The nickel metal hydride batteries (Ni-MH) are used in many electronic equipment, like cell phones, computers, cameras as well as hybrid cars. Spent batteries can be a rich source of many metals, especially rare earth elements (REE), such as lanthanum (La), cerium (Ce), neodymium (Nd), praseodymium (Pr), samarium (Sm), gadolinium (Gd). Ni-MH batteries also contain iron (Fe) as well as non-ferrous metals, i.e. nickel (Ni), cobalt (Co), zinc (Zn), manganese (Mn), etc. Leaching of such waste with sulfuric acid solutions is one among many methods recovering of useful metals in hydrometallurgical processes. The main aim of this work was separation of metal ions from pregnant leach liquor (PLL) by solvent extraction using phosphorous compounds and ionic liquids (ILs). The initial pH of the aqueous solution was 0.1. Di (2-ethylhexyl) phosphoric acid (D2EHPA), bis (2,2,4-trimethylpentyl) phosphinic acid (Cyanex 272), and phosphoniumionic liquid – trihexyl (tetradecyl) phosphonium bis (2,4,4-trimethylpentyl) phosphinate (Cyphos IL 104) were used as the selective extractants. The initial concentration of the extractants in an organic phase was equal to 0.1 mol∙dm−3. The obtained results show that the highest extraction efficiency was obtained for Fe(III) and Zn(II) in extraction experiments with 0.1 M D2EHPA at pH of 0.1. Ni(II), Co(II) and REE remained in the aqueous solutions. In the next stage, REE were extracted with the mixture of 0.1 M Cyanex 272 and 0.1 M Cyphos IL 104 at pH equal to 3.8. Finally, Ni(II) and Co(II) ions were efficiently removed from the aqueous phase using 0.1 M solution of Cyphos IL 104 at pH around 5.4.