EP3033443A2 - Molten salt electrolysis apparatus and process - Google Patents
Molten salt electrolysis apparatus and processInfo
- Publication number
- EP3033443A2 EP3033443A2 EP14836690.9A EP14836690A EP3033443A2 EP 3033443 A2 EP3033443 A2 EP 3033443A2 EP 14836690 A EP14836690 A EP 14836690A EP 3033443 A2 EP3033443 A2 EP 3033443A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- metal
- cell
- anode
- alkaline earth
- anodes
- 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
Links
Classifications
-
- 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
- C25C3/04—Electrolytic production, recovery or refining of metals by electrolysis of melts of magnesium
-
- 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
-
- 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
-
- 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
- C25C7/02—Electrodes; Connections thereof
- C25C7/025—Electrodes; Connections thereof used in cells for the electrolysis of melts
Definitions
- the invention reiates to alkali and alkaline earth metal production through electrolysis of molten chloride salts thereof.
- alkali metals such as metallic lithium and sodium and an alkaline earth metal such a magnesium
- an alkaline earth metal such a magnesium
- electricity ca 36 kWh kg Li, 11 kWh kg sodium and 11 kWh/kg magnesium
- the overall energy efficiency of monopolar electrolysis cells currently in use is only about 40% to 50%.
- the current electrolysis cells used commercially for alkali metal production use cylindrical anodes which results in a low space time yield per cell of such cells.
- a further consequence of using cylindrical anodes is that when the diameter of the anode is increased in order to increase the effective surface area of the anode available for electrolysis, the cross sectional area of the anode increases with the square of the diameter of the anode while the periphery increases only linearly. This is an important consideration since graphite, which is used as anode is a very good conductor of heat but not such a good conductor of electricity. In order to carry the necessary current without causing excessive eiect icai potential losses, the anodes must have a relatively large cross sectional area. Unfortunately this results In a lot of heat loss through the anode.
- the cell consists basically of up to 8 cylindrical graphite anodes that protrude through the bottom of the cell body into the cell.
- Around each anode is a cylindrically shaped diaphragm made of steel mesh, a perforated plate or a slotted steel plate.
- a cyiindricaiiy shaped steel cathode around each diaphragm.
- the steel cathodes are normally connected to the power source of the cell through connections protruding through the side walls of the cell.
- annular metal collector made of steel that has the function to collect the bulk of the molten metal product that is produced at the cathodes and that floats upwards into the collector from where it is taken out of the cell.
- the diaphragms are normally connected and supported by the metal collector.
- a chlorine collector or hood made of a high nickel alloy or of refractory lined steel. All the chlorine produced at the anodes is collected in this hood before it flows out of the cell.
- a second prior art closest to the invention is in the field of magnesium electrowinning i.e. the cell developed by IG Kon industry in Germany (Magnesium Encyclopedia downloaded 29 May 2013) or the diaphragm-type magnesium electrolysis cell (Electrolytic Production of Magnesium, 1972, p251, Translated from Russian by J. Schmorak).
- the brick-lined cell is divided into four to six compartments by semi-submerged refractory partition wails labelled semi walls.
- Three to five water- or air-cooled graphite anode plates are installed and tightly sealed in the refractory cover of the cell.
- the semi wails on each side of the anodes separate the magnesium metal and the chlorine gas.
- Steel cat ode plates are installed through the cell cover or through the sidewaiis in the cathode compartments.
- the sequence of electrodes in the cells is: cathode, anode, cathode, cathode, anode, cathode, cathode anode etc.
- the design of the cell is such that the flow of electrolyte caused by the chlorine bubbles produced at the anodes is upwards along the anode face, over the cathode into the space below the magnesium collection zone above the zone between the cathodes, downward behind the cathodes and then finally beiow the cathodes back into the space between a cathode and anode.
- the design may result in the flow of electrolyte from the space between the electrodes over or through the cathode into a metal collection zone. Small chlorine bubbles may be entrained in this flow and end in the metal collection zone of the cell which is undesirable.
- an apparatus for the production of metallic alkali metals, , or alkaline earth metals, M ae from the molten salts thereof including at least an electrochemical cell with planar anodes and cathodes installed in the following sequence: (a-c-a)terrorism to produce alkali metal or alkaline earth metals electrolytically from the respective chloride salts according to the following reactions:
- (a ⁇ c-a) n represents the arrangement wherein the sequence of anodes and cathodes of anode-cathode-anode are repeated n number of times, as required anode, cathode, anode, anode, cathode, anode, anode, cathode, anode, and so on.
