The Preparation of Iron-Free TiCl₄ from Reduced and Nitrided Ilmenite by Polyethylene Terephthalate

In this study, titanium tetrachloride (TiCl₄) solution was successfully synthesized from titanium oxycarbonitride (TiO_xC_yN_z) by means of chlorination process at low temperatures. Iron-free TiO_xC_yN_z was prepared by carbothermal reduction and nitridation of Ilmenite (FeTiO₃) with coal-75 wt. % PETas a reductant in a H₂/N₂ gas mixture. Aeration leaching via the Becher process for iron removal with NH₄Cl solution was the preferred method for iron removal. The effect of reduction temperature on the synthesis of titanium oxycarbonitride (TiO_0.02C_0.13N_0.85) powder suitable for iron removal has been investigated in the temperature range of 1150–1250°C. The reduced-nitrided ilmenite samples were characterized by XRD and SEM/EDX in terms of phases and morphology. The results showed that iron was formed in spherical and separated particles from TiOCN. Furthermore, the effects of temperature between 350–450°C and soaking time from 1 to 3 hours on the chlorination of iron-free titanium oxycarbonitride have been evaluated. The evaluation was based on design of experiment (DOE) to identify the significant variables on the extent of titanium extraction. DOE analysis based on weight loss validated by ICP tests, indicated a good extraction of titanium and synthesis of TiCl₄ at 450°C.