Classifications

• • 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

Definitions

• the normally stable lower chlorides orbromides, especially the dihalides, of titanium can be obtained in a convenient way and with a very high yield by the reaction of the corresponding tetrahalide vapour with heated titanium bearing material, preferably under'reduced pressure, whereby the vapoursof these lower halides areformed and can be condensed as solids in a cooler zone,
• the unsaturated tetrahalide vapour the lower halides are condensed entirely free from halide, pure titanium is bearing material and the originally applied tetrahalide is produced from the titanium recovered.
• the metallic titanium formed by this procedure consisting of small discrete leaflets (flakes) can on account of its form very readily be submitted to further metallurgical processing, for example to pressing and 'sintering, and on this account has considerable advantages over other metallic titanium products, for example .the sponge which is formed by the reduction of titanium tetrachloride with magnesium.
• pure metallic titanium can be extracted from titanium hearing material of the group consisting of impure titanium and titanium alloys (especially impure titanium ortitanium alloys, such as ferrotitanium, made by reduction of a raw material with carbon) by passing over them titanium.
• impure titanium and titanium alloys especially impure titanium ortitanium alloys, such as ferrotitanium, made by reduction of a raw material with carbon
• titanium tetrachloride or tetrabromide vapour respectively; If the decomposition is carried out using hydrogen as carrier gas, the metallic titanium may afterwards require heating in vacuum to 'remove' absorbed hydrogen.
• the titanium tetrahalide formed is also led into a separate condenser preferably the tetrahalide condenser referred to above,,so that the whole of the titanium tetrachloride or tetrabromide originally used may be re-applied for further extraction; alternatively, since the vapour pressures of the titanium tetrachloride or tetrabromide are high at moderately. elevated temperatures, they may be recirculated in the gaseous state without previous condensation.
• the diand tri-chlorides (or bromides) are highly hygroscopic solids it is usually advantageous, but not necessary, to
• a, continuous extraction can be achieved using either continuous circulationlof the tetrahalide without condensation, or-alternativelycondensihg the tetrahalide 'and'using at least two tetrahalide condensers serving alternately as condensers and evaporators.
• Graphite or a refractory carbide likewise provid'es a suitable condenser material, protective coatings (of titanium carbide) being formed in'this' case also.
• a suitable combination of temperature and pressure when using titanium tetrachloride according to the method of the invention maybe seen from the following example.
• a stream of argon was saturated with titanium tetrachloride vapour at 20 C. (thusc'ontaining titanium tetrachloride at a partial pressure of about 1-0 mm.) and was passed over pieces of impure titanium (3 to 6 mesh), containing carbon as main impurity, maintained at about 1050 C. and contained in a graphite tube lined with a material, su'chas molybdenum, showing no reaction with the gaseous products under these reaction conditions.
• reaction products passed into a cooler zone of the tube where a condensate formed consisting mainly of titanium dichloride in yield corresponding to about 40% of complete conversion of tetrachloride, but containing also much smaller amounts of metallic titanium and titanium trichloride.
• the stream of argon containing titatetrachloride' vapour was discontinued, a stream of pure argon passed and the temperature of the condensate raised toabout' 950 C. Titanium tetrachloride vapour was evolved and collected in a suitable condenser, but after some time the argon stream leaving the reaction tube no longer contained titanium tetrachloride vapour, and metallic titanium, free from carbon, remained in the condenser;
• reaction products condensing again consisted mainly of titanium dichloride (in a yield corresponding to about 35% of complete conversion of the'tet'rachloride), together with much smaller amounts of titanium trichloride and metallic titanium.
• the lower chlorides were converted to metallic titanium by'heating' to 950 C. in the manner described above;
• a process for extracting titanium from titanium bearing'material of the group consisting of impure titaniunr'a'nd" titanium alloys which comprises the following. st'eps,-all"carried out in an inert atmosphere;.heating, the titanium bearing "material, evaporating a titanium tetra halide of the group consisting of chloride and bromide, leading the vapour' of said tetrahalide in an unsaturated state over'the heated material, thereby to form a vapour mixture containing said tetrahalide and lower normally stable titanium halides, leading.
