US3909375A - Electrolytic process for the production of metals in molten halide systems - Google Patents

Electrolytic process for the production of metals in molten halide systems Download PDF

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Publication number
US3909375A
US3909375A US349472A US34947273A US3909375A US 3909375 A US3909375 A US 3909375A US 349472 A US349472 A US 349472A US 34947273 A US34947273 A US 34947273A US 3909375 A US3909375 A US 3909375A
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inter
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separation chamber
gas
gas separation
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Robin David Holliday
Peter Mcintosh
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Conzinc Riotinto of Australia Ltd
Conzinc Riotinto Ltd
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Conzinc Riotinto Ltd
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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
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/005—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells of cells for the electrolysis of melts

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  • Cells of the type discussed are not restricted to production of aluminium and magnesium, but can be applied in any system where the metal product is heavier than the solvent electrolyte, and is formed as a liquid phase for example, lead, bismuth, zinc, cerium, gallium from the respective molten halide (preferably chloride) solvents.
  • the metal product is heavier than the solvent electrolyte, and is formed as a liquid phase for example, lead, bismuth, zinc, cerium, gallium from the respective molten halide (preferably chloride) solvents.
  • the invention may comprise a system for the production of aluminium or magnesium from their respective halide salts wherein molten metal accumulates on the bottom of an electrolytic cell, as in conventional reduction technology, but where the mobile molten pool of metal does not necessarily serve as cathode on which metal is deposited, or through which current is withdrawn from the cell.
  • metal is preferably deposited on non-consumable electrodes which are inclined to the vertical at relatively small angles, for example, to 30, and which are substantially parallel to the opposite electrodes.
  • Such non-consumable electrode sheets may be connected alternately to the positive and negative poles of the power supply and hence may constitute a system of electrodes in parallel.
  • An important feature of the invention is the provision made for facilitating gas, e.g. chlorine, to be liberated from the interelectrode space during electrolysis by means of a suitable gas separation chamber so that said gas is substantially prevented from back reacting with metal in the vicinity of the cathode surface.
  • gas e.g. chlorine
  • the invention comprises a process for the electrolytic production of metals in molten halide systems, wherein metal is deposited on one of a pair of spaced substantially parallel electrodes, the opposed surfaces of which are inclined at an angle of between 5 and 30 to the vertical, and wherein gas liberated in the interelectrode space is discharged upwardly into a gas separation chamber disposed above the inter-electrode space.
  • the cathode surface on which the metal is deposited is inclined at a positive angle to the vertical and the spaced anode surface is inclined at a similar negative angle to the vertical.
  • the electrodes are preferably planar, non-consumable and closely spaced.
  • the opposed surfaces of the electrodes are preferably inclined at an angle of between 7 and 20 to the vertical.
  • the area of the melt surface and the depth of the liquid electrolyte in the gas separation chamber are preferably sufficient to permit separation of gas from the electrolyte in the gas separation chamber at substantially the same rate as said gas is produced in the interelectrode space.
  • FIG. 1 is a highly diagrammatic representation of a gas separation chamber used in explanation of two critical parameters in such a chamber;
  • FIGS. 2 and 3 are diagrammatic side-elevational views of two different cell constructions used in illustrating the differences in operation of two different cell configurations;
  • FIG. 4 is a diagrammatic side elevational view of a multi-electrode cell according to the invention.
  • FIG. 5 is a diagrammatic side elevational view of an alternative embodiment of the invention employing a more compact electrode configuration.
  • the invention in one form relates to cell designs which take maximum advantage of the compactness made possible by using a system of closely spaced planar electrodes inclined at relatively small angles (e.g. 5 to 30). to the vertical, and operating at high current densities, e.g. in excess of l amp/cm (amps per sq.cm), preferably not less than 1.5 amp/cm
  • the inter-electrode spacing is preferably less than 2 inches and preferablybetween 1.2 and 1.8 inches.
  • the angle at which the electrodes are inclined will vary with the normal operating parameters; for example, it may be expected that the angles of inclination will be greater for higher current densities and for smaller interelectrode spacings (A.C.Ds).
  • the invention thus enables the attainment of significant advantages in respect of operating and capital costs.
  • a significant operating advantage of the dry vertical electrode geometry of this invention in general, is the removal of the restriction on cell current or current density, which is always imposed on conventional liquid cathode cells by the magnetic stirring effects of the large currents.
  • the removal of this restriction by elimination of the liquid cathode and by the improved cell geometry of this invention means that cells of several hundred thousand amperes capacity are now brought within the range of practicality.
