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The solvent extraction of scandium by the mixture of di-(2-ethylhexyl) phosphate (D2EHPA) and tri-n-butyl phosphate (TBP) has been investigated in the acidic leaching solution of vanadium slag. Thermodynamic analysis of the species distribution diagrams on the Sc-S-H₂O system showed that scandium mainly exists as Sc³⁺ and Sc(SO₄)⁺, and sulfur mainly exists as HSO₄⁻ in the actual leaching solution of vanadium slag (pH = −0.75). The extraction process was studied to optimize various parameters such as the extractant concentration, dosage of TBP, phase ratio, and stirring speed. The results indicated that 83.64% of scandium and less than 2% of co-extracted elements were extracted under optimal conditions. Then, over 95% of the co-extracted elements and less than 1.1% of scandium were scrubbed from the loaded organic phase by 4.0 mol/L of HCl. Finally, 87.20% of scandium was stripped with 2 mol/L of NaOH and 1 mol/L of NaCl at a stripping O/A of 1:1.