Fundamental Study on Titanium Production Process by Disproportionation of TiCl 2 in MgCl 2 Molten Salt
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1 Kyoto International Forum for Environment and Energy Fundamental Study on Titanium Production Process by Disproportionation of TiCl 2 in MgCl 2 Molten Salt Taiji Oi and Toru H. Okabe Institute of Industrial Science, The University of Tokyo, Japan Kyoto International Forum for Environment and Energy, Dec. 4-7,
2 Titanium Features of Titanium 1. Light and high-strength 2. Corrosion resistance 3. Biocompatibility 4. Some titanium alloys: shape memory alloy super elasticity Titanium is the 9 th abundant element in the earth s crust and the 4 th abundant element for structural material. Kyoto International Forum for Environment and Energy, Dec. 4-7,
3 The Kroll Process Chlorination: TiO 2 + C + 2Cl 2 TiCl 4 + CO 2 Reduction: TiCl 4 + 2Mg Ti + 2MgCl 2 Electrolysis: MgCl 2 Mg + Cl 2 Overall reaction: TiO 2 + C (+ ) Ti + CO 2 Huge exothermic reaction for the reduction Reduction rate is extremely slow. Batch type process e.g.) 10 days are required for producing 10 ton of Ti. A new production process is urgently required for further expansion of the applications of titanium metal. Kyoto International Forum for Environment and Energy, Dec. 4-7,
4 Flow chart of the proposed new Ti production process Calcined coke Rutile, Upgraded ilmenite Fluidized bed chlorination CO, CO 2 Crude TiCl 4 (+ VOCl x, SiCl 4, SnCl 4 ) This study Scrap Ti Purification of TiCl 4 TiCl 4 (Mg) Production of TiCl 2 TiCl x (+ MgCl 2 ) VOCl x, SiCl 4, SnCl 4 (1) Production of TiCl 2 : TiCl 4 + Ti 2 TiCl 2 TiCl 4 + Mg TiCl 2 +MgCl 2 TiCl 4 Disproportionation of TiCl 2 Ti powder (or Ti on Fe) (+ MgCl 2,TiCl x ) Vacuum distillation MgCl 2 (+ TiCl x ) (2) Disproportionation of TiCl 2 : 3 TiCl 2 Ti (s) + 2TiCl 3 (g) 2 TiCl 2 Ti (s) + TiCl 4 (g) Ti powder (or Ti on Fe) Kyoto International Forum for Environment and Energy, Dec. 4-7,
5 Titanium Production Process by Disproportionation Reactions of TiCl 2 (1) TiCl 2 synthesis process: TiCl 4 (g) + Ti (s, scrap) 2 TiCl 2 (s, l) TiCl 4 (g) + Mg (l) TiCl 2 (s, l) + MgCl 2 (l) (2) Ti production process: 3 TiCl 2 (s, l) Ti (s) + 2TiCl 3 (g) (2) Ti production process : 2 TiCl 2 (s, l) Ti (s) + TiCl 4 (g) Step (1): High-efficient synthesis of TiCl 2 in MgCl 2 molten salt TiCl 4 Scrap Ti Step (2): Ti production by disproportionation of TiCl 2 in MgCl 2 molten salt TiCl 4 TiCl 3 MgCl 2 TiCl 2 Ti MgCl 2 TiCl 2 Kyoto International Forum for Environment and Energy, Dec. 4-7,
6 Features of This Process High purity Ti products with low oxygen Chloride metallurgy Applicable to titanium coating method Utilizing titanium scrap for the feed Slow reaction speed in gas phase reaction Still no efficient synthesis method of high-purity TiCl 2 These problems can be solved by utilizing condensed phase like molten salt as a reaction medium. Purpose of This Study Development of (1) high-efficient TiCl 2 synthesis process (2) Ti production process and/or Ti plating method based on disproportionation of TiCl 2 in molten salt. Kyoto International Forum for Environment and Energy, Dec. 4-7,
7 TiCl 2 Synthesis by Reaction of TiCl 4 with Ti in Molten Salt TiCl 4 (g) + Ti (s) 2 TiCl 2 (in MgCl 2 Molten Salt) Kyoto International Forum for Environment and Energy, Dec. 4-7,
8 Temperature, T / K Quasi-binary phase diagram for the MgCl 2 TiCl 2 system TiCl 2 content, x TiCl2 (mass%) K K L Overall composition before Exp. A and B 989 K? MgCl 2 TiCl 2 content, x TiCl2 (mol%) TiCl 2 Experimental Procedure Solubility at 1273 K : 83 mol% TiCl 2 Overall composition before Exp. C and D [Komarek and P. Herasymenko: J. Electrochem. Soc. 105 (1958) p 210.] Kyoto International Forum for Environment and Energy, Dec. 4-7, Temperature, T / TiCl 4 (l, g) + Ti(s, scrap) 2 TiCl 2 (s, l) TiCl 4 Ti MgCl 2 TiCl 2 MgCl 2 is expected to work as a medium that removes TiCl 2 film formed on the surface of metallic Ti by dissolving it. MgCl 2 accumulates TiCl 2 in its interior.