  • stable values of inter-electrode spacing are maintained without the need for manipulating the electrodes or adjusting the level of the pool of metal accumulated at the base of the cell.
  • Inter-electrode distance has an additional important effect because melt returning to the interelectrode space after having been gas-pumped to the surface may interact with the ascending stream of gas and liquid. This causes gas to be diverted from the upward stream and re-directed down into the interelectrode space.
  • A.C.D. Inter-electrode distance
  • A.C.D. which represents the best compromise between avoidance of gas recirculation and increase of cell voltage because of the increase of current path.
  • FIG. 1 of the accompanying drawings Two critical parameters of the gas separation chamber are the width of the melt surface (i.e. the surface between the liquid electrolyte and gas) in the gas separation chamber, and the depth of liquid electrolyte in the gas separation chamber above the cathode. These two parameters are shown in FIG. 1 of the accompanying drawings as S and D respectively.
  • the numeral 1 indicates the anode
  • 2 indicates the cathode
  • 5 indicates the liquid electrolyte in the gas separation chamber above the cathode 2
  • 8a indicates the quiescent melt level
  • S indicates the width of the melt surface
  • D indicates the depth of the electrolyte in the gas separation chamber above the cathode
  • L indicates the cathode length
  • M indicates the A.C.D. (interelectrode distance).
  • the conventional electrolytic cells used for the reduction of magnesium chloride employ vertical anodes in conjunction with high density electrolytes, i.e. electrolytes which are heavier than the molten magnesium produced, and complex cathode designs are thus necessary to collect the molten magnesium at the surface of the melt.
  • high density electrolytes i.e. electrolytes which are heavier than the molten magnesium produced
  • complex cathode designs are thus necessary to collect the molten magnesium at the surface of the melt.
  • the Blue cell relies upon forced circulation of melt to remove magnesium from the inter-electrode space in cells which use melt systems of higher density than magnesium. In these cells the molten metal floats to the surface. The cell is said to operate at 0.43 to 0.45 amp/cm typical of conventional practice. However, current efficiency is said to be about 75 percent, and it is to be noted that no actual operating conditions are described. The low current efficiency is not surprising, because the design is believed to be quite inadequate for securing separation of chlorine from magnesium. Considerable entrapment of gas between the electrodes must occur because not only are the electrodes devoid of any slope, but the inter-electrode gap is also narrow right up to and beyond the surface of the melt.
  • the cell of Blue et a1. does not provide anything approaching the compactness and efficiency of the cell of the present invention, because of the use oflow current density and more particularly the lack of provision for adequate chlorine removal, which leads to low current efficiency. Further, the expense of the additional components is likely to nullify to a large extent the claimed advantage of being able to incorporate more electrodes at lower A.C.D. within the electrolysis chamber than in conventional plant.
  • cathode surface is inclined at a positive angle, e.g. plus 5 to 30, to the vertical and faces a parallel or substantially parallel planar anode inclined at a negative angle, e.g. minus 5 to 30, to the vertical.
  • a positive angle e.g. plus 5 to 30, to the vertical
  • a parallel or substantially parallel planar anode inclined at a negative angle e.g. minus 5 to 30, to the vertical.
  • the inter-electrode spacing is preferably less than 2 inches, and desirably between 1.2 and 1.8 inches.
  • anodecathode spacing of about 1.5 inches at current densities of 1.5 amp/cm to 2.0 amp/cm?
  • Other parameters of importance in the design of the gas separation chamber are the electrolyte depth above the cathode and the width or area of the surface of the electrolyte in the gas separation chamber. It was found that provision of a gas separation chamber extending back 4 to 5 inches from the anode shoulder, across the inter-electrode gap and extending over the top of the cathode structure, was adequate for 12-inch cathodes.
  • Formula A referred to above is applicable, within the range of electrode inclinations stated.
  • FIGS. 2 and 3 of the accompanying drawings illustrate the operation of a less favourable and more favourable cell configuration, respectively.
  • the numeral 1 indicates the anode having active anode surfaces la
  • 2 indicates the cathodes having active cathode surfaces 2a
  • 8 indicates the electrolyte
  • 8a the upper surface of the electrolyte
  • 10 the inter-electrode space.
  • A indicates regions of severe gas formation and B indicates regions of less severe gas formation.
  • 9 is the gas separation chamber immediately above the cathode 2.
  • the inclination of the active electrode surfaces to the vertical was about 10 and the interelectrode distance (A.C.D.) was 1.5 inches.
  • the current density was 1 amp/cm and in FIG. 3 it was 2 amp/cm?
  • the depth of the quiescent electrolyte above the working cathode surface, within the inter-electrode space was 2 inches; and in FIG. 3 the depth of the quiescent electrolyte above the working cathode surface, within the gas separation chamber. was 4 inches.
  • the width of the upper surface of the electrolyte was 1.5 inches in FIG. 2 and 4 inches in FIG. 3.
  • FIG. 3 illustrates the effect of electrolysis using a cell design and gas separation chamber constructed in accordance with one form of this invention. Operation with improved gas liberation under the conditions shown in FIG. 3 raised the current efficiency to about 90 percent.
