In the present study, pristine ZnWO4, CoWO4, and mixed metal Zn0.5Co0.5WO4 were synthesized through the hydrothermal process using a Teflon-lined autoclave at 180 ℃. The synthesized nanomaterials were characterized by various spectroscopic techniques, such as TEM, FTIR, UV–vis, XRD, and SEM-EDX-mapping to confirm the formation of nanocomposite material. The synthesized materials were explored as photocatalysts for the degradation of xylenol orange (XO) under a visible light source and a comparative study was explored to check the efficiency of the bimetallic co-doped nanocomposite to the pristine metal tungstate NPs. XRD analysis proved that reinforcement of Co2+ in ZnWO4 lattice results in a reduction in interplanar distance from 0.203 nm to 0.185 nm, which is reflected in its crystallite size, which reduced from 32 nm to 24 nm. Contraction in crystallite size reflects on the optical properties as the energy bandgap of ZnWO4 reduced from 3.49 eV to 3.33 eV in Zn0.5Co0.5WO4, which is due to the formation of a Z-scheme for charge transfer and enhancement in photocatalytic efficiency. The experimental results suggested that ZnWO4, CoWO4, and Zn0.5Co0.5WO4 NPs achieved a photocatalytic efficiency of 97.89%, 98.10%, and 98.77% towards XO in 120 min of visible solar light irradiation. The kinetics of photodegradation was best explained by pseudo-first-order kinetics and the values of apparent rate const (kapp) also supported the enhanced photocatalytic efficiency of mixed metal Zn0.5Co0.5WO4 NPs towards XO degradation.