US2868703A - Cell feed material for the production of titanium - Google Patents

Cell feed material for the production of titanium Download PDF

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Publication number
US2868703A
US2868703A US467581A US46758154A US2868703A US 2868703 A US2868703 A US 2868703A US 467581 A US467581 A US 467581A US 46758154 A US46758154 A US 46758154A US 2868703 A US2868703 A US 2868703A
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US
United States
Prior art keywords
titanium
carbon
monoxide
carbide
feed material
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
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US467581A
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English (en)
Inventor
Wainer Eugene
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.)
Horizons Titanium Corp
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Horizons Titanium Corp
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Filing date
Publication date
Application filed by Horizons Titanium Corp filed Critical Horizons Titanium Corp
Priority to US467581A priority Critical patent/US2868703A/en
Priority to GB30352/55A priority patent/GB778354A/en
Priority to DEH25403A priority patent/DE1022804B/de
Priority to US694723A priority patent/US2904426A/en
Application granted granted Critical
Publication of US2868703A publication Critical patent/US2868703A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1295—Refining, melting, remelting, working up of titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/129—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds by dissociation, e.g. thermic dissociation of titanium tetraiodide, or by electrolysis or with the use of an electric arc
    • 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

Definitions

  • Electrolytic techniques may be conveniently classified according to the electrolyte as aqueous or non-aqueous. No successful deposition of titanium from an aqueous bath has been reported to date, but several non-aqueous baths have been successfully'operated to produce the metal.
  • a fused salt bath consisting essentially of one or more halide salts of the alkalimetals or alkaline earth metals together with a simple or complex halide of In an earlier filed applicationY Serial No'.'320,ll3, which any of -a number of well-known processes... lt may bey ture and space grouping'and nearly the same latticelsize,
  • the titaniuml carbide employed may be preparedproduced by reacting pureor pigment. grade titanium di: oxide (T102) in finely divided form (-325 mesh Tyler standard) ⁇ ⁇ with, pure carbon (prepared by calcining lampf,V black) ⁇ under carefully controlled conditions so that the ⁇ titanium dioxide is successively convertedto Ti3O5, Ti203,
  • a transition metal is electrolytically'deposited at a cathode from a salt bath prepared by reacting in a fused halide salt medium, atransitaking placebetween solid materials.
  • the amount of carbon employedshoull be slightly in excess of the stoichiometric amount requiredfor the complete conversionfof TiO2 .to'f1 ⁇ iC-The vproduct obtained is substantially pure TiC. If Vfurther purification is desired the TiC mayk be,4 crushed and any extraneous materials separated leavingA a pure TiC suitable for reaction with the titanium mon oxide'.
  • the titanium monoxide may kbe prepared in any knowny manner; It may be .prepared from titanium carbide in the manner taught inv cachot U. S. Patents 2,681,847@
  • titanium monoxide '(TiO) titanium monoxide '(TiO).
  • Thetir's't step in the conversion is carriedout by heatingna mixture of carbon and titanium dioxide to 'a temperature inthe range'between ll00 C.
  • the cell feed material may, it will be noted, be a consumable anode, or a constituent of the electrolytic bath, or a material employed in the preparationA of the bath.
  • titanium carbide and titanium monoxide under suitable ⁇ reaction conditions.
  • titanium carbide and titanium monoxide have the same cubic strucwhile removing the carbon monoxide as it forms either' by sweeping the furnacev with an inert gas such as argon,
  • titanium' monoxide so produced may, as described in the above-notedl patent application, be further heated to above 1800 C. to pro- ⁇ I dragona fused product admirablyk suited to be reacted with titanium carbide;
  • the carbide and the monoxidef may be lsomewhat impure'without impairing vthe effective? p ness of the process constituting my invention.
  • the carbide may contain some titaniumoxide and the mon? oxdemay contain-someresidual carbon or titaniu'mcar? bide.
  • a second embodimentypellets may be prepared from a mixture vfo'tf'titanium Cbide'andjitanium monoxide proportioned lso astoproduce the desired' final Ti-O C composition.
  • TheHpellets may then he fedinto the hr'th of va Vv"va 1ter 'cooled tungstenarc, water-cooledcopper hearth'arcmeltingfurnace and melted vthereon under an A"actively/5purfnpecl lvacuumlto remove carbon monoxide gas genera-ted during the process.