- the alkali metal, M is typically lithium or sodium.
- the alkaline earth metal ae is typically magnesium.
- Diaphragms which may be made of steel mesh, perforated plate, or slotted plates may be installed between each pair of opposed anodes and cathodes.
- a metal collector assembly may be installed above each cathode to collect molten alkali metal or alkaline earth metal that floats to the top of the electrolyte from where t is withdrawn from the cell.
- the metal collector assembly may be electrically isolated from both the anodes and cathode of an anode-cathode-anode set while the metai collector assembly and the diaphragms are electrically connected to each other.
- Both the metal collector assembly and the diaphragms may be cathodicaily protected by molten alkali metal or alkaline earth metal collected in the assembly, for example, by molten Li, Na and/or g.
- chlorine gas produced at the anode or anodes may cause circulation of a molten electrolyte used in the cell upwards along the face of the anode surface in the spaces between each anode and opposing cathode, over the active anode body, then downwards behind the anode body before turning around to flow upwards again over the face of the anode (or anodes).
- Chlorine produced at the anodes may disengage from the circuiating electrolyte at the top of the molten electrolyte above the active electrolysis zones between the anodes and cathodes.
- the chlorine thus produced in the head space above the electrolyte is withdrawn from the eel! and may be used for various purposes.
- a particular configuration of the apparatus is to instaii the cathodes through the bottom of the cell and the anodes through the side or opposing sides of the cell.
- the electrochemical cell may be lined with chlorine resistant refractory or be made of metal, provided that the metal exposed to chlorine gas in the head space of the cell is sufficiently resistant to attack by chlorine, e.g. nickel or a high nickel containing alloy.
- Suitable feed means may be installed to feed the salt to be eiectrolyzed into the electrochemical cell and suitable withdrawal means may be provided to withdraw the alkali or alkaline earth metal and chlorine produced in the cell from the cell.
- suitable heaters may be provided to preheat the electrochemical cell to melt the electrolyte inventory in the cell before commencing electrolysis.
- a suitable direct current power source may be supplied to provide the electrical potential and current required for the reaction.
- a process for the production of alkali metals and alkaline earth metals from the molten salts thereof by electrolysis said method including - arranging three or more electrodes in an (a-c-a) n arrangement in an electrolysis cell;
- the process may include maintaining the metallic alkali metal or alkaline earth metal under an inert atmosphere during extraction thereof.
- the molten alkali metal or alkaline earth metal salt may be a sodium, lithium or a magnesium salt.
- the sodium salt may be NaCi in which case the electrolyte may contain NaCi, CaCfe, and BaCi 2 allowing the cell to be operated at temperatures from about 550 to 700°C.
- the lithium salt may be LiC! in which case the electrolyte may consist predominantly of a mixture of KCI and LiCi allowing the cell to be operated at temperatures from about 400 to 500°C.
- the magnesium salt may be gCl2 in which case the electrolyte may consist predominantly of a mixture of KCI, NaC!, CaCfc. BaC! 2 and MgCfe allowing the cell to be operated at temperatures from about 660 to 800°C.
- the alkali metal or alkaline earth metal may be recovered at a temperature above its melting point, in liquid form.
- the alkali metal or alkaline earth metal may be recovered at a temperature below the melting point of the alkali metal or alkaline earth metal salt from which the alkali metal or alkaline earth metal is recovered.
- chlorine produced at the anodes may disengage from the circulating electrolyte at the top of the molten electrolyte above the active electrolysis zones between the anodes and cathodes.
- the chlorine thus produced in the head space above the electrolyte may be withdrawn from the cell and may be used for various purposes.
- FIG. 1 shows a vertical cross sectional schematic through the first example of an operating electrochemical cell of the invention where the anodes protrude through two opposing sides of the cell and the cathodes of the cell protrude through the bottom of the cell.
- Figure 2 shows a horizontal section schematic viewed from the top of the construction of the electrochemical cell shown in Figure 1.
- the cell (1) may have a shell (24) that may be constructed from steel.
- the cell may have a removable lid (11).
- the cell may have a refractory lining (10) that serves to protect the shell of the cell against the hot molten electrolyte inside the cell, to limit thermally Induced stresses caused by temperature increases of the shell, and to limit heat losses from the cell.