  • a feature of the form of the invention shown in FIG. 3, as compared with the cell design shown in FIG. 2, is that the width and depth of the gas separation chamber 9 immediately above the working cathode surface 2a are sufficient to ensure (a) that the gas formed in the inter-electrode space 10 during electrolysis is discharged or liberated to a substantial degree from such space 10 into the gas separation chamber 9, and (b) that said gas is liberated to a substantial degree from the electrolyte in said gas separation chamber 9.
  • the width and/or depth of the gas separation chamber 9 are at least twice the inter-electrode distance (A.C.D.).
  • the above-described cell arrangement substantially reduces the back reaction which would otherwise occur between the gas and the metal in the vicinity of the cathode surface 2a (as indicated in FIG. 2) and thus substantially increases the current efficiency of the cell.
  • FIG. 4 represents a diagrammatic side elevation of a type of multi-electrode cell designed according to the present invention. Overall dimensions of the cells are preferably as indicated in Table I. l designates the graphite anodes with electrolytically active surfaces la inclined at a negative angle of about 10 to the vertical, and provided with recesses 4 to form a gas liberation chamber which is preferably proportioned according to Formula A and which affords an adequate rate of gas evolution from the melt surface 811.
  • cathodes 2 designates the cathodes, which for aluminium production are of graphite and for magnesium production may be hollow fabricated steel structures or plain steel sheets, having cathode surfaces 2a which are at a positive angle of about to the vertical and are substantially parallel to the anode surfaces 1a, and 3 represents the refractory-lined steel shell.
  • 8 designates the electrolyte and 6 the electrical current connections for the anodes. Connections for the cathodes 2 are not shown; these may, if desired, be made directly to the shell 3. It will be understood that in any cell configuration the anode(s) may be adjusted in a vertical or substantially vertical direction for setting or-re-setting of A.C.D.
  • FIG. 5 represents a diagrammatic side elevation of a more compact electrode configuration, namely that employing bipolar electrodes.
  • the connotations of the designating numerals used are not the same as in FIG. 4.
  • l designates the graphite anode, with working surfaces la inclined according to the invention
  • 2 the bipolar electrodes with working surfaces 2a, which electrodes 2 may be monolithic graphite blocks supported at their ends by the insulating walls of the cell.
  • 3 designates the collector cathodes, which may be of steel in the case of magnesium, but of graphite in the case of aluminium cells
  • 3a represents the working surfaces of the cathodes 3.
  • 4 represents the refractory lined outer steel shell and 5 the gas liberation chamber, preferably proportioned according to Formula A.
  • the insulating lower supports 6 for the bipolar electrodes 2 serve as barriers for reducing leakage current.
  • EXAMPLE 1 A run was carried out in a cell having a single inclined anode, and of the general form shown in FIG. 3. The effective electrode area was approximately 1000 cm. Electrolyte composition was 21% MgCl -75% KCl-4%LiCl, and a total cell current of 400 amps was used, at a temperature of 850C.
  • the anode-cathode slope was 9 to the vertical and was within the recommended range for efficient operation.
  • the other parameters were chosen to test some of the less favourable conditions for gas release.
  • the most adverse feature was the use of a melt depth of only 1.5 ins. above the cathode, together with a current density of only 0.36 amp/cm. Under these conditions, considerable back reaction was anticipated to occur because of back circulation of chlorine into the inter-electrode space.
  • EXAMPLE 2 Magnesium A run was carried out using a single anode cell of the general form shown in FIG. 3 and having an effective electrode area of approximately 1000 cm The electrolyte composition was 21% MgCl 75% K Cl and 4% LiCl.
  • the anode/cathode slope was 9 to the vertical and was within the recommended range for efficient operation.
  • the cathode length L was 12 inches, S and D were each 4 inches.
  • the operating temperature was 850C, current density was 0.64 amp/cm and a total cell current of 700 amps was maintained during the 60 minute duration of the run.
  • EXAMPLE 3 Magnesium A second run was carried out in the same cell as in Example 2 using an electrolyte containing 22% MgC1 29% KCl, and 50% LiCl. Operating conditions were chosen to demonstrate one of the optimum combinations of parameters attainable in a cell model.
  • the average current efficiency was 89 percent.
  • an electrolytic cell for use in the electrolytic production of metals in molten halide systems, which comprises a pair of closely spaced substantially parallel planar non-consumable electrodes inclined at an angle of between 7 and 15 degrees to the vertical, an interelectrode spacing for said molten halide system, the cathode surface being inclined at a positive angle to the vertical and the anode surface being inclined at a similar negative angle to the vertical, the inter-electrode spacing being less than two inches, and a gas separation chamber disposed above and communicating with the inter-electrode space into which gas is discharged upwardly from the inter-electrode space, the area of the melt surface of said molten halide system in the gas separation chamber and the depth of the electrolyte in the gas separation chamber being sufficient to permit separation of gas from the electrolyte in the gas separation chamber at substantially the same rate as it is produced in the inter-electrode space, the width of the melt surface in the gas separation chamber being not less than trolyte
  • An electrolytic cell according to claim 1 wherein a pool of molten metal is formed below the electrodes but said pool does not serve as a cathode on which metal is deposited.

