EP0069681B1 - Zelle zur elektrolytischen Herstellung eines Metalls aus seinem Halogenid - Google Patents
Zelle zur elektrolytischen Herstellung eines Metalls aus seinem Halogenid Download PDFInfo
- Publication number
- EP0069681B1 EP0069681B1 EP82420065A EP82420065A EP0069681B1 EP 0069681 B1 EP0069681 B1 EP 0069681B1 EP 82420065 A EP82420065 A EP 82420065A EP 82420065 A EP82420065 A EP 82420065A EP 0069681 B1 EP0069681 B1 EP 0069681B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- cell according
- electrolytic production
- polar
- production cell
- elements
- 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
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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
- C25C3/06—Electrolytic production, recovery or refining of metals by electrolysis of melts of aluminium
- C25C3/08—Cell construction, e.g. bottoms, walls, cathodes
-
- 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 relates to a cell for the electrolytic production of metals by electrolysis in a bath of molten salts, of their anhydrous halide, and, more particularly, of the electrolytic production of aluminum from the corresponding anhydrous chloride.
- a person skilled in the art has long been inspired by the process of igneous electrolysis of alumina in a molten mixture of sodium and aluminum fluorides, in order to design devices intended for the igneous electrolysis of chloride of anhydrous alumimium in a bath of molten salts.
- the undissolved metal oxides are at the origin of a gradual accumulation, on the graphite cathodes, of a viscous layer of finely divided solids, of liquid components of the bath and of droplets of molten aluminum, which impede access to the cathodes of the electrolysis bath and which can lead to disturbances of the normal cathode mechanism, that is to say the reduction of the cations containing the metal to be produced at various degrees of oxidation.
- the aluminum chloride present in the viscous layer then consumed by electrolysis, is more and more difficult to renew, and, consequently, the other chlorides constituting the bath of molten salts can be electrolysed, resulting in loss. efficiency of the electrical energy used and pollution of the metal.
- the chlorides constituting the bath of molten salts such as the alkali (for example sodium and / or potassium and / or lithium) and alkaline earth (for example magnesium and / or calcium and / or barium), are partially electrolyzed by lack of renewal of the aluminum chloride near the cathode, giving the corresponding metals which are inserted, under cathodic potential, in the graphite of the electrodes and cause their disintegration and their crumbling.
- This premature wear of the cathodes causes the introduction of carbon particles into the bath, which contribute to the formation of sludge at the cathode, and, moreover, cause a reduction in yield.
- a cell of the aforementioned type with bipolar electrodes is described in French patent 2,152,814 which comprises, stacked horizontally, and from top to bottom, an anode, at least one intermediate bipolar electrode and a cathode, superimposed and regularly spaced by means of insulating refractory spacers, thus creating substantially horizontal spaces between electrodes in order to carry out the electrolysis of aluminum chloride in a bath of molten salts in each interpolar space, which leads to the release of chlorine on each anode surface and to the deposition of aluminum on each cathode surface.
- the chlorine produced plays the role of a pressure pump which, by suitable passages, leads to the surface the most light, and promotes decantation towards the bottom of the cell of the aluminum obtained.
- each bipolar electrode is provided with an absolutely flat cathode surface and an anode surface hollowed out with transverse channels.
- each anode surface has several of these channels which extend transversely to the lateral edge of each electrode on the side of the passage reserved for the return of the bath and for the rise of the gas. These channels are intended to pervert away the chlorine, released from the interpolar space, from the aluminum deposited on the cathode surface to limit the rechlorination of the metal produced.
- the anode surfaces can comprise transverse channels which promote the flow of chlorine out of the inter-electrode space towards a gas rise zone formed in the redian part of the cell between the stacks d 'electrodes, this area widening from the bottom to the top of the cell.
- the existence of channels on the anode surface leading to a zone of rising gases, formed in the middle part of the cell between the stacks of electrodes is intended to quickly remove the chlorine released from the interpolar space, but above all, to keep it away from the aluminum deposited on the cathode surface to limit its rechlorination.
- Such electrolysis cells are also the seat of poor thermal balances due to the disproportion between the energy power dissipated at the center of said cells and the radiating external surface.
