Metal organic framework (MOF)-derived nanocatalysts on various nanostructured supports are generally efficient heterogeneous catalysts employable for organic transformations. Herein, nickel Prussian blue (PB) nanoparticles were deployed to form NiFe2O4 nanocatalysts supported on 2D molybdenum disulfide (MoS2) through a facile heat treatment. NiFe2O4 nanocatalysts could be uniformly dispersed on the high-specific-area MoS2 surface, representing a highly efficient, inexpensive, and magnetically recoverable nanocomposite catalyst. The semiconductor property of MoS2 ensures a high electric conductivity, thus enhancing electron transfer between the reductant and the reactant. Furthermore, the strong magnetic characteristics enable its convenient separation from the reaction mixture. NiFe2O4 nanoparticles on MoS2-supported produces multiple electron transfer pathways and overcomes known drawbacks of catalytic methods that use metals alone, endowing long-term cycle stability. Overall, MoS2/NiFe2O4 exhibited an excellent catalytic activity and high yields in the reduction of nitrobenzene in water, maintained even after five cycles. © 2021