EP0217438A1 - Procédé et dispositif pour la production de lithium très pur par électrolyse ignée - Google Patents

Procédé et dispositif pour la production de lithium très pur par électrolyse ignée Download PDF

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Publication number
EP0217438A1
EP0217438A1 EP86201529A EP86201529A EP0217438A1 EP 0217438 A1 EP0217438 A1 EP 0217438A1 EP 86201529 A EP86201529 A EP 86201529A EP 86201529 A EP86201529 A EP 86201529A EP 0217438 A1 EP0217438 A1 EP 0217438A1
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EP
European Patent Office
Prior art keywords
lithium
electrolytic cell
electrolysis
lithium metal
cell
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.)
Granted
Application number
EP86201529A
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German (de)
English (en)
Other versions
EP0217438B1 (fr
EP0217438B2 (fr
Inventor
Jürgen Dr. Müller
Richard Dr. Bauer
Bernd Sermond
Eike Dr. Dolling
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.)
GEA Group AG
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Metallgesellschaft AG
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Publication date
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Application filed by Metallgesellschaft AG filed Critical Metallgesellschaft AG
Priority to AT86201529T priority Critical patent/ATE48658T1/de
Publication of EP0217438A1 publication Critical patent/EP0217438A1/fr
Publication of EP0217438B1 publication Critical patent/EP0217438B1/fr
Application granted granted Critical
Publication of EP0217438B2 publication Critical patent/EP0217438B2/fr
Anticipated expiration legal-status Critical
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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
    • C25C3/02—Electrolytic production, recovery or refining of metals by electrolysis of melts of alkali or alkaline earth metals

