Abstract: A process for pre-treating a spent caustic stream prior to oxidation which includes countercurrent multi-stage elevated temperature solvent extraction of dissolved organic material from the spent caustic using a solvent to yield a spent caustic raffinate containing only residual amounts of organic solute and steam distilling the spent caustic raffinate to remove the residual organic solutes, yielding a pretreated spent caustic stream substantially free of organic material which is then subjected to wet air oxidation and thereafter to ozonolysis to yield a wastewater stream having a low COD and BOD, which is neutralized to a pH of 8.5 to 9.0.