US2998373A - Electrolytic cell for production of titanium - Google Patents

Electrolytic cell for production of titanium Download PDF

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Publication number
US2998373A
US2998373A US9764A US976460A US2998373A US 2998373 A US2998373 A US 2998373A US 9764 A US9764 A US 9764A US 976460 A US976460 A US 976460A US 2998373 A US2998373 A US 2998373A
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US
United States
Prior art keywords
cathode
cell
chamber
flange
anolyte
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
US9764A
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English (en)
Inventor
George E Snow
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.)
New Jersey Zinc Co
Original Assignee
New Jersey Zinc Co
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority to NL131349D priority Critical patent/NL131349C/xx
Priority to NL261315D priority patent/NL261315A/xx
Application filed by New Jersey Zinc Co filed Critical New Jersey Zinc Co
Priority to US9764A priority patent/US2998373A/en
Priority to GB5030/61A priority patent/GB913477A/en
Priority to FR852842A priority patent/FR1281045A/fr
Priority to BE600273A priority patent/BE600273A/fr
Priority to LU39791D priority patent/LU39791A1/xx
Priority to DEN19624A priority patent/DE1148757B/de
Application granted granted Critical
Publication of US2998373A publication Critical patent/US2998373A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C25C3/26—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium
    • C25C3/28—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium of titanium
    • 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

