Magnetically active nickel doped zinc ferrite nanoparticles with chemical composition NixZn1-xFe2O4 (x- 0.0, 0.25, 0.5, 0.75 and 1.0) were successfully synthesized by sol-gel auto-combustion method using high purity metal nitrates and ethylene glycol as gelling agent. The prepared samples were characterized by X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), X-ray Fluorescence (XRF) and Fourier Transform Infra-Red spectral (FTIR) analyses. TEM images and particle size distribution profile reveals the agglomeration tendency during nickel doping suggest the magnetic nature of particles. The remarkable change in the magnetic behaviour of nickel doped zinc ferrite samples provide an easy recovery and regeneration of the material and thus making an excellent candidate for benzylation reaction without any remarkable fall in the catalytic performance for repeated cycles.