EP0217438B2 - Verfahren und Vorrichtung zur Herstellung von Lithiummetall hoher Reinheit durch Schmelzflusselektrolyse - Google Patents

Verfahren und Vorrichtung zur Herstellung von Lithiummetall hoher Reinheit durch Schmelzflusselektrolyse Download PDF

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Publication number
EP0217438B2
EP0217438B2 EP86201529A EP86201529A EP0217438B2 EP 0217438 B2 EP0217438 B2 EP 0217438B2 EP 86201529 A EP86201529 A EP 86201529A EP 86201529 A EP86201529 A EP 86201529A EP 0217438 B2 EP0217438 B2 EP 0217438B2
Authority
EP
European Patent Office
Prior art keywords
electrolytic cell
lithium
lithium metal
molten
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.)
Expired - Lifetime
Application number
EP86201529A
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German (de)
English (en)
French (fr)
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EP0217438B1 (de
EP0217438A1 (de
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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Application filed by Metallgesellschaft AG filed Critical Metallgesellschaft AG
Priority to AT86201529T priority Critical patent/ATE48658T1/de
Publication of EP0217438A1 publication Critical patent/EP0217438A1/de
Application granted granted Critical
Publication of EP0217438B1 publication Critical patent/EP0217438B1/de
Publication of EP0217438B2 publication Critical patent/EP0217438B2/de
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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 is known 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 that 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-like end of the cathode, a natural circulation of the melt is brought about. A further reaction of the lithium metal should not take place in the melt mixture.
  • Contaminants of any kind are 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 as set out in claim 1.
  • 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 charged 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. That is, there should neither be a separation in the electrolysis vessel which can be caused by an outflow velocity which is too low, nor a flow velocity which is too high, so that chlorine gas or air is drawn 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 caused 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.
  • From the Separation space is, after building up a buffer volume of liquid lithium and cleaned by segregation, the lithium continuously discharged into a template and z. B. shed and let cool.
  • a protective gas atmosphere for example of argon, is maintained in the separation space above the melt level.
  • 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 the part of the graphite anode which is immersed in the molten salt and which is vertically and gas-tight against the atmosphere surrounds, as well as with organs for introducing lithium chloride, protective gas and for supplying electrical energy and for discharging lithium metal and chlorine gas.
  • the cylindrical steel container fulfills the task of a separating pipe or separator, d. H. 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 in order to generate a pump drum at the entrance of the U-tube or a flow directed into the separating tube. For the purposes of the invention, this includes, for example, agitators, such as propeller stirrers, screw conveyors or centrifugal pumps.
  • the drive means are inserted through the upper cover, through which an inlet for protective gas is also expediently guided.
  • the siphon-like tube (15) over its entire length, i. H. 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 share 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.
  • the mammoth pump effect serves as the conveying force? »Of the rising chlorine gas.
  • the upper edge of the cathode is 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.
  • the circulation of the molten electrolyte is made possible via the openings 9 in the lower part of the cathode wall.
  • lithium chloride is added to the molten salt mixture in accordance with the consumption charged. 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, protrudes 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 pipe 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 pipe 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 shaped piece 6 is protected against corrosive attack by the melt by solidified melt 20.
  • a eutectic salt mixture of approximately 50% by weight lithium chloride and approximately 50% by weight potassium chloride serves as the electrolyte.
  • the operating temperature is 400 ° C.
  • the current density is 5,000 to 10,000 amps / m 2, preferably 6,000 amps / 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 high flow speed.
  • the high flow velocity in the U-tube is generated by a paddle mixer.
  • the metallic lithium separates from the molten salt mixture containing lithium metal 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, in a manner known per se, processed further under suitable conditions, such as under a protective gas atmosphere or in vacuo.
  • the high purity lithium metal obtained by the process according to the invention has the following analysis:

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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 Verfahren und Vorrichtung zur Herstellung von Lithiummetall hoher Reinheit durch Schmelzflusselektrolyse Expired - Lifetime EP0217438B2 (de)

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 EP0217438A1 (de) 1987-04-08
EP0217438B1 EP0217438B1 (de) 1989-12-13
EP0217438B2 true EP0217438B2 (de) 1992-09-02

Family

ID=6281061

Family Applications (1)

Application Number Title Priority Date Filing Date
EP86201529A Expired - Lifetime EP0217438B2 (de) 1985-09-14 1986-09-05 Verfahren und Vorrichtung zur Herstellung von Lithiummetall hoher Reinheit durch Schmelzflusselektrolyse

Country Status (6)

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

Families Citing this family (32)

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GB2216898B (en) * 1988-03-29 1992-01-02 Metallurg Inc Transporting a liquid past a barrier
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
US5935394A (en) * 1995-04-21 1999-08-10 Alcan International Limited Multi-polar cell for the recovery of a metal by electrolysis of a molten electrolyte
US5855757A (en) * 1997-01-21 1999-01-05 Sivilotti; Olivo Method and apparatus for electrolysing light metals
US5660710A (en) * 1996-01-31 1997-08-26 Sivilotti; Olivo Method and apparatus for electrolyzing 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
CA2336685C (en) 1998-07-08 2004-12-14 Alcan International Limited Molten salt electrolytic cell having metal reservoir
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
EP3521460A1 (en) 2014-09-09 2019-08-07 MetOxs 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
CA3183180A1 (en) * 2021-01-21 2022-07-28 Maciej Jastrzebski Electrorefining apparatus and process for refining lithium metal
KR20230131926A (ko) * 2021-01-21 2023-09-14 리-메탈 코포레이션 금속 생산물의 생산을 위한 전해 채취 셀 및 그의 사용방법
EP4263911A4 (en) * 2021-01-21 2025-09-03 Li Metal Corp PROCESS FOR PRODUCING REFINED LITHIUM METAL
KR20240135749A (ko) * 2022-01-13 2024-09-12 하이드로-퀘벡 Li 금속을 생성하기 위한 장치 및 방법
US11976375B1 (en) 2022-11-11 2024-05-07 Li-Metal Corp. Fracture resistant mounting for ceramic piping

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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
FR2560221B1 (fr) * 1984-02-24 1989-09-08 Rhone Poulenc Spec Chim Procede et dispositif pour la fabrication de lithium en continu

Also Published As

Publication number Publication date
JPS6267190A (ja) 1987-03-26
EP0217438B1 (de) 1989-12-13
US4740279A (en) 1988-04-26
CA1330772C (en) 1994-07-19
DE3532956A1 (de) 1987-03-19
EP0217438A1 (de) 1987-04-08
JPH0465912B2 (enrdf_load_stackoverflow) 1992-10-21
DE3667503D1 (de) 1990-01-18
ATE48658T1 (de) 1989-12-15

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