Materials with photocatalytic and adsorption properties for advanced wastewater treatment targeting reuse were studied. Making use of TiO2 as a well-known photocatalyst, Cu2S as a Vis-active semiconductor, and fly ash as a good adsorbent, dispersed mixtures/composites were prepared to remove pollutants from wastewater. X-ray diffraction, scanning electron microscopy, energy-dispersive X-Ray spectroscopy, atomic force microscopy, band gap energy, point of zero charge (pH(pzc)) and BET porosity were used to characterize the substrates. Phenol, imidacloprid and dichloroacetic acid were used as pollutants for photocatalytic activity of the new photocatalysts. Experiments using the new dispersed powders were carried out at laboratory scale in two solar simulators and under natural solar irradiation at the Plataforma Solar de Almeria, in a Compound Parabolic Collector (CPC) for a comparative analysis of pollutants removal and mineralization efficiencies, and to identify features that could facilitate photocatalyst separation and reuse. The results show that radiation intensity significantly affects the phenol degradation rate. The composite mixture of TiO2 and fly ash is 2-3 times less active than sol-gel TiO2. Photodegradation kinetic data on the highly active TiO2 are compared for pollutants elimination. Photodegradation of dichloroacetic acid was fast and complete after 90 min in the CPC, while after 150 min imidacloprid and phenol removal was 90% and 56% respectively. (C) 2016 Elsevier B.V. All rights reserved.