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US349472A 1972-04-17 1973-04-09 Electrolytic process for the production of metals in molten halide systems Expired - Lifetime US3909375A (en)

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4055474A (en) * 1975-11-10 1977-10-25 Alcan Research And Development Limited Procedures and apparatus for electrolytic production of metals
US4140594A (en) * 1977-05-17 1979-02-20 Aluminum Company Of America Molten salt bath circulation patterns in electrolysis
US4151061A (en) * 1977-11-15 1979-04-24 Nippon Light Metal Company Limited Aluminum electrolytic cell
DE2751601A1 (de) * 1977-11-18 1979-05-23 Nippon Light Metal Co Abgedichtete elektrolytische zelle
US4334975A (en) * 1979-09-27 1982-06-15 Hiroshi Ishizuka Apparatus for electrolytic production of magnesium metal from its chloride
US4342637A (en) * 1979-07-30 1982-08-03 Metallurgical, Inc. Composite anode for the electrolytic deposition of aluminum
US4405433A (en) * 1981-04-06 1983-09-20 Kaiser Aluminum & Chemical Corporation Aluminum reduction cell electrode
WO1983004271A1 (fr) * 1982-06-03 1983-12-08 Great Lakes Carbon Corporation Composant cathodique pour une cellule de reduction de l'aluminium
US4613414A (en) * 1982-12-30 1986-09-23 Alcan International Limited Method for magnesium production
US4869790A (en) * 1986-10-14 1989-09-26 The British Petroleum Company P.L.C. Metal separation process
US5286359A (en) * 1991-05-20 1994-02-15 Reynolds Metals Company Alumina reduction cell
US6074545A (en) * 1997-02-04 2000-06-13 Cathingots Limited Process for the electrolytic production of metals
US6245201B1 (en) * 1999-08-03 2001-06-12 John S. Rendall Aluminum smelting pot-cell
US20040112757A1 (en) * 2001-02-23 2004-06-17 Ole-Jacob Siljan Method and an electrowinning cell for production of metal
WO2013170299A1 (fr) 2012-05-16 2013-11-21 Lynas Services Pty Ltd Cellule électrolytique pour la production de métaux des terres rares
US10415147B2 (en) * 2016-03-25 2019-09-17 Elysis Limited Partnership Electrode configurations for electrolytic cells and related methods

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6017037B2 (ja) * 1980-12-11 1985-04-30 博 石塚 溶融塩電解用中間電極体及びこれを用いた塩化マグネシウム電解装置
CN111501069A (zh) * 2020-06-02 2020-08-07 株洲科能新材料有限责任公司 一种粗镓的熔盐电解提纯方法

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US1545383A (en) * 1922-02-18 1925-07-07 Ashcroft Edgar Arthur Apparatus for electrolyzing fused salts
US3028324A (en) * 1957-05-01 1962-04-03 British Aluminium Co Ltd Producing or refining aluminum
US3067124A (en) * 1958-07-24 1962-12-04 Montedison Spa Furnace for fused-bath electrolysis, particularly for aluminum production from alo
US3400061A (en) * 1963-11-21 1968-09-03 Kaiser Aluminium Chem Corp Electrolytic cell for production of aluminum and method of making the same
US3755099A (en) * 1971-09-08 1973-08-28 Aluminum Co Of America Light metal production