Definitions

  • the invention relates to a method for producing high-purity metallic lithium by melt flow electrolysis and to an electrolytic cell for carrying out the method.
  • Metallic lithium is obtained in technical practice by electrolysis of a molten mixture of lithium chloride and potassium chloride.
  • the potassium chloride portion serves in a known manner to lower the melting point of the lithium chloride.
  • Suitable electrolysis cells are, for example, cells without a diaphragm. Such cells have a housing made of steel, a steel cathode and a graphite anode. The cell has no inner lining.
  • the molten metallic lithium collects on the surface of the molten salt. From there it is skimmed off using ladles, or it can also be pulled off by lifting devices.
  • the developed and outflowing chlorine gas allows air to enter the cell, so there is a risk of oxidation and nitridation of the liquid metal.
  • EP-OS 107 521 discloses a process for the continuous production of lithium metal by electrolysis of lithium chloride in a molten salt mixture in an electrolysis cell with a cylindrical steel cathode inserted into the cell bottom and a graphite anode immersed in the cylinder.
  • the lithium metal salt melt is removed from the cell and the lithium metal is separated outside the cell. Due to the chlorine gas development and the venturi A natural circulation of the melt is brought about in the manner of a trained end of the cathode. A further reaction of the lithium metal should not take place in the melt mixture.
  • Contamination of any kind is extremely undesirable in lithium metal if it is to be used for nuclear purposes, for the production of alloys and for lithium batteries.
  • the invention has for its object to provide a method for producing lithium metal of high purity and to provide a suitable device for performing the method.
  • the invention solves the problem with a method for producing metallic lithium by electrolysis Molten salt mixture of lithium chloride and potassium chloride in a diaphragm-free electrolysis cell, stripping off the molten lithium, transferring it to a receiver and cooling.
  • the invention consists in collecting the metallic lithium-containing melt mixture rising in the electrode space in a ring zone surrounding the upper cathode end in the region of the melt level and from this via a siphon-like pipe connection into a communicating with the electrolytic cell and against its chlorine gas atmosphere closed separation space is withdrawn, electrolyte and lithium metal are separated in the separation space under a protective gas atmosphere and the lithium metal is discharged into a receiver under a protective gas atmosphere with recirculation of the electrolyte.
  • the lithium metal discharged is further processed in a manner known per se, for example cast into bars. While the electrolyte is being circulated in the electrolysis cell and returned to the electrode space, the anodically separated chlorine gas is sucked out of the covered gas space via the melt and obtained as such or in the form of salts.
  • the chlorine gas stream is expediently drawn through an absorption system which is loaded with a slurry of lithium hydroxide, with the use of ammonia as a reducing agent in accordance with:
  • the lithium chloride obtained in this way again serves as a raw material for the electrolysis.
  • the metal-containing electrolyte directed into the separation space is created in the siphon-like pipe connection and that the metal / molten salt mixture rising in the electrode space is immediately discharged into the separation space.
  • the level of the electrolyte melt can also be kept constant by controlled immersion of a neutral body in the electrolyte melt. In the practical implementation of the method according to the invention, the ascending metal / molten salt mixture remains on the bath surface for about 2 seconds or less.
  • the electrolyte flow is at least partially caused by the " mammoth pump effect" of the rising chlorine gas and, furthermore, is generated by a pumping effect, which is brought about by mechanical means, in the shorter leg of a siphon-like connecting tube between the electrolysis space or the annular space and the separation space.
  • Mechanical units known per se such as pumps or stirrers, are suitable for the mechanical generation of the electrolyte flow.
  • the invention further provides an electrolysis cell for carrying out the method according to the invention.
  • an electrolysis cell of the type mentioned at the outset for the electrolytic extraction of metallic lithium a steel cathode being welded to the bottom of the container in a cylindrical, closed electrolysis steel container, and which is welded into the molten salt surrounding immersed part of a graphite anode arranged vertically and gastight against the atmosphere, and with organs for introducing lithium chloride, protective gas and for supplying electrical energy and for discharging lithium metal and chlorine gas.
  • the improvement according to the invention is that in the electrolysis steel container, a steel cylinder which is closed at the top is arranged eccentrically, which projects above the electrolysis container and sits on the bottom of the vessel, and an essentially U in the cylinder wall in the lower part thereof -shaped tube is welded, the shorter leg opens into the center of the separating tube and the longer leg opens into a ring trough which surrounds the upper end of the steel cathode, and wherein the cylinder jacket has openings in the lower part.
  • the cylindrical steel container fulfills the task of a separating pipe or separator, ie liquid metallic lithium and electrolyte melt separate in it.
  • the separating tube therefore has a small diameter which is approximately 1/10 of the diameter of the electrolysis container.
  • the siphon-like tube which is connected on the one hand to the electrolysis cell or to the ring trough surrounding the upper cathode edge and on the other hand to the separating tube, has an essential function as an overflow tube for the metal / molten salt mixture.
