The separation of sulfur dioxide by a new environmentally friendly method through its sulfur reduction was investigated. Nickel catalyst was synthesized on two bases of alumina and activated carbon, using a wet impregnation method. Both catalyst series in two combinations of different percentages of nickel metal were synthesized and characterized and their performance in the reactor test in terms of conversion rate and selectivity for the desired product was compared. The effect of reaction temperature was investigated in the range of 550-800 °C. At low temperatures, activated carbon-nickel catalysts have better performance than the alumina-nickel catalyst. The effect of the molar feed ratio of SO2/CH4= 3-1 was studied and the stoichiometric feed ratio showed the best performance. Also, the investigation of reaction time for catalysts showed good long-term stability for SO2 reduction with methane in 8 hours. Keywords: SO2 reduction to sulfur, Separation of Sulfur Dioxide pollutant, Alumina-nickel catalyst, active carbon-nickel catalyst, catalyst, and reaction.