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US3330756A (en) * 1951-05-04 1967-07-11 British Aluminum Company Ltd Current conducting elements
US3202600A (en) * 1951-05-04 1965-08-24 British Aluminium Co Ltd Current conducting element for aluminum reduction cells
CH441776A (de) * 1966-05-17 1967-08-15 Marincek Borut Verfahren zur Herstellung von Metallen durch Schmelzflusselektrolyse von Oxiden

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1545383A (en) * 1922-02-18 1925-07-07 Ashcroft Edgar Arthur Apparatus for electrolyzing fused salts
US3028324A (en) * 1957-05-01 1962-04-03 British Aluminium Co Ltd Producing or refining aluminum
US3067124A (en) * 1958-07-24 1962-12-04 Montedison Spa Furnace for fused-bath electrolysis, particularly for aluminum production from alo
US3400061A (en) * 1963-11-21 1968-09-03 Kaiser Aluminium Chem Corp Electrolytic cell for production of aluminum and method of making the same
US3755099A (en) * 1971-09-08 1973-08-28 Aluminum Co Of America Light metal production

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4055474A (en) * 1975-11-10 1977-10-25 Alcan Research And Development Limited Procedures and apparatus for electrolytic production of metals
US4140594A (en) * 1977-05-17 1979-02-20 Aluminum Company Of America Molten salt bath circulation patterns in electrolysis
US4151061A (en) * 1977-11-15 1979-04-24 Nippon Light Metal Company Limited Aluminum electrolytic cell
DE2751601A1 (de) * 1977-11-18 1979-05-23 Nippon Light Metal Co Abgedichtete elektrolytische zelle
US4342637A (en) * 1979-07-30 1982-08-03 Metallurgical, Inc. Composite anode for the electrolytic deposition of aluminum
US4334975A (en) * 1979-09-27 1982-06-15 Hiroshi Ishizuka Apparatus for electrolytic production of magnesium metal from its chloride
US4405433A (en) * 1981-04-06 1983-09-20 Kaiser Aluminum & Chemical Corporation Aluminum reduction cell electrode
WO1983004271A1 (fr) * 1982-06-03 1983-12-08 Great Lakes Carbon Corporation Composant cathodique pour une cellule de reduction de l'aluminium
US4526669A (en) * 1982-06-03 1985-07-02 Great Lakes Carbon Corporation Cathodic component for aluminum reduction cell
US4613414A (en) * 1982-12-30 1986-09-23 Alcan International Limited Method for magnesium production
US4869790A (en) * 1986-10-14 1989-09-26 The British Petroleum Company P.L.C. Metal separation process
US5286359A (en) * 1991-05-20 1994-02-15 Reynolds Metals Company Alumina reduction cell
US6074545A (en) * 1997-02-04 2000-06-13 Cathingots Limited Process for the electrolytic production of metals
US6245201B1 (en) * 1999-08-03 2001-06-12 John S. Rendall Aluminum smelting pot-cell
US20040112757A1 (en) * 2001-02-23 2004-06-17 Ole-Jacob Siljan Method and an electrowinning cell for production of metal
US7144483B2 (en) * 2001-02-23 2006-12-05 Norsk Hydro Asa Method and an electrowinning cell for production of metal
WO2013170299A1 (fr) 2012-05-16 2013-11-21 Lynas Services Pty Ltd Cellule électrolytique pour la production de métaux des terres rares
KR20150013316A (ko) * 2012-05-16 2015-02-04 라이나스 서비시즈 피티와이 엘티디 희토류 금속 생산용 전해셀
CN104520476A (zh) * 2012-05-16 2015-04-15 莱纳服务有限公司 用于稀土金属的生产的电解池
EP2850226A4 (fr) * 2012-05-16 2015-09-02 Lynas Services Pty Ltd Cellule électrolytique pour la production de métaux des terres rares
CN104520476B (zh) * 2012-05-16 2017-12-12 莱纳服务有限公司 用于稀土金属的生产的电解池
US10415147B2 (en) * 2016-03-25 2019-09-17 Elysis Limited Partnership Electrode configurations for electrolytic cells and related methods
US11060199B2 (en) 2016-03-25 2021-07-13 Elysis Limited Partnership Electrode configurations for electrolytic cells and related methods
US11585003B2 (en) 2016-03-25 2023-02-21 Elysis Limited Partnership Electrode configurations for electrolytic cells and related methods

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DE2318857B2 (de) 1976-04-08
BR7302803D0 (pt) 1974-07-18
GB1412848A (en) 1975-11-05
JPS4924821A (fr) 1974-03-05
JPS5418208B2 (fr) 1979-07-05
DE2318857A1 (de) 1973-10-25
CA1044175A (fr) 1978-12-12

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