  • a mechanical conveyor is arranged in the shorter leg of the siphon-like tube to generate a pump drum at the entrance of the U-tube or a flow directed into the separating tube.
  • this includes, for example, agitators, such as propeller stirrers, screw conveyors or centrifugal pumps.
  • the drive means are inserted through the top cover, through which an inlet for protective gas is also expediently led.
  • the siphon-like tube (15) over its entire length i.e. in the longer and shorter leg, has the same diameter.
  • the longer leg (16a) or the suction pipe has a smaller diameter than the shorter leg.
  • the upper section of the shorter leg is expanded into a cylindrical part of larger diameter (16).
  • the ratio of smaller to larger diameter is 1: 2 to 1:12 and preferably 1: 5 to 1:10.
  • the graphite anode is inserted through the lid into the electrolysis vessel. It can be attached to the lid and protrude hanging into the cathode compartment. However, it is expediently passed through the lid in an insulating and easily replaceable manner and then sits on the iron container bottom via an electrically insulating molded part.
  • Such an insulating molded part advantageously consists of oxide-ceramic material, for example of molten aluminum oxide.
  • the insulating molded part is expediently protected against the corrosive attack of the molten electrolyte by partially solidified molten salt during cell operation. This is achieved by suitable temperature control.
  • the graphite anode can be designed as a solid plate or solid cylinder. Accordingly, the cathode is also designed as a box-shaped hollow cathode or as a hollow cylinder. The cathode and cell are at the same potential. The negative pole of the voltage source is connected to the cell bottom.
  • the upper edge of the cathode protrudes beyond the level of the molten electrolyte.
  • Around the outer edge of the cathode has an annular collecting channel is provided, which the ascending, L receives ithiummetall containing electrolyte and conveys it directly through an opening in the bottom of the gutter in the long leg of the siphon tube.
  • the " mammoth pump effect" of the rising chlorine gas serves as the pumping force.
  • the upper edge of the cathode is, as is usual with overflow edges, in the form of a ring gear.
  • the figure in the figure shows a device according to the invention.
  • the cathode 3 is arranged in the electrolysis cell 1 closed by cover 2 and welded to the bottom of the vessel.
  • the upper edge of the cathode 3 is provided with a collecting channel 4 for the molten salt metal which overflows.
  • the graphite anode 5 is inserted through the cover 2 and is seated on the bottom of the electrolytic cell 1 via the insulating body 6 and is surrounded by the cathode 3.
  • the positive pole of a DC power source is connected at 7 and the negative pole at 8. Via the openings 9 in the lower part of the K athodenwand the circulation of the molten electrolyte is made possible.
  • lithium chloride is recharged into the molten salt mixture in accordance with the consumption. Developed chlorine gas escapes through the outlet 11.
  • a separating tube 12 which is closed with a lid 13, is also arranged.
  • the separating tube 12 is welded into the cover 2 of the electrolytic cell 1, projects above the cell and leads to the bottom of the cell 1.
  • openings 14 enable the molten salt to be balanced with the other molten electrolyte.
  • the separating pipe 12 is connected to the gutter 4 via the siphon-like connecting pipe 15.
  • the U-shaped connecting tube 15 is inserted with its longer leg into the bottom of the gutter 4, while the opening of the shorter leg is widened to a larger tube diameter 16.
  • a stirrer 17 is arranged in the tube part 16, the shaft of which is inserted through the cover 13 of the separating tube 12.
  • an inlet for protective gas is also attached.
  • the molten lithium metal is discharged from the separating tube via the tube 19.
  • the insulating molded piece 6 is protected against corrosive attack by the melt by solidified melt 20.
  • a eutectic salt mixture of approx. 50% by weight lithium chloride and approx.
  • the operating temperature is 400 ° C.
  • the current density is 5,000 to 10,000 amps / m 2 , preferably 6,000 A mp./m 2 .
  • the cell voltage is accordingly 6.2 to 9.2 volts.
  • the current yield is over 90%.
  • Normal structural steel is used as the material for the cell and cathode.
  • the wall thickness of the cell is about 20 mm, the cell has no ceramic lining.
  • the anode made of electrographite is inserted centrally in the cathode compartment. The distance between the electrodes is about 50 mm.
  • the anodically separated chlorine collects in the gas space above the molten salt and is removed from the cell at a low vacuum.
  • the molten salt mixture containing lithium metal rising from the electrode space runs into the collecting trough.
  • the lithium metal, which is already partially floating there, is immediately conveyed to the inlet of the siphon-like pipe with a great deal of melt at a high flow rate.
  • the high flow velocity in the U-tube is generated by a paddle mixer.
  • the metallic lithium separates from the molten salt mixture containing argon under an argon atmosphere and floats, while the molten salt mixture leaves the separating tube in a downward flow and returns to the circuit.
  • the molten lithium metal collected cleans itself of further impurities by segregation and is discharged continuously or discontinuously and further processed under suitable conditions, such as under a protective gas atmosphere or in a vacuum, in a manner known per se. That according to the inventive method
  • the obtained high-purity lithium metal has the following analysis: The advantages of the process according to the invention can be seen in the fact that metallic lithium of high purity is obtained economically in a device of simple and technically not complex construction in continuous operation.

