Iron-doped hydrochar can effectively remove the methyl orange dye (MO). In this study, iron-doped hydrochar (5% Fe@BC) was successfully synthesized through a two-step hydrothermal carbonization (HTC) process, using FeSO4.7H2O and sawdust. It was subsequently employed for MO removal. The characterization of the synthesized Fenton-like catalyst (5% Fe@BC) was conducted, using scanning electron microscopy, Fourier-transform infrared and X-ray diffraction techniques to confirm the presence of iron species. The effects of different operating parameters such as catalyst mass, H2O2 concentration, solution pH, organic pollutant concentration, and reaction temperature have been examined. The Box-Behnken design combined with three factors: catalyst mass X1, temperature X2, organic pollutant concentration X3. The response surface methodology coupled with Box-Behnken Design was used to optimize the key variables and response. With this approach, an exhaustive assessment of the variables influencing the optimization process was performed. A significant quadratic model was generated through analysis of variance with a P-value of 0.0001 and an R2 of 0.99. This confirms a strong relationship between the variables and the response, as well as a high level of model predictability. The optimum conditions were achieved with a catalyst mass of 0.5 g/L, a temperature of 35.5 °C, and an MO concentration of 50 mg/L. The result indicates that 93% of the discoloration efficiency was achieved within 60 min under the optimal conditions. Iron doping in the (5% Fe@BC) plays a crucial role in the degradation and removal of MO. Therefore, the 5% Fe@BC prepared from sawdust and iron salts (FeSO4·7H2O) through a two-step HTC process is an inexpensive and effective catalyst for removing organic pollutant from aqueous solutions, using heterogeneous Fenton-like process.