  • consumable electrodes maybe aro-melted v ⁇ toi produce the desired' alloy.
  • Vrl ⁇ hus la powde rjed lt'ure'of titanium ⁇ carbideandititanium ⁇ monoxide proporti nedfas'above't may be moiste'n'edwith methylated spiritsfand rthen" pressed 'or extrudedf'intothe form of pencils suitable for use las electrodes and then baked or paIrtially sintered.
  • Vrl ⁇ hus la powde rjed lt'ure'of titanium ⁇ carbideandititanium ⁇ monoxide proporti nedfas'above't may be moiste'n'edwith methylated spiritsfand rthen" pressed 'or extrudedf'intothe form of pencils suitable for use las electrodes and then baked or paIrtially sintered.
  • bashed ontliegaccompapyingjgure representing'the. phase TiO"-TiC,'and'the meltingfpoints for the ternary/'system TTOz-C represented..asTfTOfTiC.
  • i' 'i Event gen as one phase and gamma I ⁇ iO,Cy as a second phase.
  • I have obtained an alloy analyzing 5.2% O, 5.5% C and 89.1% Ti by weight. From the gure this would represent an alloy of alpha titanium saturated with respect to oxygen and carbon whose total weight is equal to 97.7%.v o f the composition, the remaining 2.3% being free titanium carbide.
  • the products obtainable by my process have been found, by analysisto'contain from-89% to 92% titanium,' from 2.5%' to 5.5 carbon, and fr om'l.5% to 5% oxygen, depending on the temperature at which the molten. mass .was l1'eld, the proportionsofTiO and TiC employed, the degree of, vacuum, and the length of time the molten mass was held at temperature.
  • titan Infoxygenfcarbon compounds fby their extremely 'high anum @erneut example, .Knzie and .Hoke inQ U. -S., Pa tent 204Q,854eported a product correspond-v ing to the formula Ti2OC2 with a titaniumycontent' b..- tweentejfzg; and .69 whilean U,s. Patent 2,129,161,
  • Ki 'e ra d .fVi/ainde scribe a substance containing about 65.5 T1-corresponding to -'l i3QC3.
  • the titanium-oxygencarbon product of my invention may be added to a fused suggest themselves to those skilled in the art, it being obvious that the product of this invention may be used as a starting material for the preparation of titanium compounds as well as for the electrolytic recovery of titanium.
  • an improved cell feed material for the electrolytic recovery of titanium a composition of matter in which the titanium content is greater than 89% by weight and comprising two phases: a rst phase constituting the major portion of the composition and consisting of alpha titanium containing an amount of carbon and oxygen corresponding to an amount suii'lcient to saturate titanium present in the liquid state while the improved cell feed 0 material is being produced from titanium monoxide and titanium carbide in a process in which at least one of said starting materials is present in the molten state and containing small amounts of titanium carbide as a second phase; in a relative proportion insufficient to lower the titanium content of the two phases to below 89% titanium by weight.
  • composition of matter in which the ltitanium content is between 89% by weight and 92% by weight, the carbon content is between 2.5% and 5.5% by weight and the oxygen content is between 1.5% and 5% by weight, which combination comprises two phases: a small amount of titanium carbide as a second phase in a matrix of alpha titanium saturated with carbon and oxygen.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Carbon And Carbon Compounds (AREA)
US467581A 1954-11-08 1954-11-08 Cell feed material for the production of titanium Expired - Lifetime US2868703A (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US467581A US2868703A (en) 1954-11-08 1954-11-08 Cell feed material for the production of titanium
GB30352/55A GB778354A (en) 1954-11-08 1955-10-24 Manufacture of titanium-oxygen-carbon alloys
DEH25403A DE1022804B (de) 1954-11-08 1955-11-07 Titanreiches Rohmaterial fuer Elektrolysierzellen und Verfahren zur Herstellung desselben
US694723A US2904426A (en) 1954-11-08 1957-11-06 Method of preparing cell feed for the fused salt electrolytic production of titanium

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US467581A US2868703A (en) 1954-11-08 1954-11-08 Cell feed material for the production of titanium

Publications (1)

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US2868703A true US2868703A (en) 1959-01-13

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US467581A Expired - Lifetime US2868703A (en) 1954-11-08 1954-11-08 Cell feed material for the production of titanium
US694723A Expired - Lifetime US2904426A (en) 1954-11-08 1957-11-06 Method of preparing cell feed for the fused salt electrolytic production of titanium

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US694723A Expired - Lifetime US2904426A (en) 1954-11-08 1957-11-06 Method of preparing cell feed for the fused salt electrolytic production of titanium

