In this work, for the first time, CuO/Ti6O13 mesoporous nanocomposite was synthesized by direct intercalation of CuO nanoparticles into hexatitanate layers in the presence of ultrasound. In fact mesoporous potassium hexatitanate with high pore size (44.94 nm) was used as a support. CuO nanoparticles were grown into the titanate pores which caused formation of ultra small CuO with uniform size and high surface area. In fact, titanate is considered as a substrate for better dispersion and nucleation of the CuO nanoparticles which prevented the agglomeration and overgrowth of guest molecules. The prepared sample was characterized by XRD, FE-SEM, TEM, UV–vis spectra, N2 adsorption-desorption, Raman spectra and FT-IR techniques. The product was used as a heterogeneous Fenton-like catalyst for the degradation of Orang G (OG). The effect of important parameters, including pH, H2O2 addition rate and catalyst loading on the decolorization of OG were investigated. Based on the results, CuO/Ti6O13 catalyst exhibited high catalytic activity for OG degradation in aqueous solution at neutral pH of the dye. Moreover, breaking of H2O2 during the catalytic reaction was monitored by pectroscopic method. The results confirmed the decomposition of H2O2 to produce •OH which is the main active species for the degradation of OG.

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