Abstract: Pyrolysis and combustion technology is an available method to treat spent organic solvent——intermediate level radioactive TBP/kerosene. The pilot system with the treatment capacity of 25 kg·h -1 is designed and installed. Influences of technical parameters such as pyrolysis temperature, feeding rate, feed composition, etc, on pyrolysis rate and fixation rate of phosphorus indicate that pyrolysis rate of TBP and fixation rate of phosphorus are more than 99 5 % at given condition, the decontamination factors(DF) of U,Sr and Cs in the whole system are more than 10 6.