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DE (1) DE1022804B (de)
GB (1) GB778354A (de)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060237327A1 (en) * 2004-04-21 2006-10-26 Materials & Electrochemical Research Corp. Thermal and electrochemical process for metal production
US20070029208A1 (en) * 2003-08-20 2007-02-08 Withers James C Thermal and electrochemical process for metal production
US20080190778A1 (en) * 2007-01-22 2008-08-14 Withers James C Metallothermic reduction of in-situ generated titanium chloride
US20120152756A1 (en) * 2009-08-06 2012-06-21 Chinuka Limited Treatment of titanium ores
CN103320822A (zh) * 2013-06-27 2013-09-25 中国铝业股份有限公司 一种金属表面电镀钛的方法
CN109161704A (zh) * 2018-09-18 2019-01-08 东北大学 一种Mg-Zn-Ca合金的熔配方法
US11821096B2 (en) 2019-01-14 2023-11-21 Zhejiang Haihong Holding Group Co., Ltd. Device and method for preparing high-purity titanium powder by continuous electrolysis

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3330646A (en) * 1964-02-03 1967-07-11 Harold J Heinen Method for producing molybdenum from molybdenite
US3999981A (en) * 1974-08-05 1976-12-28 Ontario Research Foundation Production and recovery of metallic carbides from ores and concentrates
GB2372257A (en) * 1999-06-25 2002-08-21 Bambour Olubukola Omoyiola Extraction of aluminum and titanium

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2205386A (en) * 1935-08-12 1940-06-25 Fansteel Metallurgical Corp Production of metals and alloys
US2487214A (en) * 1944-04-27 1949-11-08 Wesleyan University Fused pyrosulfate-halide solvent electrolyte
US2661286A (en) * 1950-01-13 1953-12-01 Mallory Sharon Titanium Corp Titanium base alloys containing silicon
US2722509A (en) * 1952-11-12 1955-11-01 Horizons Titanium Corp Production of titanium

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1523103A (en) * 1920-03-12 1925-01-13 D Adrian Alexander L Duval Method of obtaining metals from their respective oxides or ores
GB754981A (en) * 1954-04-23 1956-08-15 Metro Cutanit Ltd Improvements in and relating to methods of reducing oxides of titanium and zirconiumand making titanium and zirconium alloys

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2205386A (en) * 1935-08-12 1940-06-25 Fansteel Metallurgical Corp Production of metals and alloys
US2487214A (en) * 1944-04-27 1949-11-08 Wesleyan University Fused pyrosulfate-halide solvent electrolyte
US2661286A (en) * 1950-01-13 1953-12-01 Mallory Sharon Titanium Corp Titanium base alloys containing silicon
US2722509A (en) * 1952-11-12 1955-11-01 Horizons Titanium Corp Production of titanium

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070029208A1 (en) * 2003-08-20 2007-02-08 Withers James C Thermal and electrochemical process for metal production
US7410562B2 (en) 2003-08-20 2008-08-12 Materials & Electrochemical Research Corp. Thermal and electrochemical process for metal production
US7985326B2 (en) 2003-08-20 2011-07-26 Materials And Electrochemical Research Corp. Thermal and electrochemical process for metal production
US9249520B2 (en) 2003-08-20 2016-02-02 Materials & Electrochemical Research Corp. Thermal and electrochemical process for metal production
US7794580B2 (en) 2004-04-21 2010-09-14 Materials & Electrochemical Research Corp. Thermal and electrochemical process for metal production
US20060237327A1 (en) * 2004-04-21 2006-10-26 Materials & Electrochemical Research Corp. Thermal and electrochemical process for metal production
US9150943B2 (en) 2007-01-22 2015-10-06 Materials & Electrochemical Research Corp. Metallothermic reduction of in-situ generated titanium chloride
US20080190778A1 (en) * 2007-01-22 2008-08-14 Withers James C Metallothermic reduction of in-situ generated titanium chloride
US20120152756A1 (en) * 2009-08-06 2012-06-21 Chinuka Limited Treatment of titanium ores
US9181604B2 (en) * 2009-08-06 2015-11-10 Chinuka Limited Treatment of titanium ores
CN103320822A (zh) * 2013-06-27 2013-09-25 中国铝业股份有限公司 一种金属表面电镀钛的方法
CN109161704A (zh) * 2018-09-18 2019-01-08 东北大学 一种Mg-Zn-Ca合金的熔配方法
CN109161704B (zh) * 2018-09-18 2020-03-24 东北大学 一种Mg-Zn-Ca合金的熔配方法
US11821096B2 (en) 2019-01-14 2023-11-21 Zhejiang Haihong Holding Group Co., Ltd. Device and method for preparing high-purity titanium powder by continuous electrolysis

Also Published As

Publication number Publication date
US2904426A (en) 1959-09-15
DE1022804B (de) 1958-01-16
GB778354A (en) 1957-07-03

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