Abstract: Pyrolysis and combustion technology is an available method to treat spent organic solvent——intermediate-level radioactive TBP/kerosene. In the process TBP is decomposed into C 4H 8 and P 2O 5 that would corrode equipment and pipes. In order to convert P 2O 5 into calcium phosphate or pyrophosphate, and then separate them from the pyrolysis reactor, calcium hydroxide and emulsifier solutions are added to the TBP/ kerosene to form stable emulsion after intense mixing. The influences of the different parameters, such as emulsifier kind, emulsifier content, DBP content and temperature, etc., in the pure TBP/kerosene-DBP system on the emulsion is studied. The results show that the mixing do not emulsify if the content of DBP is more than 0.4%. The demonstration with the spent TBP/kerosene show that the emulsion is well-distributed. The emulsion is stable in 24 h and can be transported by pump.