A practical methodology and novel, economical materials were proposed to successfully prepare nano particle catalysts for phenol hydroxylation. The preparation was carried out via mechanical alloying (MA) of CuxSn(100-x)) powder mixtures (where x = 30, 50, 70, and 100%wt). The mechanical alloyed nano particles were characterized using various techniques. X-ray diffraction patterns indicated that eta-Cu6Sn5, epsilon-Cu3Sn, and CuSn phases could be formed in the mechanical alloyed CuxSn(100-x)) materials. Transmission electron micrographs and selected area electron diffraction patterns confirmed the presence of eta-Cu6Sn5, epsilon-Cu3Sn, and CuSn phases. Activity of the catalysts, using the optimal conditions of 70 degrees C reaction temperature for 1 h, 50 mg of Cu0.5Sn0.5, and 1:3 phenol:H2O2 ratio, provided more than 98% conversion with 70% catechol (CAT) and 29% hydroquinone (HQ). Experimental results suggested that the presence of the epsilon-Cu3Sn phase gave higher activity while Sn reduced benzoquinone (BQ) to HQ. The catalyst maintained its stability with no structural collapse for more than 24 h. (C) 2016 Elsevier B.V. All rights reserved.