In this paper, the synthesis of 2,4,6-trinitrophenol from phenol was improved in the range of 0–65°C, and the yield was 79.4%. The effectiveness of the synthesis process was confirmed by Nuclear Magnetic Resonance, Fourier Transform Infrared Spectrometer, and Scanning Electron Microscope. The thermal stability of the product was further studied by differential scanning calorimetry and accelerating rate calorimeter. The kinetic model established by combining linear regression and nonlinear regression methods shows that the apparent activation energy of the energetic material synthesized under the green process is about 130 kJ/mol. [ABSTRACT FROM AUTHOR]