This paper discussed the preparation of palladium (PdO) and nickel (NiO) oxides nanoparticles (NPs). These nanoparticle oxides were successfully synthesized by thermal decomposition method using complexes of Schiff base of 4-aminoantipyrine derivative as a precursor at temperature of 800 °C. Schiff base (AEB) was synthesized via a reaction between 4-aminoantipyrine, benzaldehyde and ethylenediamine at stoichiometric 1:1:1 molar ratio at 60 °C for 2 h. The suggested structure of Schiff base was predicted by elemental analyses, 1 Hand 13 C-NMR, FT-IR, UV-Vis, mass, and thermogravimetric (TGA) techniques. The prepared oxides were characterized by Fourier transform infrared spectrometry (FT-IR), powder X-ray diffraction (XRD), and transmission electron microscopy (TEM). From XRD data, the final thermal decomposition products are PdO and NiO with the particle size of 28 and 13 nm, respectively. From the TEM micrographs, the particle size are in good agreement with XRD data and indicate that the products have uniformly spherical particles. The synthesized PdO and NiO oxide nanoparticles were used to removal of the methylene blue (MB) from aqueous solution. Adsorption of MB dye onto the synthesized oxide NPs were performed based on various parameters such as effect of adsorbent dosage, contact time and pH of the pollutant media. The results suggest that the PdO and NiO NPs are excellent adsorbent for the removal of MB dye.