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Polyoxometalates (POMs) are a family of promising homogeneous catalysts for various processes. The design of POM-based heterogeneous catalysts, while important for real-world catalysis, is an important topic. Herein, a green and effective mechanochemical assembly strategy was developed to encapsulate the POM inside the ordered mesoporous polymer (OMP) with biomass tannin as the precursor. The strategy was realized by solid-state ball milling of the POM, using 3-aminophenol and tannin with F127 as the template, and removing the template by calcination. The POM-containing materials possessed uniform mesopores (5–10 nm) and high surface areas (150–250 m2g−1). In particular, the H5PM10V2O40-based OMP exhibited good activity (33% conversion and 100% selectivity) and stability (reused in five runs) for the hydroxylation of benzene to phenol. The results of experiments and characterizations demonstrated that the unique confinement structure and the reversible V5+/V4+redox pairs induced by the strong interaction between the OMP and PMoV may account for the good catalytic performance.