Textile industry is responsible for the main environmental pollution problems as they release undesirable dye effluents which are known to be very toxic and harmful. The Fenton process in degradation azo dye offers the best solution than physical and biological methods except that they generated a large amount of sludge. Recently, high entropy alloy as a new material with equimolar alloys of five or more element present exhibit remarkable catalytic properties. However, the understanding of catalytic action and its stability were not widely discovered yet. Herein, the study FeCoCrNiAlBSi HEAs as a heterogeneous catalyst particularly in Fenton process is studied to provide superior efficiency in degradation of Methyl Orange (MO) by Fenton process.