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In this work, a simple and sustainable approach is proposed to recover rare earths and iron from an ultrafine NdFeB waste. Rare earths are directly recovered by one-step precipitation in hydrofluoric acid and the dissolved iron by electrodeposition. The rate constant and activation energy of the reaction of rare earth hydroxide with hydrofluoric acid are investigated to understand the kinetics of iron leaching and rare earth precipitation. The rare earth precipitation is much faster than the iron leaching, enabling the rare earths separation from iron after a complete iron dissolution. The cathodic deposits of iron were characterized by X-ray photoelectron spectrometer (XPS) and scanning electron microscope (SEM). The nano-scale FeF2(s) and Fe(s) were deposited on Pt electrode in hydrofluoric acid solution with pH 2.3 and pH 2.89, respectively. The reduction of Fe(III) to Fe(0) was investigated by cyclic voltammetry, chronopotentiometry and open circuit chronopotentiometry. This reduction was a quasi-reversible process which was controlled by diffusion. The temperature dependence of the diffusion coefficient was established as lnD = −9.84 − 1805.43/T and the activation energy value of the diffusion process was calculated to be −15.01 kJ mol−1. The relationship between the Gibbs energy of intermetallic Fe-Pt formation and the temperature was established to be ΔG = −487.53 + 0.936T. The hydrofluoric acid after the electrodeposition could be recycled for the leaching of the ultrafine NdFeB waste again.