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United States Patent 19 11 Patent Number: 5,397,375 O'donnell Et Al

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United States Patent 19 11 Patent Number: 5,397,375 O'donnell Et Al USOO5397375A United States Patent 19 11 Patent Number: 5,397,375 O'Donnell et al. (45) Date of Patent: Mar. 14, 1995 54 PROCESS FOR THE PRODUCTION OF 52 U.S.C. ........................................ 75/368; 75/617; METALLICTTANUMAND 75/619 INTERMEDIATES USEFUL IN THE 58) Field of Search .......................... 75/617,619, 368 PROCESSING OF LMENTE AND RELATED MNERALS 56) References Cited 75) Inventors: Thomas A. O'Donnell, Burwood; U.S. PATENT DOCUMENTS John Besida, Yarraville; Tersesa K. 2,647,826 8/1953 Jordan ................................... 75/368 H. Pong, Coburg; David G. Wood, St. 2,986,462 5/1961 Wright .................................. 75/617 Kilda, all of Australia 3,825,415 7/1974 Johnston ............................... 75/619 73 Assignee: The University of Melbourne, 3,847,596 11/1974 Holland ................................. 75/619 Parkville, Australia Primary Examiner-Peter D. Rosenberg 21 Appl. No.:w 107,787 Attorney,Macpeak Agent,& Seas or Firm-Sughrue, Mion, Zinn, 22 PCT Filed: Feb. 21, 1992 57 ABS CT 86 PCT No.: PCT/AU92/00062 The invention relates to a process for the production of S371 Date: Oct. 22, 1993 metallic titanium, characterized in that the process com S 102(e) Date: Oct. 22, 1993 prises reducing a titanium-fluorine compound selected from titanium tetrafluoride and any hexafluorotitanate 87 PCT Pub. No.: WO92/14851 soluble in a molten fluoroaluminate, with metallic alu PCT Pub. Date: Sep. 3, 1992 minum in a molten fluoroaluminate. A process for the 30 Foreign Application Priority Data production of intermediates useful in the processing ilmenite and related minerals is also described. Feb. 21, 1991 AU Australia .............................. PK4721 5ll int. Cl'............................................... C22B5/OO 7 Claims, No Drawings 5,397,375 2 ium (Al) is added. Aluminium is chosen as the reductant PROCESS FOR THE PRODUCTION OF because it is compatible with the melt, being oxidized in METALLICTTANUMAND INTERMEDIATES the first instance to aluminium fluoride (AlF3) and then USEFUL IN THE PROCESSING OFILMENTE interacting with sodium fluoride (NaF) to form cryolite AND RELATED MENERALS (Na3AlF6). In addition, aluminium is much less energy intensive and cheaper to produce than sodium or mag This invention relates to a process for the production nesium reductants used in the current processes. of metallic titanium and intermediates useful in the pro Recovery of metallic titanium is achieved as a conse cessing of ilmenite and related minerals. quence of the relative densities of the reactants and the Australia is the major world producer of ilmenite 10 molten medium. Aluminium is less dense than cryolite which is exported for about A$75 per tonne. The cost which, in turn, is less dense than metallic titanium. of metallic titanium in ingot form is about A$20,000 per Therefore, metallic titanium has a tendency to collect at tonne. In a more refined form, for example, as the titani the bottom of the reaction bath and may be tapped from umbased alloy from which jet engine fan blades are that position with molten cryolite. fabricated, the value of metallic titanium is very much 15 The overall reaction for the reduction of Na2TiF6 by greater. Metallic titanium is, by comparison with most aluminium to metallic titanium in cryolite occurs in other metals and alloys, very resistant to chemical cor accordance with the equation: rosion and is in great demand in the manufacture of chemical plants and for heat-exchangers and other units in power plants. Another important application is the 20 use of metallic titanium in surgical and dental implants The pure compound Na3AlF6 constitutes a neutral and supports. an a strength-for-weight basis, metallic molten medium. If the melt is deficient in NaF, i.e. titanium is stronger than steel and is widely used in the contains an excess of AlF3, the medium is acidic. If the construction of supersonic military aircraft. A cheaper melt contains an excess of NaF, then the medium is manufacturing route to the production of titanium 25 basic. would make feasible its use in civil aircraft to replace Na2TiF6 may be reduced by aluminium to metallic aluminium alloys which have proved to be subject to titanium directly in acidic or basic cryolite i.e. the direct fatigue failure. This is one of the many applications in reduction from Ti(IV) to Ti(0) may occur. However, which the light, strong and non-corrosive metallic tita the ultimate reduction to the metal is preferably carried nium would find wide commercial usage, if available 30 out in neutral cryolite. Under neutral conditions Ti(IV) more cheaply than from current processes. needs to be reduced only to Ti(II), which will dispro Currently, metallic titanium is produced commer portionate spontaneously in neutral medium according cially by two closely related processes. Titanium tetra to the