A process for recovering quantities of carbonyl compound material from spent solvent-in-water emulsions derived from paint overspray treatment and capture systems in which the spent solvent-in-water emulsion is removed from the paint overspray treatment and capture system and fed into a reaction vessel. The reaction vessel employed includes an outer housing defining a reaction chamber and a plurality of mixing blades movably positioned in the reaction chamber. The surface area of the mixing blades are maintained at a temperature sufficient to generate volatilized carbonyl compound. The interior of the reaction vessel is maintained under a vacuum. The spent solvent-in-water emulsion is processed in the reaction vessel for an interval sufficient to generate volatilized carbonyl compound. The generated volatilized carbonyl compound material is removed from the reaction vessel for recycle and reuse and the residual solid material remaining in the reaction vessel after generation of the volatilized carbonyl compound material is removed. The spent solvent-in-water emulsion which can be treated by the solvent recovery process of the present invention contains carbonyl compounds selected from the group consisting of secondary alcohol esters, secondary alcohol ester derivatives, and mixtures thereof and has a boiling point of at least 150.degree. C., a vapor pressure between about 0.5 Torr at 20.degree. C. The spent solvent-in-water emulsion processed by the carbonyl recovery method can either be previously dewatered to produce a spent solvent-in-water emulsion material with little or no water remaining or can be processed with most or all of the water portion of the emulsion present. In such instances, the water portion may be con-generated with the carbonyl compound.