This study provides a thorough examination of the utilization of hydrophobic deep eutectic solvents (HDESs) for the extraction of 1,2-dichloroethane (1,2-DCA) from effluent, with an emphasis on a sustainable and environmentally friendly approach. The extraction efficacy of six HDES systems was initially evaluated, and the combinations of thymol/camphor (Thy/Cam) and menthol/thymol (Men/Thy) exhibited superior performance. Subsequently, these two HDESs were chosen for a comprehensive parametric analysis. The impact of contact time demonstrated that extraction equilibrium was reached at 15 min for both systems, thereby achieving a balance between high efficiency and time efficiency. Next, the impact of the HDES-to-water mass ratio was investigated. A 1:1 ratio was determined to be the most effective, as it minimized solvent consumption and provided high efficiency. An additional examination of the molar ratios of the HDES components revealed that the 1:1 ratio exhibited the most effective extraction performance. This was due to the fact that imbalances in the solvent mixture resulted in diminished efficiency as a result of disrupted molecular interactions. The extraction efficiency was significantly influenced by the initial concentration of 1,2-DCA, with higher concentrations resulting in superior results as a result of the increased mass transfer driving forces. In general, the Men/Thy and Thy/Cam systems have shown noteworthy stability and efficiency under different conditions, which makes them highly suitable for large-scale applications.