following equation: chloride (TiCl14) is reduced by either metallic sodium (Na) or magnesium (Mg). Each process yields an initial 35 material called "titanium sponge' which may contain 10 to 20% of sodium chloride (NaCl) or magnesium Metallic titanium i.e. Ti(0) is produced, and the chloride (MgCl2) as products of the initial reaction. To Ti(IV) regenerated by the disproportionation reaction avoid inclusion in the sponge of chlorides of titanium in is available for reduction by aluminium to Ti(II) and lower oxidation states (e.g. TiCl2 or TiCl3), excess re subsequent disproportionation. This cyclic process con ducing metal (Na or Mg) is also in the sponge. Both tinues until all Ti(IV) is reduced to Ti(O). methods of production are batch processes and the Advantageously Na2TiF6 is added progressively to sponge, on solidification after reaction, must be re the cryolite bath in order to minimise loss of volatile moved from the reactor manually. It is reported that TiF4 which might result from thermal decomposition of jack-hammers and even explosives are used. The sponge 45 Na2TiF6. Sodium fluoride (NaF) may be added with is then purified at least three times by vacuum arc-melt Na2TiF6 preferably in the ratio 2:1 in order to maintain ing. The processes are both labour and energy intensive. neutrality of the molten cryolite in accordance with the We have now found that a flee-flowing powder of above equation. Aluminium may be added in a stoichio metallic titanium can be produced by employing a pro metric amount or in excess. cess which is similar to conventional aluminium smelt 50 It will be appreciated that the process of the present 1ng. invention may form the basis of a continuous process According to the present invention there is provided similar to that used for aluminium smelting. In one ap a process for the production of metallic titanium, char proach Na2TiF6, Al and NaF may be added to the acterized in that the process comprises reducing a titani cryolite medium, in which case the product of the reac um-fluorine compound selected from titanium tetrafluo 55 tion is cryolite itself. A mixture of molten cryolite and ride and any hexafluorotitanate soluble in a molten the suspended metal may then be tapped from the bot fluoroaluminate, with metallic aluminium in a molten tom of the reactor. The solid material produced may fluoroaluminate. then be crushed and initial separation of cryolite and The preferred titanium-fluorine compound is an alkali titanium metal carried out by any suitable known tech hexafluorotitanate, more preferably, sodium hexa nique, for example, flotation or cyclone separation. Any fluorotitanate (Na2TiF6) or potassium hexafluorotita cryolite remaining attached to the titanium metal parti nate (K2TiF6). cles may be dissolved away from the titanium metal Preferably the molten fluoroaluminate is a hexa using any solution based on a metal cation which will fluoroaluminate, more preferably, cryolite (Na3AlF6). complex with fluoride ions, preferably a solution of a In one particular embodiment of the invention, so 65 water soluble aluminium compound, such as a solution dium hexafluorotitanate (Na2TiF6) or potassium hexa of aluminium nitrate. fluorotitanate (K2TiF6) is dissolved in cryolite (Na Since the process of the present invention is similar to 3AlF6) at about 1000 to 1100 C. and metallic alumin conventional aluminium smelting, an alternative proce 5,397,375 3 4. dure of electrowinning may be used in which Na2TiF6 nate ((NH4)2TiF6) which may be used to produce and AlF3 are added continuously to a cryolite bath, Ti K2TiF6 or Na2TiF6 which is the preferred feedstock being deposited at a graphite cathode. Advantageously employed in the process for the production of metallic a sacrificial anode reaction could be utilized. AlF3 titanium described above. would need to be added in the correct stoichiometric Preferably the alkali fluoride in step c) is potassium amount relative to Na2TiF6 (4:3) in order to maintain fluoride (KF) or sodium fluoride (NaF). neutrality in the cryolite. The alkalifluorometallate produced in step c) may be The feedstock for the process of the present invention K2TiF6 or Na2TiF6 which is the preferred feedstock is preferably K2TiF6 or Na2TiF6. It will be understood employed in the process for the production of metallic however that other sources of titanium may be used, 10 titanium described above. such as, TiF4. A major disadvantage of TiF4 is that it In an alternative process, water and optionally base is reacts readily with atmospheric moisture to form hy added to the metal fluoride compound dissolved in the drogen fluoride and is difficult and dangerous to handle, organic solvent in step a) to produce a hydrated metal whereas Na2TiF6 and K2TiF6 are stable in moist air and oxide. safe and easy to handle. 15 The hydrated metal oxide product from the alterna We have now developed a process for the safe and tive process may be treated to produce a metal oxide easy conversion of TiF4 to K2TiF6 or Na2TiF6. In its pigment or a refractory ceramic.
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