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Waste coal fly ash (CFA) cause serious environmental and economic problems because of its adverse effects and increasing cost of its disposal. This fly ash can be re-utilized in different fields like geo-polymerization, as color ingredient in ornamental concrete, soil stabilization and recovery of rare earth metals. Fly ash can be used as a potential candidate for the synthesis of activated carbon, due to the presence of large amount of unburned carbon, which could be further utilized as an adsorbent in various industrial applications. Production of activated carbon from waste material is not only cost effective but also a proficient way out of CFA disposal. In this research, the results will focus on synthesis of activated carbon from coal fly ash by physiochemical treatment. The CFA samples were hydrothermally chemically treated with different ratios of acid mixture comprises of H2SO4 and H3PO4 followed by the physical treatment with CO2 under high temperature in a tubular reactor. Characterization of the synthesized activated carbon was done by using different techniques such as BET (Brunauer–Emmett–Teller), FTIR (Fourier transform Infrared spectroscopy) and RAMAN. The BET results showed that the pore volume increases as the concentration of H2SO4 in the acid mixture increases and highest surface area of 72 m2/g was obtained after physicochemical treatment. The surface energy distribution by modified DFT (Density Functional Theory) was also analyzed as a function of acid mixture for the produced activated carbon. Presence of functional groups on the surface of activated carbon was confirmed by spectroscopic characterization.