- the cell for the electrolytic production of a metal by electrolysis of its anhydrous halide in a bath of molten salts comprises an external envelope of apparently parallelepipedic shape having means of cooling, inlet and outlet openings for the fluids liquids and gases, as well as electrical power supply means, envelope inside which there is, in its lower part, a receptacle zone for collecting the metal produced, in its middle part, at least one series of electrodes arranged in piles, each pile comprising in the vertical direction and from top to bottom a current supply electrode, intermediate multipole elementsp and a current output electrode defining between them regular interpolar spaces, and, in its upper part , a gas collection area, said cell being characterized in that the multipole elements are assembled in a vertical stack and that the s interpolar spaces are substantially vertical.
- Intermediate multipolar elements are composed of stacked prismatic elements whose cross section generally has a shape resembling the letter Y.
- Each prismatic multipolar element has an upper trough-shaped part playing the role of cathode surface, defined by the two upper branches of the Y, the walls of which have a constant thickness, and a lower part playing the role of lower surface of the Y, whose thickness is at least equal to the thickness of the walls of the trough, but which is preferably equal to twice the thickness of each of the upper branches.
- each upper branch of the straight section of the trough that is to say the Y-shaped section, can deviate from the axis of symmetry of the two upper branches, so as to avoid disturbances that could occur in this area between the multipole elements.
- the thickness of the walls of the trough of each multipole element is generally between 10 and 100 millimeters, and preferably between 25 and 50 millimeters.
- the bottom of the trough, formed by the upper branches of the Y-shaped section, can be provided with a longitudinal channel formed by a groove which promotes the collection and evacuation of the metal obtained during electrolysis.
- the multipolar element is generally obtained by spinning a carbonaceous paste, followed by cooking, and finally, graphitization according to well known methods.
- the cathode part of the multipolar elements can be coated with a layer based on zirconium diboride or titanium diboride.
- each multipole element is generally at least equal to 200 millimeters and may preferably be between 300 and 500 millimeters. This height is neither limited nor critical with regard to the electrolysis operation. It is generally defined by the user for each particular case and does not have, by its structure, any limitation.
- each multipole element is defined by the dimensional characteristics of the cell itself.
- the prismatic multipolar elements are stacked one above the other, and wedged together by means of insulating refractory parts and resistant to the aggressive action of the medium.
- the upper element, brought from the current, is constituted by a prismatic piece preferably deprived of a trough, the cross section of which can be cruciform, in T or in I, or even practically formed of the only lower branch of the section in Y.
- the lower element, current output, is a prismatic piece whose cross section is close to the letter H, the letter M or the letter N.
- the various prismatic elements can be stacked horizontally or even very slightly inclined depending on the slope of the element resting on the bottom of the cell. In the latter case, the flow of liquid metal is then favored.
- the lower end of the ventral edge of the multipolar element can be provided with a device for guiding the liquid metal net, for example of the 'pouring spout' type. best channeling its flow.
- the stacking of the multipolar elements makes it possible, by the interposition of the wedging pieces, to ensure a regular distance between the elements and to create homogeneous interpolar zones ensuring good recirculation of the electrolysis bath.
- the lower element is immersed in at least one liquid metal net in contact with the current outlet device.
- the upper element is connected to the electrical conductors by means of known means such as, for example, the sealing of graphite parts, of copper or steel bars.
- the adjacent stacks thus created are regularly positioned, both with respect to each other and with respect to the walls of the cell, thanks to the pieces of wedging shapes, and, possibly, to other shaped pieces of refractory, insulating materials. , as well as thanks to horizontal or sloping grooves made in the bottom of the cell.
- the electrolysis bath previously enriched in metallic chloride, then purified, is introduced into the cell through orifices located in its lower part, while the excess bath depleted by the electrolysis operation is evacuated by overflow into its upper part or by siphon.
- the recirculation of the bath in the interpolar spaces is ensured by the mechanical drive caused by the release of chlorine gas, mainly along the side walls.
- the internal surface of the cover (4) which is directly exposed to the aggressive vapors of the molten salt bath and to the gaseous effluents resulting from the electrolysis, is made of a suitable resistant material such as alloys containing nickel, chromium, iron, copper, molybdenum, and, optionally, coated with protective ceramics and / or provided with cooling means.
