Immobilization of metalnanoparticles in hollowfibermembranes via alternating adsorption of polyelectrolytes and negatively charged Au nanoparticles yields catalytic reactors with high surface areas. SEM images show that this technique deposits a high density of unaggregated metalnanoparticles both on the surfaces and in the pores of the hollowfibers. Catalytic reduction of 4-nitrophenol with NaBH4, which can be easily monitored by UV–vis spectrophotometry, demonstrates that the nanoparticles in the hollowfibermembrane are highly catalytically active. In a single pass through the membrane, >99% of the 4-nitrophenol is reduced to 4-aminophenol, but this conversion decreases over time. The conversion decline may stem from catalyst fouling caused by by-products of 4-aminophenol oxidation