9 TiCl 2 Synthesis: Experimental TiCl 4 (l, g) flow Stainless-steel tube for TiCl 4 feed Thermocouple (T 2 ) Thermocouple (T 1 ) Heating element Alumina crucible Stainless-steel outer chamber Stainless-steel container Stainless-steel basket Ti sponge 20 mm Experimental temperature, T 1 = 1273 K Ar atmosphere Molten MgCl 2 10 mm Kyoto International Forum for Environment and Energy, Dec. 4-7,
10 TiCl 2 Synthesis: Experimental Results (1) Solidification of the salt Ti sponge residue after experiment (a) (b) (c) (d) (e) Black flake precipitate with green salt 10 mm Kyoto International Forum for Environment and Energy, Dec. 4-7,
11 TiCl 2 Synthesis: Experimental Results (2) Exp. No. (Position) C (a) C (b) C (c) C (d) C (e) D (a) D (b) D (c) D (d) D (e) TiCl 4 feed rate, r (g/min) Table Analytical results of the obtained samples. Ti a Concentration of element i, C i (mass%) Cl b Mg a Fe a < Ni a <0.02 <0.02 <0.02 Cr a x value in TiCl x (28.9) (25.1) (17.7) (17.8) (5.12) a: Determined by ICP-AES. b: Determined by potentiometric titration method. Kyoto International Forum for Environment and Energy, Dec. 4-7,
12 TiCl 2 Synthesis: Experimental Results (3) Table Yield of TiCl x and Ti consumption rate. Exp. No. TiCl 4 feed rate, r / g min -1 Yield of TiCl x, R TiClx (%) Ti consumption ratio, R Ti ' (%) A B C D Direct reaction of TiCl 4 with Ti* Yield of TiCl x : 23~35% Consumption ratio of feed Ti: 42~45% The efficiency of TiCl x formation was improved by using molten MgCl 2 as a reaction medium. * Takeda et al., The 1 st Workshop on Reactive Metal Processing (2006). Kyoto International Forum for Environment and Energy, Dec. 4-7,
13 Titanium Production By Disproportionation of TiCl 2 in Molten Salt 2 TiCl 2 Ti (s) + TiCl x (g) (in MgCl 2 Molten Salt) Kyoto International Forum for Environment and Energy, Dec. 4-7,
14 Disproportionation: Experimental Viton rubber stopper Thermocouple Coolant outlet Coolant inlet Experimental temperature, T= 1273 K Reaction time, t= 3 or 6 h Ar atmosphere Stainless-steel chamber Alumina tube Heating element Nickel crucible MgCl 2 TiCl x 10 mm Ti sponge Kyoto International Forum for Environment and Energy, Dec. 4-7,
15 Disproportionation: Experimental Results (1) Salt in Ni crucible after experiments Black Chip with silver powder 10 mm b-1 from top side b-2 from bottom side (a) (b) Black sintered object coated by gold membrane 10 mm 10 mm Kyoto International Forum for Environment and Energy, Dec. 4-7,
16 Disproportionation: Experimental Results (2) Table Analytical results of the obtained samples. Exp.No. (position) Temp., T / K Time, t / h Mass of salt, w salt /g Ti a Concentration of element i in obtained Ti sample, C i (mass%) Cl b Mg a Fe a Ni a Cr a Initial < Y(a) Y(b) Z(a) < Z(b) < a: Determined by ICP-AES analysis. b: Determined by potentiometric titration method. Calculating the amount of the remaining TiCl 2 Reaction ratio of TiCl x, R TiClx : 73% (3 h) 97% (6 h) Kyoto International Forum for Environment and Energy, Dec. 4-7,
17 Disproportionation: Experimental Results (3) XRD pattern of the sample obtained after leaching After leaching (Exp. Y(b)) (1273 K, 21.6 ks) Intensity, I (a.u.) :α-ti, JCPDS: Angle, 2θ (degree, Cu K α1 ) Pure Ti was successfully obtained. Kyoto International Forum for Environment and Energy, Dec. 4-7,
18 Disproportionation: Experimental Results (4) Table Analytical results of the obtained samples after leaching. Exp.No. (position) Y(a) Y(b) Z(a) Z(b) Time, t / h Concentration of element i in obtained Ti sample, C i (mass%) a Ti Mg Fe Ni Cr a: Determined by X-ray fluorescence analysis (XRF); the value excludes carbon and gaseous elements. Titanium powder with a purity of over 99% was successfully obtained. Kyoto International Forum for Environment and Energy, Dec. 4-7,
19 Conclusions A high-efficient synthesis process for TiCl 2 and a production process for titanium metal were investigated by using reactions in molten salt. The efficiency of TiCl 2 synthesis was improved when using molten MgCl 2 as a reaction medium. The feasibility of the titanium production process by disproportionation of TiCl 2 in molten MgCl 2 was confirmed. Kyoto International Forum for Environment and Energy, Dec. 4-7,
20 Future Works More efficient production process of TiCl 2 from TiCl 4 Clarification of detailed reaction mechanism for producing Ti from TiCl 2 Investigation of titanium coating methods by using disproportionation reactions of TiCl 2 Kyoto International Forum for Environment and Energy, Dec. 4-7,
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