A silver nanoprism solution was prepared by reacting silver nitrate (AgNO3), trisodium citrate dihydrate (C6H5Na3O7·2H2O), sodium borohydride (NaBH4), and ascorbic acid (C6H8O6) in distilled water. The successful formation of the silver nanoprisms was confirmed by UV–visible spectroscopy considering the 350–400 nm and 600–650 nm wavelength ranges. The C60 fullerene nanowhisker-silver nanoprism composite was synthesized through a liquid-liquid interfacial precipitation (LLIP) method using C60-saturated toluene, the silver nanoprism solution, and isopropyl alcohol and characterized by X-ray diffraction, Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy. Its catalytic activity was assessed for the reduction of 2-nitrophenol by monitoring the reaction through UV–vis spectroscopy. A kinetics study was conducted, which indicated that the C60 fullerene nanowhisker-silver nanoprism composite catalyzed reduction of 2-nitrophenol follows a pseudo-first-order reaction.