A series of iron-oxide nanoparticles were prepared inside the pores of macroporous resins by in situ forced hydrolysis of Fe3+ ions chemisorbed at the pore walls. The resulting composites were identified with transmission electron microscopy (TEM), UV-visible and near IR spectroscopy and surface photovoltage spectroscopy (SPS). The phase of the resulting iron-oxide panicles embedded in resin was beta-FeOOH. The particles ranged from 2 to 5 nm in size and were spherical in shape. These composites were used in catalysis for hydroxylation of phenol with H2O2. They showed very high hydroxylation activity due to nanosized beta-FeOOH particles inside resins with very little aggregation and also showed easy physical separation due to the polymer matrix. In addition, the acidic environment around the beta-FeOOH particles accelerated their hydroxylation activity.