- the interior of the electrolysis cell comprises, in its lower part, a zone (12) collecting the liquid metal produced, in its middle part, an electrolysis zone (13) filled with the bath of molten salts enriched in metal chloride , finally, in its upper part, a zone (14) for collecting the gaseous effluents with a view to their evacuation by (11).
- a first opening (10) extending through the cover in the upper (14), middle (13) and lower (12) zones allows the insertion of a liquid metal evacuation tube.
- Another opening (8) constitutes the means of entry of the bath enriched in metallic chloride, while the opening (9) is used for the evacuation of the depleted bath, and the opening (11) constitutes a means of exit of the effluents gaseous.
- each stack (15) comprises a current supply electrode (16) provided with a supply bar (17) embedded in said electrode and connected to the current supply (7) passing through the cover (4), multipolar intermediate elements (18), a current output electrode (19) fitting, by grooves (20) in the bottom (21) of the tank, in which current output bars (22) can be embedded .
- the intermediate multipole elements (18) create between them interpolar spaces (23), regular and substantially vertical.
- said cell comprises the casing (1) of refractory steel, provided with cooling fins (2), internally lined with the resistant coating (3) to the action of the bath of molten salts and of chlorine, as well as the orifices (7) for the current leads, (8) for the introduction of the bath enriched in metallic chloride, (9) for the evacuation of the bath depleted by electrolysis in this chloride, (10) for the evacuation of the liquid metal and (11) for the exit of the gaseous effluents.
- Said cell also comprises ten vertical stacks (15) comprising the aforementioned multipolar electrodes.
- the current supply electrode (16) consisting of a prismatic piece of graphite, the cross section of which is formed from the lower branch of the letter Y, is also provided with a current supply bar (17 ) embedded in the mass and connected to the power supply (7) not shown.
- Each intermediate multipole element (18) has a trough-shaped upper part (24) defined by the two upper branches (25) and (26) of the Y, and a lower part (27) called the ventral edge, defined by the lower branch of the Y whose thickness is at least equal to that of the walls (25) and (26).
- the bottom of the trough (24) is provided with a longitudinal channel (28), constituted by a groove favoring the collection and the evacuation of the metal obtained by electrolysis.
- the current output electrode (19) is also a prismatic piece, the cross section of which recalls the man of the letter H, the lower branches (29) and (30) of which are nested in the grooves (20) of the sole (21 in which the current output bar (22) is embedded.
- the various prismatic elements constituting the stack ensure, thanks to the interposition of wedging pieces of insulating refractory (31), a regular distance between these elements by creating interpolar zones (23) also called interpolar spaces , ensuring good recirculation of the electrolysis bath, favorable recovery of the molten metal, and excellent evacuation of gaseous effluents between the walls (25), (26) of the trough and (27) of the ventral edge.
- the multipolar elements are assembled in a vertical stack and vertical interpolar spaces, thus preventing the encounter between the molten metal flowing towards the bottom of the tank and the gaseous effluents migrating towards the upper part of said cell.
- each stack comprises an electrode (16) for supplying the current, then intermediate multipole elements (18) and an electrode (19) which allows the output of the current.
- the current supply electrode (16) consisting of a prismatic graphite piece, is provided with a current supply bar (17) connected to the current supply (not shown).
- Each intermediate multipole element (18), formed of a prismatic piece of graphite, has an upper part (24) in the shape of a trough, defined by the walls (25) and (26) and a lower part (27), edge ventral.
- the bottom of the trough (24) is provided with a longitudinal channel (28) constituted by a groove promoting collection and evacuation of the metal obtained during the electrolysis of metal chloride.
- the current output electrode (19) consisting of a prismatic piece of graphite, has two lower walls (29) and (30) which fit into inclined grooves (20) of the sole (21) of the cell.
- the electrode (19) is connected to the output terminal (34) of the current via the liquid metal located in the collector (35) at the bottom of the tank, in which the lower ends of the evacuation tube are immersed. (10) of the molten metal and of the current output terminal (34), protected by their sheath (36) and (37) in insulating refractories.
- the various prismatic elements constituting a stack are kept at regular distance from each other by the interposition of wedging pieces (31) in insulating refractory, creating the interpolar spaces (23).