- Four planar anodes (19) and two planar cathodes (23) of the cell (1) are shown in Figure 1. The anodes and cathodes are arranged in the following order: anode-cathode-anode-anode-cathode-anode, or (a-c-a) 2 .
- Each cathode is separated from the opposing pair of anodes by a diaphragm (20) and a metal collector (18) is positioned above each cathode to collect the molten alkali metal or alkaline earth metal (17) that is produced on the surfaces of the cathode.
- the molten alkali metal or alkaline earth metal (17) has a lower density than the electrolyte ( 5) and therefore floats into the metal collector (18).
- the piping to remove the molten metal from the metal collector is not shown in Figure 1.
- the alkali metal or alkaline earth metal salt feed (14) to the cell is introduced into a feed vessel (13) where it is dissolved in electrolyte that is circulated from and back to the cell via hot pipe lines (21) between the feed vessel (13) and the cell.
- the cathodes (23) protrude through the shell (24) and refractory lining (10) of the cell through the bottom of the cell.
- the mounting (22) of each cathode serves to position the cathode, to insulate it from the shell (24) and also to cool the cathode (23) as dictated by the thermal design requirements of the cell. Details of the mounting are not shown, since means to achieve the mentioned objectives are well-known in the field.
- Chlorine is produced on the surfaces of the anodes (19) and rises as gas bubbles (16) towards the surface of the electrolyte bath where it disengages from the electrolyte and exits the cell through an exit port ( 2).
- the alkaline earth metal is Mg.
- the gas bubbles (16) form predominantly on the vertical surfaces of the anodes (19) on the sides opposing the vertical surfaces of the cathodes (23).
- the bulk density of the electroiyte bubbie mixture in the spaces between the anodes and the diaphragm (20) is lower than the bulk density of the electrolyte in the space (25) between two opposing anodes and also to that of the electrolyte in the space between the anodes and the inner surface of the refractory lining (10).
- This difference in density causes the electrolyte to flow upwards in the space between the anode (19) surfaces and the diaphragms and downwards in the latter spaces as indicated by the broken arrows.
- the density of the electrolyte bubble mixture in the space between the anodes (19) and diaphragms (20) is lower than that of the electrolyte in the space between the diaphragms (20) and the cathodes (23).
- Some electrolyte therefore flows through each diaphragm in the upper part of the diaphragm towards the cathode, then downwards and lastly back through the diaphragm (20) in the lower part of the diaphragm towards the anode (19) opposite the specific diaphragm (20).
- Such flow is essential to replenish the alkali metal or alkaline earth metal cations that are reduced to metal on the cathode (23) surfaces but if such flow is too high, chlorine bubbles may pass through the diaphragm (20) and eventually rise into the metal collectors (18) where it reacts undesirably with the collected molten metal.
- the diaphragms By appropriate design of the diaphragms, the spacing between the different electrodes and diaphragms and the spacing between the electrodes and the inner surface of the cell refractory lining (10), the electrolyte flow around the anodes ( 9) are significantly increased relative to the circulating electrolyte flow through the diaphragms (20).
- FIG 2 it is shown how four units of anode-cathode-anode assemblies can be installed in a single cell with two assemblies on each side of the cell when the anodes (1 ) protrude through two opposing side wails of the cell and the cathodes (23) protrude through the bottom of the cell. Also shown are anode mountings (26) that similarly to the cathode mountings (22) shown in Figure 1 serve to position the anodes, to insulate the anodes from the shell (24) and to cool the anodes. Details of the anode mountings (26) are not shown.
- Figure 3 and Figure 4 iiiustrate diagrammatically the design of a second example of a cell designed in accordance with the invention where the anodes protrude through the bottom and the cathodes through a side wall of the cell.
- Figure 3 shows a vertical cross sectional schematic through an operating electrochemical DCi
- Figure 4 shows a vertical cross section through the construction and one of the anodes of the cell at a 90° angle relative to the cross section shown in Figure 3.
- slots (27) or other suitable flow channels are provided in the anodes.
- the circulation is caused by the same density differences as described in the first example.
- FIG. 4 The installation of the anodes (19) through the bottom of the cell and the cathodes (23) through a side wall of the cell is illustrated in Figure 4.
- the slots (27) through the anodes are also shown and a diaphragm (20) behind the anode.
