<p>Molybdenum–Titanium (Mo–Ti) alloy targets are widely used in large-sized thin-film transistor–liquid crystal displays because of their low weight and excellent diffusion barrier properties. However, the targets utilization rate is typically low, causing significant resource wastage. This study employed a sulfuric acid (H₂SO₄)–hydrogen peroxide (H₂O₂) mixed system to leach spent Mo–Ti targets residue, with tributyl phosphate (TBP) being used as an extractant for selective Mo extraction and recovery. The effects of leaching parameters on the leaching efficiency of Mo and Ti and the effects of extraction, washing, and stripping on the separation of Mo and Ti were systematically studied. In the H₂SO₄–H₂O₂ system, Mo and Ti are effectively leached in the forms of [H₂Mo₂O₃(O₂)₄] and [TiO(H₂O₂)]²⁺, respectively. Owing to the difference in their ionization abilities, the neutral extractant TBP enables the possibility of separating them. Mechanistic studies revealed Mo extraction in the form of the peroxide complex [H₂Mo₂O₃(O₂)₄] with the TBP/Mo = 2/1 complex [H₂Mo₂O₃(O₂)₄][TBP]₂ forming, as verified by Fourier transform–infrared analysis and slope analysis. In contrast, the Ti formed the cationic complex [TiO(H₂O₂)]²⁺, which remained unextracted. The mass ratio of Ti/Mo was reduced from 0.5 in the raw material to 7.97 × 10⁻⁶ in the stripping solution, achieving efficient separation of Mo and Ti. The Ti content at this point meets the requirements for producing grade 0 ammonium molybdate (MSA-0) specified in Chinese standards. The proposed process provides an efficient solution for strategic metal resource recovery from electronic waste.</p> Graphical Abstract <p></p>