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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)
EP86201529A 1985-09-14 1986-09-05 Procédé et dispositif pour la production de lithium très pur par électrolyse ignée Expired - Lifetime EP0217438B2 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT86201529T ATE48658T1 (de) 1985-09-14 1986-09-05 Verfahren und vorrichtung zur herstellung von lithiummetall hoher reinheit durch schmelzflusselektrolyse.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19853532956 DE3532956A1 (de) 1985-09-14 1985-09-14 Verfahren und vorrichtung zur herstellung von lithiummetall hoher reinheit durch schmelzflusselektrolyse
DE3532956 1985-09-14

Publications (3)

Publication Number Publication Date
EP0217438A1 true EP0217438A1 (fr) 1987-04-08
EP0217438B1 EP0217438B1 (fr) 1989-12-13
EP0217438B2 EP0217438B2 (fr) 1992-09-02

Family

ID=6281061

Family Applications (1)

Application Number Title Priority Date Filing Date
EP86201529A Expired - Lifetime EP0217438B2 (fr) 1985-09-14 1986-09-05 Procédé et dispositif pour la production de lithium très pur par électrolyse ignée

Country Status (6)

Country Link
US (1) US4740279A (fr)
EP (1) EP0217438B2 (fr)
JP (1) JPS6267190A (fr)
AT (1) ATE48658T1 (fr)
CA (1) CA1330772C (fr)
DE (2) DE3532956A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1989009296A1 (fr) * 1988-03-29 1989-10-05 Metallurg, Inc. Transport d'un liquide au-dela d'une barriere

Families Citing this family (32)

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US4882017A (en) * 1988-06-20 1989-11-21 Aluminum Company Of America Method and apparatus for making light metal-alkali metal master alloy using alkali metal-containing scrap
US4973390A (en) * 1988-07-11 1990-11-27 Aluminum Company Of America Process and apparatus for producing lithium from aluminum-lithium alloy scrap in a three-layered lithium transport cell
US4988417A (en) * 1988-12-29 1991-01-29 Aluminum Company Of America Production of lithium by direct electrolysis of lithium carbonate
US5417815A (en) * 1994-02-07 1995-05-23 Martin Marietta Energy Systems, Inc. Liquid surface skimmer apparatus for molten lithium and method
WO1996033297A1 (fr) * 1995-04-21 1996-10-24 Alcan International Limited Cellule multipolaire pour la recuperation d'un metal par electrolyse d'un electrolyte fondu
US5660710A (en) * 1996-01-31 1997-08-26 Sivilotti; Olivo Method and apparatus for electrolyzing light metals
US5855757A (en) * 1997-01-21 1999-01-05 Sivilotti; Olivo Method and apparatus for electrolysing light metals
US6056803A (en) * 1997-12-24 2000-05-02 Alcan International Limited Injector for gas treatment of molten metals
RU2135615C1 (ru) * 1997-12-25 1999-08-27 Открытое акционерное общество "Новосибирский завод химконцентратов" Способ получения лития
US6497807B1 (en) 1998-02-11 2002-12-24 Northwest Aluminum Technologies Electrolyte treatment for aluminum reduction
JP3870026B2 (ja) 1998-07-08 2007-01-17 住友チタニウム株式会社 金属用の液溜を備えた溶融塩電解セル
DE19859563B4 (de) * 1998-12-22 2008-01-24 Basf Ag Verbessertes Verfahren zur elektrochemischen Herstellung von Alkalimetall aus Alkalimetallamalgam
US6436272B1 (en) 1999-02-09 2002-08-20 Northwest Aluminum Technologies Low temperature aluminum reduction cell using hollow cathode
US6787019B2 (en) * 2001-11-21 2004-09-07 E. I. Du Pont De Nemours And Company Low temperature alkali metal electrolysis
JP2009019250A (ja) * 2007-07-13 2009-01-29 Osaka Titanium Technologies Co Ltd 金属製造方法および装置
CN101469373B (zh) * 2007-12-28 2011-05-11 中国蓝星（集团）股份有限公司 一种制锂装置
DE102008031437A1 (de) * 2008-07-04 2010-01-07 Siemens Aktiengesellschaft Mobiler Energieträger und Energiespeicher
JP5470332B2 (ja) * 2010-06-24 2014-04-16 アイ’エムセップ株式会社 アンモニア電解合成方法とアンモニア電解合成装置
CN101962782A (zh) * 2010-08-11 2011-02-02 华东理工大学 一种去除锂电解质KCl-LiCl中杂质Al的方法
CN102002730A (zh) * 2010-12-08 2011-04-06 华东理工大学 一种去除锂电解质KCl-LiCl中杂质MgCl2的方法
AU2015315441B2 (en) * 2014-09-09 2020-10-29 Clean Resources PTE. LTD. A system, apparatus, and process for leaching metal and storing thermal energy during metal extraction
JP6610089B2 (ja) * 2014-10-03 2019-11-27 Ｔｄｋ株式会社 安定化リチウム粉及びそれを用いたリチウムイオン二次電池
US9499880B2 (en) 2015-03-06 2016-11-22 Battelle Memorial Institute System and process for production of magnesium metal and magnesium hydride from magnesium-containing salts and brines
CN107574458B (zh) * 2017-09-20 2024-03-29 宜春赣锋锂业有限公司 一种集中收集锂的金属锂电解槽
CN112011803A (zh) * 2020-05-19 2020-12-01 金昆仑锂业有限公司 一种带有集锂室的熔盐电解槽
RU2741723C2 (ru) * 2020-06-09 2021-01-28 Общество с ограниченной ответственностью "Экостар-Наутех" Способ получения металлического лития и установка для его осуществления
EP4263913A4 (fr) 2021-01-21 2025-05-14 Li-Metal Corp. Cellule d'extraction électrolytique pour la production d'un produit métallique et son procédé d'utilisation
AU2022211401A1 (en) * 2021-01-21 2023-08-10 Li-Metal Corp. Process for production refined lithium metal
WO2022155752A1 (fr) * 2021-01-21 2022-07-28 Li-Metal Corp. Appareil d'électroraffinage et procédé de raffinage du lithium métallique
EP4463580A4 (fr) * 2022-01-13 2026-03-25 Hydro Quebec Appareil et procédé de production de lithium métallique
US11976375B1 (en) 2022-11-11 2024-05-07 Li-Metal Corp. Fracture resistant mounting for ceramic piping
KR102879381B1 (ko) * 2023-06-20 2025-10-31 (주)하나기술 리튬 잉곳 연속식 제조장치

