This study reports the decolorization of an Azo dye (DR16) in a Y-shaped microreactor using Fenton process. The effect of important operation parameters, including dye, H2O2, and Fe2+ concentrations; solution pH; and feed flow rates on the decolorization efficiency under continuous conditions, has been studied. The results showed that at pH values between 3 and 4, more DR16 vanished from feed stream. Moreover, higher decolorization efficiencies were obtained at higher Fe2+ and H2O2 concentrations as well as lower dye concentration and feed flow rate. The results indicated that it is possible to reach an efficiency of 86% for DR16 dye decolorization in just 4.2 s, as residence time, using this microreactor. This was obtained due to efficient reactants mixing in the microreactor mixing point. This study illustrates the advantage of using microreactors for continuous flow decolorization process in the comparison with conventional use of batch stirred tank reactors.