Potassium ferrate(VI) (K2FeO4) was successfully synthesized via improved chemical dry oxidation method using sodium peroxide (Na2O2) and ferric oxide (Fe2O3) and the product was characterized by ICP, XPS, XRD, FTIR, UV/VIS and SEM. The experimental results indicated that the synthesized potassium ferrate(VI) had an orthorhombic crystal structure space group, D-2h. The yield of the synthesized K2FeO4 was 26.7 % (calculated according to Fe) and the purity of the potassium ferrate(VI) reached to 98.7 %. The degradation tests of methyl orange (25 mg/L, 40 mL) were also performed in this work. The results showed that azo organic pollutants, such as methyl orange, could be effectively degraded by K2FeO4.