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US3512928A - Purification of magnesium chloride salts for electrolytic magnesium production - Google Patents

Purification of magnesium chloride salts for electrolytic magnesium production Download PDF

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Publication number
US3512928A
US3512928A US649824A US3512928DA US3512928A US 3512928 A US3512928 A US 3512928A US 649824 A US649824 A US 649824A US 3512928D A US3512928D A US 3512928DA US 3512928 A US3512928 A US 3512928A
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US
United States
Prior art keywords
carbon
magnesium
bath
oxygen
purification
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
US649824A
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English (en)
Inventor
Leland R Lyons
Walter R Mccormick Jr
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.)
AMAX MAGNESIUM Corp A CORP OF
Original Assignee
Nat Lead 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
Application filed by Nat Lead Co filed Critical Nat Lead Co
Application granted granted Critical
Publication of US3512928A publication Critical patent/US3512928A/en
Assigned to AMAX MAGNESIUM CORPORATION reassignment AMAX MAGNESIUM CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: NL INDUSTRIES, INC.,
Anticipated expiration legal-status Critical
Assigned to CONGRESS FINANCIAL CORPORATION, 1133 AVENUE OF THE AMERICAS, NEW YORK, NY 10036, A CORP. OF CA reassignment CONGRESS FINANCIAL CORPORATION, 1133 AVENUE OF THE AMERICAS, NEW YORK, NY 10036, A CORP. OF CA SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). AUGUST 31, 1989 Assignors: AMAX MAGNESIUM A CORP. OF DE
Assigned to ITT COMMERCIAL FINANCE CORP., A CORP. OF NV reassignment ITT COMMERCIAL FINANCE CORP., A CORP. OF NV SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: AMAX MAGNESIUM CORPORATION
Assigned to AMAX MAGNESIUM CORPORATION, A CORP. OF DE reassignment AMAX MAGNESIUM CORPORATION, A CORP. OF DE ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: AMAX INC., A NY CORP.
Assigned to MAGNESIUM CORPORATON OF AMERICA reassignment MAGNESIUM CORPORATON OF AMERICA RELEASE BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: ITT COMMERCIAL FINANCE CORP.
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/26—Magnesium halides
    • C01F5/30—Chlorides
    • 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

Definitions

  • This invention pertains to improvements in the productlon of magnesium metal by electrolysis of magnesium chloride in fused salt baths containing the same.
  • the Invention pertains more particularly to the substantial elimination from such baths and/or from fused salts employed in such baths, of oxygen bearing compounds WlllCl] attack the anodes and/or refractory lining of the electrolysis cell.
  • sulfates in particular, present in the bath attack the carbon anode and refractory lining of the electrolysis cell with deleterious effects as above noted.
  • these sulfates or other oxygen bearing materials which are soluble in the bath may be eliminated from the bath or from fused salts introduced into the bath, by appropriate additions thereto of carbon in a highly dispersed or reactive form, such as activated carbon, or carbon bearing materials which produce activated carbon in the bath at the bath operating temperature, such as organic matter from marine organisms which produce activated carbon char at bath operating temperatures.
  • Other bath additions which I have found suitable are such substances as molasses, which upon destructive distillation in the bath produces carbon particles of colloidal particle s1ze, uniformly dispersed throughout the bath.
  • the preferred treatment of the salts employed in the bath for eliminating or rendering innocuous, oxygen bearing compounds present in the salts is to pretreat them by fusion in the presence of the aforesaid activated or colloidal carbon dispersion or in admixture with an organic material production thereof in the fused salt.
  • the activated or colloidal carbon dispersion should be present in the fused salt in at least the amount required to react with the oxygen values which are evolved as CO and/or CO and as S0
  • the invention finds particular application to elimination of residual sulfate values from aqueous salt solutions containing magnesium chloride and sulfate values, which have been processed substantially to eliminate the sulfate values for recovery of the magnesium values as MgCl Examples of this are naturally occurring brines,
  • a process for recovering magnesium or MgCl from such brine consists in subjecting the brine to successive concentrations, first to eliminate principally the sodium values as NaCl, and thence principally the potassium values as potassium-magnesium double salts, leaving MgCl and MgSO, in solution in the mother liquor, which is substantially desulfated by treatment with calcium chloride, with precipitation of CaSO which is removed by filtration.
  • the residual potassium values precipitate as the double salt, carnallite, along with residual NaCl, to leave an essentially MgCl mother liquid, which is further concentrated and ultimately reduced to powder form by spray drying.
  • the essentially MgCl powder thus produced nevertheless contains sufficient of the sulfate radical as upon fused salt electrolysis thereof to attack the electrolysis cell carbon anodes and refractory lining, unless either pretreated in fused state with sulficient activated carbon present or produced therein upon fusion, or added as such or in an organic material productive thereof, to remove the SO, values, or unless sutficient such activated carbon is present, produced or introduced into the electrolysis cell along with the powdered MgCl to accomplish this result.
  • the data show that the dispersed carbon produced by melting the dried and the dried and dehydrated MgCl powders reduce the S content to less than 0.05% in each instance, from initial values of about 0.1O.13%.
  • EXAMPLE II The effect of adding carbOn in the form of molasses to the concentrated MgCl solution obtained by processing a naturally occurring brine in the manner above set forth, is shown by this example, wherein for each 100 grams of MgCl in solution, there was added in one test, 2 grns of epsom salts, MgSO -7H O, and 0.5 gm. molasses of specific gravity 1.38, and in another test was added 1 gm. of epsom salts and 0.07 gm. of said molasses. The two test solutions were then spray dried, HCl dehydrated, and melted with results as to S0, and carbon contents at various stages as follows:

