A source of Ti and V found in Brazil contains important content of both elements and has not been explored yet. Such resources would supply the demand for the battery market (Li‐ion and redox flow), robotics, unmanned aerial vehicles, and 3D printers. The hydrometallurgical route is essential to obtain different high purity products. The goal of the present work was to study the HCl leaching of Ti and V from the non‐magnetic fraction of ilmenite‐based ore. The effects of solid–liquid ratio, NaHF2, Fe0, and chloride ions were evaluated. The optimized conditions were the solid–liquid ratio of 1/6–1/12 and NaHF2 of 10 wt.% for 4 h under reducing leaching. Kinetic modelling fitted better for the chemical reaction model. The activation energy was 14.5, 15.4, and 15.5 J/mol for Ti, V, and Fe, respectively. No improvement was obtained as the concentration of chloride ions increased.