- the various prismatic elements (16), (18) and (19) have a slight slope promoting the flow of the metal through the longitudinal channels (28).
- these various prismatic elements - (16), (18) and (19) of a stack are offset longitudinally with respect to each other as shown by the intermediate elements (38), (39) and (40) by example, in such a way that the threads of liquid metal escaping from the trough (24) of each of the prismatic elements via the longitudinal channel (28) cannot be in contact with each other, thus preventing the creation of short circuits between the various prismatic elements of the same stack.
- ventral edge (27) is provided with a device (33) for guiding the thread of liquid metal, of the pouring spout type, best channeling the flow of said metal.
- the bath of molten salts has not been shown in the case of FIG. 5, to allow a better perception and understanding of the internal structure of the cell according to the invention.
- the level of the electrolysis bath in said cell can vary during the operation, but must bathe all the interpolar spaces.
- the molten metal placed on the cathode surfaces flows into the trough (24) of each interpolar space (23) by the longitudinal evacuation channel (28), falls in the liquid metal zone (12) and is collected in the liquid metal collector (35) from which the metal is discharged via the sump (10).
- the current output can also be done through the output terminal (34) which plunges into the liquid metal located in the collector (35).
- the level of the bath of molten salts inside the cell being kept practically constant, the tank exhausted in electrolysed metal chloride is discharged through the orifice (9), while the bath enriched in metal chloride to be electrolyzed is introduced. via the power supply (8) (not visible).
- Example 1 (according to Figures 1 and 5):
- An anhydrous aluminum chloride electrolysis cell was produced according to the invention, consisting of a casing (1) of refractory steel, provided with cooling fins (2) and internally lined with a coating (3). resistant to the action of chlorine and molten salt baths based on alkaline chloroaluminates.
- This coating consisted of a stack of bricks made of silicon carbonitrides with crossed joints, maintained by a grout based on silicon nitride.
- each intermediate multipole element was ensured by nitride shims of silicon, a material resistant to environmental corrosion, thus ensuring a distance between each multipolar intermediate element equal to 1 cm in the substantially vertical part.
- the bottom of the trough (24), a little further from the ventral edge (27), defined by the walls (25) and (26) was provided with a longitudinal channel (28) 2 cm wide and 3 centimeters high.
- the current supply electrode (16) was itself connected to the electrical supply circuit via a current supply bar (17).
- the electrode allowing the current output (19) was in contact with the liquid metal.
- the current outlet was effected by a steel bar sealed in the carbon sole.
- the aluminum chloride electrolysis bath was composed, at the inlet of the tank, of 18.8% of LiCl, 28.2% of NaCl and 53% of AICI 3 by weight.
- the bath was maintained at the temperature of 720 ° C ⁇ 10 ° C.
- the supply of AICI 3 was effected by the supply orifice (8), while the depleted bath was evacuated by overflow using the orifice (9).
- the feed rate in enriched bath was 62 kg / h and was adjusted by measuring the conductivity of the bath using a conductimetric cell and a level detector (not shown).
- the aluminum produced was extracted by suction inside the sump (10) formed in an insulating refractory tube.
- the chlorine was discharged with the other gaseous effluents via the tube (11).
- An aluminum chloride electrolysis cell according to the invention was produced, comprising, as in Example 1, the same multipolar intermediate elements, but of which the cathode part (internal wall of the trough) had been covered with '' a mixture composed of 60% by weight of zirconium diboride and 40% by weight of high temperature coal tar, then calcined at 1200 ° C.
- the feed rate in the enriched bath was 248 kg / h. Its introduction was regulated according to the response of a conductimetric cell and a level detector (not shown).
- the current output was carried out using a steel bar sealed in the sole.
- An aluminum chloride electrolysis cell was produced according to the invention, retaining the same type of stack as in Example 2, but the intermediate cathode elements and the current output electrodes were coated with diboride. titanium.
- the aluminum chloride electrolysis bath had the same composition as above and was maintained at the temperature of 720 ° C. ⁇ 10 ° C.
- the feed rate in the enriched bath was 248 kg / h and was adjusted from measurement of the conductivity of the bath and of a level detector.