- a metal collector (18) is positioned on top of the cathode (23) and the shown diaphragm (20) and it may typically be sloped to direct the flow of molten metal towards the top of the collector from where it is withdrawn through pipe work that is not shown.
- circulation of the electrolyte from the anode surface to the metal collection zone in the current planar electrode arrangements causes mixing of and back reaction of such chlorine with the molten metai in the metal collection zone.
- LiCi Apart from a reduction in efficiency by this, back reaction of C1 ⁇ 2 with Li, Na or Mg causes the formation of LiCi.
- NaCi or MgCfe in the metai collection zone LiCi and NaCI in particular have melting points that are substantially higher than the melting points of the electrolytes used with the result that solid salt is deposited in the metai collection zone that can cause blockages of the molten metal withdrawal lines.
- gCb also has a higher melting point than the electrolyte, but the difference is substantially ess. Many Mg cells actually operate above the melting point of MgCfe that is ca 714°C.
- the electrochemical cell design of the invention causes a large molten electrolyte flow pattern upwards along the face of the anode surface, over the active anode body, then downwards behind the anode body before turning around to flow upwards again over the face of the anode (or anodes).
- planar anodes and cathodes are used which enhances up-scaling of the cell and also increases the packing density of electrodes in the cell.
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
ZA201306171 | 2013-08-16 | ||
PCT/ZA2014/000038 WO2015024030A2 (en) | 2013-08-16 | 2014-08-15 | Molten salt electrolysis apparatus and process |
Publications (2)
Publication Number | Publication Date |
---|---|
EP3033443A2 true EP3033443A2 (en) | 2016-06-22 |
EP3033443B1 EP3033443B1 (en) | 2018-03-28 |
Family
ID=52468831
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP14836690.9A Not-in-force EP3033443B1 (en) | 2013-08-16 | 2014-08-15 | Molten salt electrolysis apparatus and process |
Country Status (3)
Country | Link |
---|---|
US (1) | US20160215405A1 (en) |
EP (1) | EP3033443B1 (en) |
WO (1) | WO2015024030A2 (en) |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FI129211B (en) | 2018-09-11 | 2021-09-30 | Tercosys Oy | Energy management method and arrangement |
DE102022000153A1 (en) | 2022-01-17 | 2023-07-20 | KS iPR UG (haftungsbeschränkt) | ELECTROLYTE MEMBRANE FOR THE SEPARATION OF WATER VAPOR INTO HYDROGEN AND OXYGEN USING ELECTRIC ENERGY AND/OR GENERATION OF ELECTRICAL ENERGY USING HYDROGEN AND OXYGEN BY A LITHIATED IRON OXIDE - IRON REDOX REACTION IN A LIQUID CARBONATE SALT |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1501756A (en) | 1922-08-18 | 1924-07-15 | Roessler & Hasslacher Chemical | Electrolytic process and cell |
DE1558726B2 (en) | 1951-01-28 | 1973-09-06 | ELECTROLYZING CELL | |
US3544444A (en) | 1967-05-19 | 1970-12-01 | Du Pont | Fused salt electrolysis cell having anode with tapered well therein |
US5904821A (en) | 1997-07-25 | 1999-05-18 | E. I. Du Pont De Nemours And Company | Fused chloride salt electrolysis cell |
US6497807B1 (en) * | 1998-02-11 | 2002-12-24 | Northwest Aluminum Technologies | Electrolyte treatment for aluminum reduction |
US6827828B2 (en) * | 2001-03-29 | 2004-12-07 | Honeywell International Inc. | Mixed metal materials |
CN101709485B (en) * | 2009-12-18 | 2012-07-04 | 中国铝业股份有限公司 | Aluminum electrolytic cell for producing virgin aluminum by inert anode |
-
2014
- 2014-08-15 EP EP14836690.9A patent/EP3033443B1/en not_active Not-in-force
- 2014-08-15 WO PCT/ZA2014/000038 patent/WO2015024030A2/en active Application Filing
- 2014-08-15 US US14/911,135 patent/US20160215405A1/en not_active Abandoned
Also Published As
Publication number | Publication date |
---|---|
WO2015024030A3 (en) | 2015-07-23 |
EP3033443B1 (en) | 2018-03-28 |
WO2015024030A2 (en) | 2015-02-19 |
US20160215405A1 (en) | 2016-07-28 |
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