The CSIR is developing a process to produce commercially pure (CP) Grade 4 titanium metal powder via direct metallothermic reduction of TiCl 4. Crude titanium produced by this method is inevitably contaminated with unreacted reducing metal and titanium subchlorides occluded in halide salt. For the product to meet stringent titanium industry quality requirements, the concentration of impurities must be held to acceptably low levels. Acid leaching was identified as a suitable method for purifying the crude reduction mass, due to the solubility of the by-products and the potential for cost-saving provided by this method compared to vacuum distillation. However, purification by leaching poses drawbacks such as high oxygen impurity concentrations in the product, due to the dissolution of subchlorides in water to form insoluble hydroxides and oxychlorides that concentrate on the surface of the titanium powder. The crude titanium was leached under different conditions using water and 1 M and 0.035 M hydrochloric acid at a temperature below 50°C. The 1 M acid leach yielded a product with the lowest oxygen content, demonstrating that when the pH of the media and temperature are controlled, the drawbacks associated with acid leaching can be overcome and the process used successfully for downstream purification of the crude product.

The CSIR-Ti process employs lithiothermic reduction of titanium tetrachloride feedstock to produce titanium sponge. The product is therefore contaminated by a range of lithium and chloride species. In this study we examine the effects of particle size, temperature, and HCl concentration as input leaching variables on the removal of chlorides from the crude titanium sponge. A review of the aqueous chloride chemistry of Li and Ti provided initial conditions for leaching of impurity species from the sponge. Experimental results confirm that the effectiveness of leaching and removal of dissolved impurities from the sponge are dependent on leaching kinetics, which are influenced by temperature, particle size, and morphology. Of the variables tested, reaction temperature had the strongest influence on the oxygen content of the leached product. The HCl lixiviant concentration had a negligible effect under the conditions tested. Leaching of crude titanium sponge (-10 mm size fraction after crushing) at 14°C in either 1 M or 0.032 M HCl yielded a titanium sponge product that met the ASTM standard specification for commercially pure Grade 1 titanium, i.e., oxygen content < 0.18 mass% and chloride content < 0.15 mass%.