In the present work, PbO-x wt% Al2O3 nanocomposites (where x = 0, 10, 20, 30, 40, 50, 60, 70, and 100 wt%) were prepared by a microwave irradiation method. Their structural parameters, morphology, and chemical bonds, were investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier-transform infrared spectroscopy (FTIR). It was noticed that the produced phases have an orthorhombic crystal structure and the smaller average crystallite sizes were formed when the ratio of Al2O3 is 40 wt%. The FTIR analysis reveals the formation of various bonds between Al or Pb and O. The TEM analysis reveals that the PbO-x%Al2O3 composites (x = 20, 40, and 60), composed of dense particles, and their size are smaller compared to the pure Al2O3 sample. The optical bandgap obeys the direct allowed transition and decreases from 4.83 eV to 4.35 eV as the PbO ratio in the composites increases from 0 to 100%. The intensity of the photoluminescence emission, at the same wavelength, increases as the PbO ratio increases from 0% to 60% implying that increasing the PbO content increases the capacity of free carriers within the trap centers. The prepared composites are used as a catalyst to remove the methylene blue (MB) from the wasted water under UV-visible or visible light irradiations. The photocatalytic degradation of MB was investigated by applying various kinetic models. It was found that the PbO-30% Al2O3, and PbO-40% Al2O3 composites are the best ones amongst other compositions. Furthermore, the pseudo-second-order model is the best model for describing the deterioration mechanism among the models studied. The formed composites could be suitable for the degradation of organic dyes for water purification as well as applications that required a higher optical bandgap.