In this work, magnetic zirconium oxide (ZrO 2 /Fe 3 O 4) nanocomposites were synthesized in different mass ratio as (1:1), (3:2), (5:2) and (7:2) and fairly characterized by various techniques like; X-ray diffraction, X-ray energy dispersion analysis, scanning electron microscope, transmission electron microscopy, Fourier transform infrared spectroscopy, and vibrating sample magnetometer. Characterization results showed the prepared nanocomposite had stable core/shell structure in nanometer scale, 12 nm, with magnetically property that nominate it for catalytic application in chemical reactions. The prepared nanocomposites were evaluated in the reduction reaction of methylene blue and in the presence of NaBH 4 as a catalyst. Observed results revealed that the ZrO 2 /Fe 3 O 4 nanocomposites in mass ratio as 5:2 exhibited remarkable catalytic activity with excellent reusability. Obtained results are presented and discussed here.