Using the heterometallic oxo-centered trinuclear [ ZnFe2O(CH3COO)6(H2O)3]·2H2O complex as a novel precursor, pure and single-phase ZnFe2O4 nanostructure was prepared under microwave irradiation [abbreviated as ZnFe2O4 (MW)] within a very short time of 10 min. Also, ZnFe2O4 nanostructure [abbreviated as ZnFe2O4 (CT)] was produced by the conventional thermal method of this precursor. The characteristics of ZnFe2O4 nanostructures were compared by XRD, SEM, EDS, FT-IR, VSM, DRS and UV–Vis spectroscopy. Both samples revealed a cubic spinel structure with nanosheet morphology and average particle sizes of 40 and 47 nm, respectively. The ZnFe2O4 (MW) nanostructure were used as a novel sonocatalyst for the degradation of methylene blue and rhodamine B with conversions of 95% and 91%, which is up to 40% more than ZnFe2O4 (CT) activity. The higher sonocatalytic activity of ZnFe2O4 (MW) is relevant to its higher porosity and smaller particle size. The trapping experiment results confirmed that the ultrasound assisted catalytic degradation proceeds mainly through ·OH radicals. Further, the ZnFe2O4 sonocatalyst was easily separated by a magnet and reused without significant loss of activity.