Electrolyte recovery is seldomly considered in state-of-art lithium-ion battery recycling methods but rather evaporates and decomposes uncontrolled during the pre-treatment steps. However, controlled and safe removal of the electrolyte is inevitable and of high importance to the recycling industry to minimize the environmental impact of the recycling processes by preventing severe threats produced by the inflammable, toxic and hazardous components of the electrolyte. This study investigated the effects of temperature and process time of a low temperature thermal treatment process on electrolyte recovery. The process exhaust gases and recovered products were analyzed by In-Situ Fourier-transform infrared spectroscopy (FT-IR) and gas chromatography-mass spectrometry (GC–MS) to determine the effectiveness of the significant process parameters. The results show that the electrolyte solvents, which are dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), and ethylene carbonate (EC), were successfully recovered for 80 minutes of processing time at 130 ℃. The LiPF6 decomposition products hydrogen fluoride (HF) and phosphoryl fluoride (POF3) were detected in the exhaust gas stream and recovered as acidic solutions. Thermal treatment below 150 ℃ is a promising approach for the recovery of the electrolyte solvents prior to the metal recycling stage due to its simplicity, feasibility, and environmental benefit.