In this study, we present the first case of applying the MOF⁺ technique for in situ preparation of a hybrid material, namely, Zn-MOF-74@ (Pd@Fe₂O₃). This as-synthesized material can well maintain both the integrity of the framework and porosity. Notably, Zn-MOF-74@(Pd@Fe₂O₃) exhibits outstanding catalytic performance in the hydrogenation reaction of alkene and semihydrogenation reaction of phenylacetylene, thus providing a new guideline for the design of MOF-based hybrid materials for catalytic purpose.