Toxic wastewaters from the textile industry have made its way into rivers and other waterways, posing a serious health treat on both human and wildlife. Herein, this data set presents the potential use of MoO3 nanoparticles supported on ZIF-8 in the photodegradation of a cationic dye molecule. The data presented in this article report a concise description of experimental conditions for the spray-dried ZIF-8 synthesis and subsequent deposition of MoO3 nanoparticles via rotary chemical vapor deposition (RCVD). The photodegradation and analysis data reviled that the MoO3-NPs@ZIF-8 3 wt% displayed the ability of degrading methylene blue up to 82% and 95% after 180 and 300 min, respectively.