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US2862863A (en) * 1957-09-23 1958-12-02 Kenneth F Griffith Apparatus for electrolytic production of a metal product from fused salts
FR2560221A1 (fr) * 1984-02-24 1985-08-30 Rhone Poulenc Spec Chim Procede et dispositif pour la fabrication de lithium en continu
EP0096990B1 (fr) * 1982-06-14 1986-07-30 Alcan International Limited Production de métal par électrolyse d'un électrolyte fondu

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US3396094A (en) * 1962-10-25 1968-08-06 Canada Aluminum Co Electrolytic method and apparatus for production of magnesium
FR2243277B1 (fr) * 1973-09-07 1976-06-18 Commissariat Energie Atomique
US4420381A (en) * 1981-02-26 1983-12-13 Alcan International Limited Electrolytic method and cell for metal production
FR2532332B1 (fr) * 1982-08-31 1986-04-04 Rhone Poulenc Spec Chim Procede pour la preparation continue de lithium par electrolyse du chlorure de lithium dans un melange de sels fondus et appareillage pour la mise en oeuvre dudit procede

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2862863A (en) * 1957-09-23 1958-12-02 Kenneth F Griffith Apparatus for electrolytic production of a metal product from fused salts
EP0096990B1 (fr) * 1982-06-14 1986-07-30 Alcan International Limited Production de métal par électrolyse d'un électrolyte fondu
FR2560221A1 (fr) * 1984-02-24 1985-08-30 Rhone Poulenc Spec Chim Procede et dispositif pour la fabrication de lithium en continu

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1989009296A1 (fr) * 1988-03-29 1989-10-05 Metallurg, Inc. Transport d'un liquide au-dela d'une barriere

Also Published As

Publication number Publication date
EP0217438B1 (fr) 1989-12-13
DE3532956A1 (de) 1987-03-19
JPH0465912B2 (fr) 1992-10-21
EP0217438B2 (fr) 1992-09-02
CA1330772C (fr) 1994-07-19
ATE48658T1 (de) 1989-12-15
DE3667503D1 (de) 1990-01-18
US4740279A (en) 1988-04-26
JPS6267190A (ja) 1987-03-26

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