The inadequate discharge of effluents from different sources without prior treatment can impact the characteristics of soil and water, which reflect serious environmental problems. Advanced oxidative processes (AOP) appear as a viable alternative for environmental remediation, including wastewater treatment. Herein, α-MoO3 and α-Fe2O3 semiconductors were synthesized at low temperature by a Pechini-based method and then applied in photocatalysis. The catalytic efficiency was performed under visible light toward the degradation of an organic persistent pollutant (Rhodamine B dye, RhB), commonly present in industries wastewater. The results indicated that the synthesized α-MoO3 or α-Fe2O3 photocatalysts presented a pronounced activity and promoted an efficient RhB degradation after 15 min of reaction. α-MoO3 had a degradation efficiency of 93% and 98%, while α-Fe2O3 showed 67% and 100% RhB degradation without and with the addition of H2O2, respectively. These results suggest that the synthesized oxides have high oxi-reductive capacity, which can be used for a fast and effective photodegradation of RhB and other organic persistent pollutants to minimize environmental impacts.