Abstract. This work establishes a simple method for synthesising layered double hydroxides (LDHs) powders with coprecipitation. The characteristics of the samples were investigated y X-ray diffraction (XRD), scanning electron microscopy (SEM) and spectrophotometer UV-Vis (DRS). Non-uniform distribution was shown for LDHs samples by SEM. Photocatalytic efficiencies were tested using methylene blue (MB) dye as a model contaminant under UV irradiation. In particular, Zn-Al-Ti LDH exhibited an excellent performance towards MB degradation compared with commercial TiO 2 nanoparticles. Methylene blue removal percentage was reached at almost 100%, whereas commercial TiO 2 reached a removal rate of only 66% under the same conditions within 20 min. The aim of the current work is to prepare Zn-Al-Ti layered double hydroxides nanocomposite and to evaluate their photocatalytic activity in the removal of methylene blue under UV irradiation.