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A facile and novel method was developed to fabricate silica-based hierarchical porous Janus microcapsules (HPJMs SiO) for catalysis. The resulting Au@HPJMs SiO nanocomposites showed enhanced catalysis, great stability, convenient recovery and reuse without losing catalytic efficiency.

Constructing three-dimensional (3D) hierarchical materials with spatial compartmentalization of multiple catalytic functionalities effectively facilitates the chemical processes’ intensification, especially for bulky-molecule-involved cascade reaction. Herein, a facile and novel core–shell colloidal crystal templating strategy was developed to synthesize highly ordered arrays of integrated yolk–shelled nanoreactor consisting of monolithically interconnected ZIF-8 shell and sulfonated polystyrene yolks decorated with rhodium nanoparticles. The obtained nanoreactor achieves efficient catalytic one-pot cascade Knoevenagel condensation-hydrogenation reactions for larger molecules, by taking advantage of the superior mass diffusion properties of the hierarchical macro/microporous metal–organic framework (MOF) skeleton, robust monolith nature, and spatially separated functionalities. This work offers an important strategy for preparing MOF-based composites with a hierarchical framework, accelerating various applications of MOFs, such as electrochemical applications, photothermal conversion, and heterogeneous catalysis.