This paper reviews two separation methods applying two-step two-liquid flotation for recovering ultra-fine rare earth fluorescent powders (i.e., red, green, and blue). The paper aims to extract the science behind separation by two-liquid flotation, and to provide resulting engineering tips for material recycling. Two-liquid flotation, also called liquid-liquid extraction, involves two solvents (i.e., non-polar and polar solvents) to capture hydrophobic/hydrophobized particles at their interface, and a surfactant to selectively modify the surface property of the target powder(s). For separating a three powder mixture, two different developed flowsheets, composed of two-step separation are discussed. The major difference found was the polar solvents used. The first flowsheet (called the aqueous-organic system) employed water as a polar solvent while the second flowsheet (called the organic-organic system) utilized N,N-dimethylformamide, DMF as a polar solvent. The organic-organic system at the optimized conditions achieved both the grade and recovery of all the separated fluorescent powders at greater than 90% while the aqueous-organic system did not satisfy these criteria. This paper also reviews the mechanism behind the separation, as well as performing a cost comparison between the two methods. The cost comparison indicates that the organic-organic system is a more cost effective method for recovering rare earth fluorescent powders than the aqueous-organic system. Since the size of powders (i.e., several µm) is too small for the application of conventional separation technologies (e.g., froth flotation), two-liquid flotation is a unique pathway for the material recycling of ultra-fine rare earth fluorescent powders.