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Metal organic framework (MOF) has been paid great attention as a potential candidate for various applications in the field of energy and environment, particularly in air purification. Among various MOFs, MIL-101(Fe) represents an interesting material possessing many advantages, including the ease of fabrication, high porosity, high specific surface area with open metal sites, making it a promising material in the field of harmful gas treatment. Taking these advantages, MIL-101(Fe) was synthesized by facile microwave-solvothermal method and applied as a photocatalyst for the degradation of NOx. The de-NOx e?ciency of the synthesized powder was evaluated with respect to various operating parameters including substrates, sample doses, light spectrum and light intensity, initial NO concentration, and relative humidity. The results have shown that the e?ciency of NOx photocatalytic degradation reaches to 77％ under solar irradiation via 0.1 g of MIL-101(Fe) with optimum condition of reaction, (alumina substrate, 350 ppb of initial NO concentration, 40–50％ of relative humidity). Then this work provides the optimum condition for the e?cient photocatalytic degradation of NOx.