Pure and Mo doped ZrW 2 O 8 compounds have been synthesised by a sol-gel process. The structure, morphology and properties of as synthesised samples have been investigated using X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, UV-Vis spectrometer and photoluminescence. The analysis results reveal that the crystal structure, morphology, band gap and photocatalytic activity of ZrW 2 − x Mo x O8 compounds can be tuned by changing the Mo doping content. When compared with pure ZrW 2 O 8 , the substitution of Mo in different doping ratios narrows the band gap energy. The photocatalytic activity of the samples is evaluated by the degradation of rhodamine B, indicating that the photocatalytic activities of ZrW 2 − x Mo x O8 compounds depend on the Mo doping content. The incorporation of Mo dopants can modify the electronic structure of ZrW 2 O 8 and prohibit the recombination of photo-induced charge carriers. ZrWMoO 8 has the greatest photocatalytic activity, and it displays good stability during the photocatalytic and recycling processes.