Abstract The use of Titanium-based Metal-Organic Frameworks (MOFs) as substitutes for titanium dioxide in photocatalytic applications is a recent topic of study. A promising approach is to perform a titanium exchange within a zirconium-based MOF to build a material that combines the properties of the two metals, high thermal stability, and photoactivity. In this work, a novel Zr/Ti MOF that incorporated a dioxo-molybdenum (VI) complex was successfully prepared using two post-synthetic steps. First, a molybdenum complex was anchored to a bipyridine-dicarboxylate linker of a UiO-67 type MOF. Second, a Ti4+ ion exchange for Zr4+ at the zirconium MOF nodes was performed. The as-prepared samples were characterized by PXRD, TGA, FT-IR, N2 adsorption, XPS, SEM and UV–vis in diffuse reflectance mode. The introduction of titanium changed the optical properties of UiO-67 adding advantages through the TiO2 moieties attached to its structure. This was attributed to the metal exchange and the formation of oxo-bridged hetero-Zr-Ti clusters with some loss of crystallinity. Additionally, the addressed surface characterization showed that dioxo-molybdenum (VI) and titanium were incorporated into the structure of Zr-MOF with a small decrease in the surface BET area.