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Manufacture And Refinement Of Metals (AREA)
US649824A 1967-06-29 1967-06-29 Purification of magnesium chloride salts for electrolytic magnesium production Expired - Lifetime US3512928A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US64982467A 1967-06-29 1967-06-29

Publications (1)

Publication Number Publication Date
US3512928A true US3512928A (en) 1970-05-19

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
US649824A Expired - Lifetime US3512928A (en) 1967-06-29 1967-06-29 Purification of magnesium chloride salts for electrolytic magnesium production

Country Status (7)

Country Link
US (1) US3512928A (de)
BE (1) BE717238A (de)
DE (1) DE1767896C3 (de)
FR (1) FR1579660A (de)
GB (1) GB1232074A (de)
IL (1) IL30160A (de)
NO (1) NO119634B (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3953574A (en) * 1974-11-25 1976-04-27 N L Industries, Inc. Process for purifying molten magnesium chloride
US4076602A (en) * 1975-04-14 1978-02-28 Wheeler Roger M Method of producing magnesium metal and chlorine from MgCl2 containing brine
US4248839A (en) * 1979-07-30 1981-02-03 Nl Industries, Inc. Chlorination of impure magnesium chloride melt

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1331688A (en) * 1917-09-29 1920-02-24 British Aluminium Co Ltd Production and utilization of magnesium chlorid
GB293410A (en) * 1927-04-06 1928-07-06 Ig Farbenindustrie Ag Process for the production of anhydrous chlorides free from oxides
US1798091A (en) * 1925-10-27 1931-03-24 Lichtenberger Theodor Process for manufacturing the chlorides of the alkaline-earth metals from the sulphates of the alkaline-earth metals
US1923594A (en) * 1928-04-24 1933-08-22 Magnesium Dev Corp Process for producing anhydrous nonvolatile metal chlorides
US1933499A (en) * 1928-10-04 1933-10-31 Magnesium Dev Corp Process for producing anhydrous magnesium chloride
US3098722A (en) * 1959-01-16 1963-07-23 Nat Distillers Chem Corp Purification of metal halides
US3148950A (en) * 1961-02-27 1964-09-15 Crown Zellerbach Corp Process of treating metal sulfates
US3218122A (en) * 1963-05-22 1965-11-16 American Cyanamid Co Purification of ferric chloride
US3305302A (en) * 1963-10-02 1967-02-21 Gen Refractories Co Process of beneficiating magnesite

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1331688A (en) * 1917-09-29 1920-02-24 British Aluminium Co Ltd Production and utilization of magnesium chlorid
US1798091A (en) * 1925-10-27 1931-03-24 Lichtenberger Theodor Process for manufacturing the chlorides of the alkaline-earth metals from the sulphates of the alkaline-earth metals
GB293410A (en) * 1927-04-06 1928-07-06 Ig Farbenindustrie Ag Process for the production of anhydrous chlorides free from oxides
US1923594A (en) * 1928-04-24 1933-08-22 Magnesium Dev Corp Process for producing anhydrous nonvolatile metal chlorides
US1933499A (en) * 1928-10-04 1933-10-31 Magnesium Dev Corp Process for producing anhydrous magnesium chloride
US3098722A (en) * 1959-01-16 1963-07-23 Nat Distillers Chem Corp Purification of metal halides
US3148950A (en) * 1961-02-27 1964-09-15 Crown Zellerbach Corp Process of treating metal sulfates
US3218122A (en) * 1963-05-22 1965-11-16 American Cyanamid Co Purification of ferric chloride
US3305302A (en) * 1963-10-02 1967-02-21 Gen Refractories Co Process of beneficiating magnesite

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3953574A (en) * 1974-11-25 1976-04-27 N L Industries, Inc. Process for purifying molten magnesium chloride
US4076602A (en) * 1975-04-14 1978-02-28 Wheeler Roger M Method of producing magnesium metal and chlorine from MgCl2 containing brine
US4248839A (en) * 1979-07-30 1981-02-03 Nl Industries, Inc. Chlorination of impure magnesium chloride melt

Also Published As

Publication number Publication date
DE1767896A1 (de) 1972-03-30
FR1579660A (de) 1969-08-29
DE1767896C3 (de) 1975-01-02
DE1767896B2 (de) 1974-05-22
IL30160A0 (en) 1968-08-22
BE717238A (de) 1968-12-02
GB1232074A (de) 1971-05-19
NO119634B (de) 1970-06-15
IL30160A (en) 1972-09-28

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AS Assignment

Owner name: AMAX MAGNESIUM CORPORATION, 600 LANIDEX PLAZA, PAR

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:NL INDUSTRIES, INC.,;REEL/FRAME:003829/0452

Effective date: 19801107

AS Assignment

Owner name: CONGRESS FINANCIAL CORPORATION, 1133 AVENUE OF THE

Free format text: SECURITY INTEREST;ASSIGNOR:AMAX MAGNESIUM A CORP. OF DE;REEL/FRAME:005165/0690

Effective date: 19890831

AS Assignment

Owner name: AMAX MAGNESIUM CORPORATION, A CORP. OF DE, UTAH

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:AMAX INC., A NY CORP.;REEL/FRAME:005161/0219

Effective date: 19890809

Owner name: ITT COMMERCIAL FINANCE CORP., A CORP. OF NV, NEVAD

Free format text: SECURITY INTEREST;ASSIGNOR:AMAX MAGNESIUM CORPORATION;REEL/FRAME:005271/0220

Effective date: 19890831

AS Assignment

Owner name: MAGNESIUM CORPORATON OF AMERICA, UTAH

Free format text: RELEASE BY SECURED PARTY;ASSIGNOR:ITT COMMERCIAL FINANCE CORP.;REEL/FRAME:006723/0341

Effective date: 19930922