A phosphonium-based bifunctional ionic liquid (IL) Cyp-IL was synthesized to recover molybdenum and vanadium from industrial waste resources, such as the spent hydrodesulfurization catalysts. In comparison with the reported versatile Aliquat 336-based ionic liquid, the developed ionic liquid Cyp-IL was investigated for its potential application recovery of vanadium and molybdenum from industrial wastes. To assess the efficiency of the comparative extraction process, a comprehensive comparison analysis was conducted between the ammonium-based bifunctional ionic liquid Aliquat 336 and the developed phosphonium-based bifunctional ionic liquid Cyp-IL. Vanadium and molybdenum in the ionic liquid-loaded phases were selectively precipitated using NH 4 Cl and BaCl 2 solutions in a basic medium. Compared to Aliquat 336-based Ali-IL, Cyp-IL exhibited superior performance in the extraction and separation processes of molybdenum and vanadium such as a recovery rate of Mo 91% and V 82.5% vs Mo 85% and V 72% by the ammonium-based bifunctional ionic liquid Ali-IL. The recovered components, such as molybdenum and vanadium, were characterized by energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), and scanning electron microscopy (SEM). This method capacitates the sustainable recovery of pure vanadium and molybdenum compounds while minimizing the environmental impact.