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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)
- Secondary Cells (AREA)
Claims (19)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR8111021 | 1981-05-29 | ||
FR8111021A FR2506789A1 (fr) | 1981-05-29 | 1981-05-29 | Cellule de production electrolytique d'un metal a partir de son halogenure |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0069681A1 EP0069681A1 (de) | 1983-01-12 |
EP0069681B1 true EP0069681B1 (de) | 1986-02-05 |
Family
ID=9259162
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP82420065A Expired EP0069681B1 (de) | 1981-05-29 | 1982-05-26 | Zelle zur elektrolytischen Herstellung eines Metalls aus seinem Halogenid |
Country Status (13)
Country | Link |
---|---|
US (1) | US4459195A (de) |
EP (1) | EP0069681B1 (de) |
JP (1) | JPS57203784A (de) |
AU (1) | AU548317B2 (de) |
BR (1) | BR8203117A (de) |
CA (1) | CA1167409A (de) |
DE (1) | DE3268930D1 (de) |
ES (1) | ES512612A0 (de) |
FR (1) | FR2506789A1 (de) |
GR (1) | GR68280B (de) |
IN (1) | IN157813B (de) |
NO (1) | NO821803L (de) |
NZ (1) | NZ200772A (de) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AU2713684A (en) * | 1983-04-26 | 1984-11-01 | Aluminium Company Of America | Electrolytic cell |
DE19533773A1 (de) * | 1995-09-12 | 1997-03-13 | Basf Ag | Plattenstapelzelle |
US8199023B2 (en) * | 2008-10-15 | 2012-06-12 | Alcoa Inc. | Systems, methods and apparatus for tapping a metal electrolysis cell |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US659655A (en) * | 1899-03-31 | 1900-10-16 | Edwin Edser | Apparatus for the electrolytic decomposition of alkaline salts. |
GB1403892A (en) * | 1971-09-08 | 1975-08-28 | Aluminum Co Of America | Electrolytic metal producing process and apparatus |
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 |
FR2409326A1 (fr) * | 1977-11-18 | 1979-06-15 | Nippon Light Metal Co | Cellule d'electrolyse d'aluminium |
US4308115A (en) * | 1980-08-15 | 1981-12-29 | Aluminum Company Of America | Method of producing aluminum using graphite cathode coated with refractory hard metal |
-
1981
- 1981-05-29 FR FR8111021A patent/FR2506789A1/fr active Granted
- 1981-09-10 GR GR66010A patent/GR68280B/el unknown
-
1982
- 1982-03-08 IN IN267/CAL/82A patent/IN157813B/en unknown
- 1982-04-19 US US06/369,583 patent/US4459195A/en not_active Expired - Fee Related
- 1982-05-26 EP EP82420065A patent/EP0069681B1/de not_active Expired
- 1982-05-26 DE DE8282420065T patent/DE3268930D1/de not_active Expired
- 1982-05-26 JP JP57089606A patent/JPS57203784A/ja active Pending
- 1982-05-27 NZ NZ200772A patent/NZ200772A/xx unknown
- 1982-05-28 NO NO821803A patent/NO821803L/no unknown
- 1982-05-28 AU AU84282/82A patent/AU548317B2/en not_active Ceased
- 1982-05-28 BR BR8203117A patent/BR8203117A/pt unknown
- 1982-05-28 CA CA000404037A patent/CA1167409A/fr not_active Expired
- 1982-05-28 ES ES512612A patent/ES512612A0/es active Granted
Also Published As
Publication number | Publication date |
---|---|
JPS57203784A (en) | 1982-12-14 |
AU548317B2 (en) | 1985-12-05 |
DE3268930D1 (en) | 1986-03-20 |
CA1167409A (fr) | 1984-05-15 |
FR2506789B1 (de) | 1983-10-07 |
IN157813B (de) | 1986-06-28 |
EP0069681A1 (de) | 1983-01-12 |
ES8304220A1 (es) | 1983-02-16 |
FR2506789A1 (fr) | 1982-12-03 |
GR68280B (de) | 1981-11-20 |
NO821803L (no) | 1982-11-30 |
NZ200772A (en) | 1985-09-13 |
US4459195A (en) | 1984-07-10 |
ES512612A0 (es) | 1983-02-16 |
AU8428282A (en) | 1982-12-02 |
BR8203117A (pt) | 1983-05-10 |
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