In the present study, ZnO nanostructures were synthesized and immobilized on the surface of diatomite via a simple sonochemical method for the photocatalytic degradation of formaldehyde in the aqueous phase. The characterization of as-prepared ZnO/diatomite nanocomposite was carried out by means of scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FT-IR). The photocatalysis of formaldehyde was favored at neutral pH. At a ZnO to diatomite ratio of 0.3, increasing the photocatalyst dosage from 0.2 to 1.5 g/L resulted in increasing the photocatalytic removal of formaldehyde from 37.51% to 88.05%. At a formaldehyde concentration of 100 mg/L, the complete removal of formaldehyde was attained within the reaction time of 50 min. A mineralization efficiency of 53% was achieved, thereby confirming a suitable mineralization of formaldehyde within the short reaction time of 60 min.