The recovery of osmium from residual osmium tetroxide (OsO4) is a necessity imposed by its high toxicity, but also by the technical-economic value of metallic osmium. An elegant and extremely useful method is the recovery of osmium as a membrane catalytic material, in the form of nanoparticles obtained on a polymeric support. The subject of the present study is the realization of a composite membrane in which the polymeric matrix is the polypropylene hollow fiber, and the active component consists of the osmium nanoparticles obtained by reducing an alcoholic solution of osmium tetroxides directly on the polymeric support. The method of reducing osmium tetroxide on the polymeric support is based on the use of 10-undecenoic acid (10–undecylenic acid) (UDA) as a reducing agent. The osmium tetroxide was solubilized in t–butanol and the reducing agent, 10–undecenoic acid (UDA), in i–propanol, t–butanol or n–decanol solution. The membranes containing osmium nanoparticles (Os–NP) were characterized morphologically by the following: scanning electron microscopy (SEM), high-resolution SEM (HR–SEM), structurally: energy-dispersive spectroscopy analysis (EDAX), Fourier transform infrared (FTIR) spectroscopy. In terms of process performance, thermal gravimetric analysis was performed by differential scanning calorimetry (TGA, DSC) and in a redox reaction of an organic marker, p–nitrophenol (PNP) to p–aminophenol (PAP). The catalytic reduction reaction with sodium tetraborate solution of PNP to PAP yielded a constant catalytic rate between 2.04 × 10−4 mmol s−1 and 8.05 × 10−4 mmol s−1.