The milk whey is a by-product of the dairy industry with a relevant protein concentration which can be employed as a wall material in spray drying processes. In this work, milk whey was used to encapsulate high oleic palm oil (HOPO) nanoemulsions. The HOPO/whey ratio and the atomization system (two-fluid nozzle and rotary disc) had a significant influence in the capsule formation. In addition, the release of the oleic acid (AO) from HOPO was evaluated by dialysis bag method for powders obtained by both types of atomizers. Different powders were obtained with good physical properties (particle diameter: 6.1–18.8 μm, aw: 0.058–0.125, moisture: 0.86–2.39%, bulk density: 390–770 kg/m3, dissolution rate: 55–115s) from stable nanoemulsions with high encapsulation efficiencies (77 to 99%). On the other hand, the release percents of AO were 82.8 and 75.8% for the two-fluid nozzle and the rotary disc, respectively. The release was not completed in the tested time (7 h) due to stable HOPO-whey linkages, and the gradient that must be broken was higher. Aditionally, an inverse relation was found between diameter particle and AO release.