• vapour mixture toacooler zone whereby the lower halides condense as-solids except fora small amount which decomposes into tetrahalidevapour and purified titaniu m which condenseswith thelowerh'alides, reducing the tetrahalide pressure in said cooler zone to a value.
• A'process for extracting titanium from titanium hearing material of the group consisting of impure tita-' nium and titanium alloys which comprises the following steps, all carried out in an inert atmosphere; heating the titanium bearing material, evaporating a titanium tetrahalide of the group consisting of chloride and bromide, leading the vapour of said tetrahalide in an unsaturated state and under a partial vacuum over the heated material thereby to form a vapour mixture containing said tetrahalide and lower normally stable titanium halides, leading said vapour mixture to a cooler zone whereby the lower halides condense as solids except for a small amount which decomposes into tetrahalide vapour and purified titanium which condenses with the lower halides, reducing the tetrahalide pressure in said cooler Zone to a value lower than the decomposition pressure of the lower halides while heating the condensate therein to a temperature below the temperature at which under the applied pressure the halides will dissoci
• a process for extracting titanium from titanium bearing material of the group consisting of impure titanium and titanium alloys which comprises the following steps, all carried out in an inert atmosphere; heating the titanium bearing material, evaporating a titanium tetrahalide of the group consisting of chloride and bromide, leading the vapour of said tetrahalide in an unsaturated state over the heated material, thereby to form a vapour mixture containing said tetrahalide and lower normally stable titanium halides, leading said vapour mixture to a cooler zone whereby the lower halides condense as solids except for a small amount which decomposes into tetrahalide vapour and purified titanium which condenses with the lower halides as flakes, reducing the tetrahalide pressure in said cooler zone to a value lower than the decomposition pressure of the lower halides while heating the condensate therein to a temperature below the temperature at which under the applied pressure the halides will dissociate into metallic titanium and free halogen,
• a process for extracting titanium from titanium bearing material of the group consisting of impure titanium and titanium alloys which comprises the following steps, all carried out in an inert atmosphere; heating the titanium bearing material, evaporating a titanium tetrahalide of the group consisting of chloride and bromide, leading the vapour of said tetrahalide in an unsaturated state over the heated material, thereby to form a vapour mixture containing said tetrahalide and lower normally stable titanium halides, leading said vapour mixture to a cooler zone whereby the lower halides condense as solids except for a small amount which decomposes into tetrahalide vapour and purified titanium which condenses with the lower halides, reducing the tetrahalide pressure in said cooler zone to a value lower than the decomposition pressure of the lower halides while heating the condensate therein to a temperature below the temperature at which under the applied pressure the halides will dissociate into metallic titanium and free halogen, thereby to de
• a process for extracting titanium from titanium bearing material of the group consisting of impure titanium and titanium alloys which comprises the following steps, all carried out in an inert atmosphere; heating the titanium bearing material, evaporating a titanium tetrahalide of the group consisting of chloride and bromide, leading the vapour of said tetrahalide in an unsaturated state over the heated material, thereby to form a vapour mixture containing said tetrahalide and lower normally stable titanium halides, leading sai-d vapour mixture to a cooler zone whereby the lower halides condense as solids except for a small amount which decomposes into tetrahalide vapour and purified titanium which condenses with the lower halides, reducing the tetrahalide pressure in said cooler zone to a value lower than the decomposition pressure of the lower halides while heating the condensate therein to a temperature below the temperature at which under the applied pressure the halides will dissociate into metallic titanium and free halogen

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• 1951
  • 1951-09-05 GB GB20957/51A patent/GB722901A/en not_active Expired
• 1952
  • 1952-08-19 US US305292A patent/US2785973A/en not_active Expired - Lifetime
  • 1952-08-29 FR FR1145103D patent/FR1145103A/fr not_active Expired
  • 1952-09-05 DE DEF9844A patent/DE974695C/de not_active Expired

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