Definitions

  • the metallic titanium deposit on the cathode may then be harvested either in situ in the bath or the cathode and anode may be withdrawn from the fused salt bath for harvesting the cathode deposit.
  • a particularly satisfactory form of cathode comprises an open-bottomed cylindrical cathode which, during cell operation, rests upon or adjacent the bottom of the cell in such relation to the cell bottom as to prevent physical contact bet-ween the two portions of the molten bath on opposite sides of the junction of the cathode and the cell bottom. Such a cathode does not require removal of the anode for harvesting of the cathode.
  • Freezing the fused salt bath electrolyte at the cathodecell bottom junction has been found to be a partial solution to this problem.
  • the water cooling necessary to freeze the salt introduces such excessive stresses in the cell bottom as to cause even a metallic cell to crack, and the frozen salt adjacent the cathode bottom requires time for thawing before the cathode is free to be withdrawn.
  • the improved cathode structure of my invention makes it possible to prevent physical contact of anolyte and catholyte portions of the bath on opposite sides of the cathode adjacent this junction and thus prevents deposition of metallic titanium, either electrically or chemically, adjacent the zone of contact or zone of near-contact between the open bottom of the cathode and the bottom of the cell.
  • the cathode is immediately removable from and easily replaceable in its operative position in the cell.
  • My novel cathode structure comprises an inverted trough-shaped annular chamber connected to the cathode adjacent the open bottom thereof and an upstanding flange on the bottom of the cell extending upwardly into the interior of said chamber.
  • the interior portion of the chamber into which the flange extends is adapted to contain a gaseous atmosphere inert with respect to the fused salt bath, whereby the anolyte and catholyte portions of the bath on opposite sides of the flange are prevented from coming into physical contact with one another by the body of said gas entrapped in the chamber. There is, accordingly, no ionic contact between the anolyte and catholyte adjacent the flange.
  • FIG. 1 comprises a partial cross-sectional elevation showing the cathode just prior to its ultimate positioning Within the cell;
  • FIG. 2. is :a partial cross-sectional elevation showing the cathode in its operating position
  • FIG. 3 is a cross-sectional elevation of an electrolytic cell embodying the invention.
  • an anode 6 is positioned centrally within the cell.
  • the anode may be suspended above the cell bottom 7 or it may, as in other conventional cell design, extend upwardly through the bottom of the cell.
  • a cylindrically-shaped cathode 8 is concentrically positioned about the anode and divides the molten salt bath within the cell 5 into an anolyte portion A and a catholyte portion C. The lower openbottomed portion of the cathode 8 is.
  • an inwardly (or outwardly) and downwardly projecting flange 10 which, together with the lowermost portion of the cathode, forms an inverted annular trough-shaped chamber around the periphery of the open bottom of the cathode.
  • the cathode is lowered into its ultimate position only after a gas such as argon, helium, or the like, inert with respect to the fused salt bath, is bubbled intothe inverted trough-shaped chamber through a removable tube 11 or the like.
  • the gas is bubbled into the chamber for a suflicient period of time not only to form a gas pocket in the upper portion of the chamber but to insure complete displacement of air initially trapped in the chamber as the cathode is lowered [from the top of the cell.
  • the cathode is lowered to its ultimate position, shown in FIG. 2, with the chamber registering with an upstanding flange 12 struck up from the bottom 7 of the cell.
  • the inert gas trapped in the upper portion of the trough-shaped chamber at the bottom of the cathode prevents the molten salt bath from filling the chamber, and consequently the topof the upstanding flange 12 extends above the level of molten salt within the chamber.
  • This arrangement prevents physical communication between the anolyte and catholyte portions on opposite sides .2 3 of the upstanding flange 12 and thus prevents communication between the main body of anolyte A and catholyte C on opposite sides of the cathode adjacent the bottom of the cathode.
  • the bottom of the cathode 8 can be suspended above and out of contact with the cell bottom 7 in order to maintain electrical isolation of the cathode and cell bottom where this condition is desired.
  • the cathode can equally well rest upon the bottom of the cell if this electrical isolation of cathode and cell is not required, and even 'under these conditions it has been found that the lack of physical communication between anolyte and catholyte portions of the fused salt bath prevents the 'formationof any significant amounts of metallic titanium at the zone of contact of the cathode and cell bottom.
  • the gas seal device was used in a 72" diameter cell with a 40" diameter bottom entry anode and a 44" diameter cathode operated as described in the United States patent to Reimert and Fatzinger No. 2,848,397.
  • the cathode 8 was supported from the cell roof 13 (FIG. 3) by current-carrying rods 14, and the cell atmosphere above the bath was separated into anode and cathode compartments by a cylindrical baflle 15 in which chlorine evolved from the anode 6 was collected and removed from the cell through an exhaust line 16.
  • the inverted trough-shaped chamber was 4% high with an outside diameter of 48%".
  • the upstanding annular flange 12 attached to the cell bottom was 3% high.
  • a sealing device for joining the cathode to the bottom of the cell which-comprises an inverted troughshaped annular chamber connected to the cathode adjacent the open bottom thereof, and an upstanding flange on the bottom of the cell extending upwardly into the interior of said chamber, the interior portion of the chamber into which the flange extends being adapted to contain a gaseous atmosphere inert with respect to the fused salt bath, whereby the anolyte and catholyte portions of the bath on opposite sides of the flange are prevented from-coming into physical contact with one another by the body of said gas entrapped in the chamber.
  • a sealing device for joining the cathode to the bottom of the cell which comprises an inwardly and downwardly extending flange joined to the surf-ace of the cathode above the bottom edge thereof-so as to form an inverted trough-shaped annular chamber connected to the cathode adjacent the open bottom thereof, and an upstanding flange on the bottom of the cell extending upwardly into the interior of said chamber, the interior portion of the chamber into which the flange extends being adapted to contain a gaseous atmosphere inert with respect to the fused salt bath, whereby the anolyte and catholyte portions of the bath on opposite sides of the flange are prevented from coming into physical Contact with one 'ahoth'er by the 'body of said gas entrapped in the chamber
  • a sea-ling device for joining the cathode to the bottom of the cell which comprises an outwardly and downwardly extending flange joined to the 'surfaceof the cathode above the bottom-edge thereof so as to form an inverted trough-shaped annular chamber connected to the cathode adjacent the open bottom thereof, and an upstanding flange on the bottom of the cell extending upwardly into the interior of said chamber, the interior portion of the chamber into which the flange extends being adapted to contain a gaseous atmosphere inert with respect to the fused salt bath, whereby the anolyte and catholyte portions of the bath on opposite sides of the flange are prevented from coming into physical contact with one another by the body of said gas entrapped in the chamber.
  • a sealing device for joining the cathode to the bottom of the cell which comprises an inverted troughshaped annular chamber connected to the cathode adjacent the open bottom thereof, and an upstanding flange on the bottom of the cell extending upwardly into the interior of said chamber, the interior portion of the chamber into which the flange extends being adapted to contain a gaseous atmosphere inert with respect to the fused salt bath, whereby the anolyte and catholyte portions of the bath on opposite sides of the flange are prevented from coming into physical contact with one another by the body of said gas entrapped in the chamber, the bottom of the cathode being suspended out of physical contact with the cell bottom.
  • a sealing device for joining the cathode to the bottom of the cell which comprises an inverted troughshaped annular chamber connected to the cathode adjacent the open bottom thereof, and an upstanding flange on the bottom of the cell extending upwardly into the interior of said chamber, the interior portion of the chamber into which the flange extends being adapted to contain a gaseous atmosphere inert with respect'to the fused salt bath, whereby the anolyte and catholyte portions of the bath on opposite sides of the flange are prevented from coming into physical contact with one another by the body of said gas entrapped in the chamber, the bottom of the cathode being supported on the cell bottom.

