A heterojunction of UiO-66 and MoS₂ are fabricated via hydrothermal method and their photocatalytic performance towards methyl red adsorption was investigated. A series of characterizations, such as HRTEM, EDX, XRD, BET, FTIR, were carried out to investigate the synthesis and morphological properties of hybrid materials and confirmed the growth of MoS₂ nanostructures on the surfaces of UiO-66 and its self-assembly as a flower-like structure which efficiently prohibited the photogenerated charge carriers’ recombination. The electrochemical impedance spectra (EIS) are measured to investigate photoelectrochemical behavior. Compared to pure UiO-66 and MoS₂, the flower-like hybrids (UMS 20 %) shown exceptional performance for methyl red degradation under UV-irradiation. the degradation values at different irradiation times were investigated by two concentrations of methyl red 10 and 5 mg/L. UiO-66, MoS₂ and UiO-66/MoS₂ hybrid show high-performance photocatalytic efficiency towards Methyl Red. Cationic methyl red decomposition showed a synergistic effect of the hybrids (UiO-66/MoS₂) on wastewater treatment.