The olive mill wastewater (OMW) treatment process is modeled and optimized through new design of experiments (DOE). The first step of the process is coagulation–flocculation using three coagulants (modeled with the mixture design) followed by photo-degradation (modelled with the full factorial design). Based on this methodology, we successfully established a direct correlation between the system’s composition during the coagulation–flocculation step and the conditions of the photo-catalytic degradation step. Three coagulants are used in this study, Fe³⁺ solution, lime, and cactus juice, and two parameters are considered for the photo-degradation conditions: dilution and catalyst mass. Utilizing a sophisticated quadratic model, the analysis of the two observed responses reveals the ideal parameters for achieving maximum efficiency in coagulation–flocculation and photo-degradation processes. This is attained using a quasi-equal mixture of limewater and cactus juice, exclusively. To achieve an optimal photo-catalytic degradation, it is essential to maintain a minimal dilution rate while employing an elevated concentration of TiO₂. It was found that the experimental tests validations were in good concordance with the mathematical predictions (a decolorization of 92.57 ± 0.90% and an organic degradation of 96.19 ± 0.97%).

This work is dedicated to the study of the effect of the synthesis conditions (drying and calcination) of sulfated zirconia on the final catalytic behavior of bifunctional composite catalysts prepared by the physical mixing of the sulfated zirconia (methanol dehydration catalyst) with Cu/ZnO/Al₂O₃ (CZA; methanol synthesis catalyst). The main objective was to optimize the CZA-ZrO₂/SO₄²⁻ composite catalyst for its use in the direct production of dimethyl ether (DME) from syngas. Sulfated zirconia aerogel (AZS) and xerogel (XZS) were prepared using the sol–gel method using different solvent evacuation conditions and calcination temperatures, while the Cu-ZnO(Al) catalyst was synthesized using the coprecipitation procedure. The effectivity of CZA-ZrO₂/SO₄²⁻ composite catalysts for the direct production of dimethyl ether (DME) from syngas was evaluated in a flow reactor at 250 °C and 30 bar total pressure. The characterization of the sulfated zirconia aerogels and xerogels using different techniques showed that the mesoporous aerogel (AZS_0.5300) exhibited the best textural and acidic properties due to the gel drying under supercritical conditions and calcination at 300 °C. As a result, the composite catalyst CZA-AZS_0.5300 exhibited seven times higher DME production than its xerogel-containing counterpart (364 vs. 52 μmol_DME·min⁻¹·g_cat⁻¹). This was attributed to its well-matched metal surface, mesoporous structure, optimal crystallite size and, most importantly, its higher acidity.