes a device for implementing the method.
  • the condensation surface is at least equal to the evaporation surface in order to keep the process all its efficiency in purification.
  • the enclosure having been purged of its air by introducing into (8) an argon current which can be evacuated by the valve, the impure lithium is introduced into the container by the supply means by following the level by means of the probe and heated by means of electrical resistances to the suitable temperature regulated by the thermocouple placed in (7).
  • the enclosure is put under suitable pressure by switching on the pumping device while the lower part is cooled by sending a cold fluid into the jacket so as to maintain the temperature of the condensing surface at the desired value and controlled by the thermocouple placed in (19).
  • the stirring means is then put into service.
  • the impurities escape to the evaporation surface of the metal bath and the vapors condense on the condensation surface.
  • the heat transfer fluid is brought to a temperature sufficient to melt the condensed impurities, preferably between 100 and 200 °.

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
EP86420106A 1985-04-24 1986-04-22 Procédé et dispositif de purification du lithium Expired EP0202174B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT86420106T ATE35293T1 (de) 1985-04-24 1986-04-22 Verfahren und vorrichtung zur lithiumraffination.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8506606 1985-04-24
FR8506606A FR2581080B1 (fr) 1985-04-24 1985-04-24 Procede et dispositif de purification du lithium

Publications (2)

Publication Number Publication Date
EP0202174A1 EP0202174A1 (fr) 1986-11-20
EP0202174B1 true EP0202174B1 (fr) 1988-06-22

Family

ID=9318850

Family Applications (1)

Application Number Title Priority Date Filing Date
EP86420106A Expired EP0202174B1 (fr) 1985-04-24 1986-04-22 Procédé et dispositif de purification du lithium

Country Status (12)

Country Link
US (2) US4738716A (es)
EP (1) EP0202174B1 (es)
JP (2) JPS61253331A (es)
CN (1) CN1004081B (es)
AT (1) ATE35293T1 (es)
CA (1) CA1272033A (es)
DD (1) DD244766A5 (es)
DE (1) DE3660338D1 (es)
ES (1) ES8704550A1 (es)
FR (1) FR2581080B1 (es)
IL (1) IL78580A (es)
IN (1) IN162925B (es)

Families Citing this family (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4781756A (en) * 1987-07-02 1988-11-01 Lithium Corporation Of America Removal of lithium nitride from lithium metal
DE8811839U1 (de) * 1988-09-17 1989-02-02 Degussa Ag, 6000 Frankfurt Gasdichter Behälter für Warmlagerung und -transport
CN1059709C (zh) * 1997-11-05 2000-12-20 北京市吉利源系统工程公司 金属锂真空蒸馏提纯方法及装置
US6048507A (en) * 1997-12-09 2000-04-11 Limtech Process for the purification of lithium carbonate
AU2002212010A1 (en) * 2000-10-27 2002-05-06 Mcgill University Recovery of purified volatile metal such as lithium from mixed metal vapours
CN100487143C (zh) * 2003-11-14 2009-05-13 昆明永年锂业有限公司 高纯锂的制备方法
CN100339498C (zh) * 2005-06-16 2007-09-26 王洪 高钠金属锂及其制造方法
CN100432248C (zh) * 2006-06-27 2008-11-12 戴日桃 特纯金属锂精炼提纯工艺
CN101892394B (zh) * 2009-12-18 2013-07-24 中南大学 一种从锂云母中提取锂的方法和设备
US8679224B2 (en) 2011-08-31 2014-03-25 Babcock & Wilcox Technical Services Y-12, Llc Hydrogen, lithium, and lithium hydride production
CN104388688B (zh) * 2014-11-17 2016-07-06 东北大学 一种真空金属热还原炼锂的装置及方法
CN108107092B (zh) * 2017-11-17 2019-09-27 清华大学 一种带有参比电极的锂离子电池的浸润制备方法
US11761057B1 (en) 2022-03-28 2023-09-19 Lyten, Inc. Method for refining one or more critical minerals

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2879157A (en) * 1955-10-04 1959-03-24 Mine Safety Appliances Co Purification of alkali metals by heat transfer
JPS5224104A (en) * 1975-07-23 1977-02-23 Vladimir Semenobuitsuchi Chier Apparatus for continuous vacuum refining of metals
JPS52133010A (en) * 1976-04-30 1977-11-08 Japan Atom Energy Res Inst Purifying apparatus for liquid metallic lithium
CH659000A5 (de) * 1981-11-07 1986-12-31 Leybold Heraeus Gmbh & Co Kg Destillations- und sublimationsvorrichtung mit einem kondensator.
JPS61133331A (ja) * 1984-11-30 1986-06-20 Toyota Motor Corp 金属の蒸留方法及び装置
FR2574091B1 (fr) * 1984-12-04 1988-12-23 Novatome Procede et dispositif de traitement prealable de sodium liquide contenant des impuretes dissoutes

Also Published As

Publication number Publication date
ES8704550A1 (es) 1987-04-01
FR2581080A1 (fr) 1986-10-31
US4842254A (en) 1989-06-27
IN162925B (es) 1988-07-23
DE3660338D1 (en) 1988-07-28
ATE35293T1 (de) 1988-07-15
JPH0368937B2 (es) 1991-10-30
CA1272033A (fr) 1990-07-31
DD244766A5 (de) 1987-04-15
FR2581080B1 (fr) 1987-06-19
CN86102633A (zh) 1986-12-03
CN1004081B (zh) 1989-05-03
IL78580A0 (en) 1986-08-31
ES554264A0 (es) 1987-04-01
JP2615124B2 (ja) 1997-05-28
JPS6479330A (en) 1989-03-24
JPS61253331A (ja) 1986-11-11
EP0202174A1 (fr) 1986-11-20
IL78580A (en) 1989-01-31
US4738716A (en) 1988-04-19

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