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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)
US9764A 1960-02-19 1960-02-19 Electrolytic cell for production of titanium Expired - Lifetime US2998373A (en)

Priority Applications (8)

Application Number Priority Date Filing Date Title
NL131349D NL131349C (de) 1960-02-19
NL261315D NL261315A (de) 1960-02-19
US9764A US2998373A (en) 1960-02-19 1960-02-19 Electrolytic cell for production of titanium
GB5030/61A GB913477A (en) 1960-02-19 1961-02-10 Fused electrolyte electrolytic cells
FR852842A FR1281045A (fr) 1960-02-19 1961-02-15 Production de titane
BE600273A BE600273A (fr) 1960-02-19 1961-02-16 Production de titane.
LU39791D LU39791A1 (de) 1960-02-19 1961-02-17
DEN19624A DE1148757B (de) 1960-02-19 1961-02-18 Elektrolytische Zelle, insbesondere zur Herstellung von Titan durch Schmelzflusselektrolyse

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US9764A US2998373A (en) 1960-02-19 1960-02-19 Electrolytic cell for production of titanium

Publications (1)

Publication Number Publication Date
US2998373A true US2998373A (en) 1961-08-29

Family

ID=21739567

Family Applications (1)

Application Number Title Priority Date Filing Date
US9764A Expired - Lifetime US2998373A (en) 1960-02-19 1960-02-19 Electrolytic cell for production of titanium

Country Status (6)

Country Link
US (1) US2998373A (de)
BE (1) BE600273A (de)
DE (1) DE1148757B (de)
GB (1) GB913477A (de)
LU (1) LU39791A1 (de)
NL (2) NL261315A (de)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4521281A (en) * 1983-10-03 1985-06-04 Olin Corporation Process and apparatus for continuously producing multivalent metals
CN101235520B (zh) * 2008-03-05 2010-06-09 东北大学 TiCl4熔盐电解制取金属钛的方法与电解槽

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2848397A (en) * 1954-07-06 1958-08-19 New Jersey Zinc Co Electrolytic production of metallic titanium
US2871178A (en) * 1957-02-14 1959-01-27 Titanium Metals Corp Electrode sealing and power connection apparatus
US2900318A (en) * 1955-11-29 1959-08-18 New Jersey Zinc Co Electrolyzing device
US2908619A (en) * 1958-08-01 1959-10-13 New Jersey Zinc Co Production of titanium

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2848397A (en) * 1954-07-06 1958-08-19 New Jersey Zinc Co Electrolytic production of metallic titanium
US2900318A (en) * 1955-11-29 1959-08-18 New Jersey Zinc Co Electrolyzing device
US2871178A (en) * 1957-02-14 1959-01-27 Titanium Metals Corp Electrode sealing and power connection apparatus
US2908619A (en) * 1958-08-01 1959-10-13 New Jersey Zinc Co Production of titanium

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4521281A (en) * 1983-10-03 1985-06-04 Olin Corporation Process and apparatus for continuously producing multivalent metals
CN101235520B (zh) * 2008-03-05 2010-06-09 东北大学 TiCl4熔盐电解制取金属钛的方法与电解槽

Also Published As

Publication number Publication date
NL261315A (de)
DE1148757B (de) 1963-05-16
NL131349C (de)
BE600273A (fr) 1961-06-16
LU39791A1 (de) 1961-04-17
GB913477A (en) 1962-12-19

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