The new hydrophobic-based deep eutectic solvents (DESs) were prepared from different hydrogen bond acceptors and 1-nonanol as a hydrogen bond donor. The DESs thermo-physical characteristics were investigated, with the variation of temperature results of density, speed of sound, conductivity, viscosity, refractive index, and surface tension. In this work, for the first time, we employed hydrophobic deep eutectic solvents for extraction methyl orange dye in the aqueous solution through the liquid–liquid extraction method. The new hydrophobic deep eutectic solvents based on the tetrapropylammonium bromide and tetraethylammonium iodide showed high extraction efficiency (91–96%) during 15 to 35 min of the extraction process, and other deep eutectic solvents based on the n-dodecyl trimethyl ammonium bromide, benzilic acid, diphenylamine, dioxybenzone do not show such outcome.
