In this study, polyphenols obtained from camu-camu pulp residue were recovered and concentrated from aqueous two-phase flotation (ATPF) by evaluating different operating conditions, such as solvent type, pH, ammonium sulfate concentration, flotation time, air flow, and volumetric ratio. Under optimal conditions, the polyethylene glycol 400/ammonium sulfate ATPF system showed an efficiency of 81.02% and a concentration coefficient two times higher than traditional aqueous two-phase extraction. Experiments were also carried out on a semi-pilot scale, using an apparatus with a 2.5-L working volume. The results showed that the semi-pilot system was comparable to the smaller scale system.