The extraction of zinc(II) and iron(II) with solutions of dibutylbutyl phosphonate (DBBP) from hydrochloric acid solutions is studied. Iron(II) is slightly extracted by the considered extractant. The isotherms of zinc(II) extraction with DBBP are compared with those for TBP. They indicate that extraction effectiveness of DBBP as an extractant is higher than for tributyl phosphate (TBP). It is found that the extraction ability of zinc(II) chlorocomplexes from hydrochloric acid solutions decreases with decreasing DBBP content. Addition of kerosene increases hydrophobicity of DBBP at the same time slightly decreasing the efficiency of zinc(II) extraction. 80 vol% DBBP is applied successfully to separate zinc(II) from iron(II) in the following stages: extraction with excess of DBBP (o/w = 5:1), scrubbing of loaded extractant with small amount of water (w/o = 1:5) to remove iron(II), stripping with water to remove zinc(II) from loaded DBBP (w/o = 1:1).