Selective solvent extraction of zinc(II) and copper(II) from aqueous acidic chloride solutions by mixture of bis(2,2,4-trimethylpentyl)phosphinic acid (Cyanex 272) and trioctymethylammonium chloride (Aliquat 336) in kerosene has been investigated. Detailed studies have been conducted by varying pH, hydrochloric acid, and chloride concentrations in aqueous phase as well as extractants concentration in organic phase. A full and high selective solvent extraction of zinc(II) over copper(II) from acidic chloride solutions has been achieved by 0.1 M Cyanex 272 and 0.06 M Aliquat 336 in kerosene while efficient Zn(II) stripping has been performed by using 1 M sulphuric acid. The following selectivity coefficients of zinc(II) over Cu(II) (S-Zn/Cu) during their solvent extraction from 1 M NaCl at pH 0.5 by Cyanex 272, Aliquat 336, and their mixture were found to be equal to: 1.7, 62, and 3162, respectively.