The Al65Cu20Fe15 (in at.%) rapidly solidified ribbon in the form of brittle flakes was produced by melt-spinning technique. It consists the cell or dendrites of the icosahedral quasicrystalline I-phase surrounded by copper rich cubic τ-Al(Cu, Fe). The pulverized ribbon (fraction <32 μm) was subjected to NaBH4 or 20% aqueous NaOH treatment, which led to the formation of oxide in the form of thin flakes at the outer layer of the powder particles. Test of the catalytic properties of the as spun ribbon and powder before and after treatment was made in the reaction of phenylacetylene hydrogenation. It was shown that for as received ribbon, even at very mild conditions (60 °C, H2 pressure of 5 bar), 40% of phenylacetylene was converted to hydrogenation products with 0.7 styrene/ethylbenzene ratio. The use of pulverized ribbon resulted in improvement of activity, with the same ratio of reaction products. The effect of treatment with NaBH4 led to improvement of the catalyst activity, while strongly alkaline solution of NaOH worsened significantly the catalytic activity, but improved selectivity to styrene (styrene/ethylbenzene=1.2).