The present study reports homogeneous precipitation method for the preparation of Zn2+ substituted Ni-Co LDH precursors and their subsequent conversion to Ni1−xZnxCo2O4 nanoparticles (NPs) via calcination. Different analytical techniques were used for characterization of the precursors and the Ni1−xZnxCo2O4 NPs. After characterization, catalytic activity of the Ni1−xZnxCo2O4 NPs was investigated towards oxidation of styrene. The effect of reaction time and amount of catalyst on the oxidation of styrene was also investigated. The Ni1−xZnxCo2O4 NPs exhibit better performance as catalyst for the styrene oxidation compared to undoped NiCo2O4 NPs.