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In this study, series of nanolayered structures of Zn–Al LDHs were prepared by urea hydrolysis. Nanofibers and nanonets of the Al-doped ZnO were formed via the decomposition of the nanolayers under high pressure and temperature. Nanospheres were also prepared for comparison. The different morphologies of the prepared nanomaterials were confirmed by several techniques. An improvement for the optical properties of the doped zinc oxides was observed through narrowing of their band gap energies because of transforming the nanolayers to nanonets and nanofibers. The photocatalytic activities of the prepared nanomaterials were studied through photocatalytic degradation of the pollutants of acid green dyes. Complete decolorization and mineralization of green dyes happened in the presence of the nanolayers and nanospheres within 4–6 h, while the nanonets and the nanofibers achieved the complete decolorization and degradation of the dyes at shorter time 1.3 h. These results could be explained though the kinetic study of the photocatalytic degradation of dyes. It was concluded that the nanonets and the nanofibers were very effective for the photocatalytic degradation of pollutants.