The aim of this work is to prepare catalysts for energy efficient conversion of polystyrene (PS) and its waste into valuable products with high conversion at 250 °C. The FeCo/Alumina bimetallic catalyst was synthesized by aqueous impregnation and structurally determined using scanning-transmission electron microscopy, temperature programmed desorption, X-ray diffraction, and X-ray photoelectron spectroscopy. Successfully, we have achieved up to 91% liquid yield with selectivities for styrene monomer (SM) up to 45 wt% and ethylbenzene (EB) up to 55 wt%, depending on the exposure time at 250 °C by FeCo/Alumina which is comparable to those of reactions at high temperatures (≥350 °C). Further increase of catalyst loadings from 200 to 400 mg also led to the decrease in styrene yield and increase in ethylbenzene yield. The analysis of the resulting clear liquid by gas chromatography/mass spectrometry (GC/MS) indicates the generation of products in the gasoline range.