The treatment of industrial wastewater is crucial for recovering water of high purity, especially considering its significance in mitigating environmental pollution and ensuring sustainable water resources. This study focuses on the purification of industrial wastewater, emphasizing the separation of tetrahydrofuran (THF) from aqueous solutions using membrane-based techniques. Composite membranes incorporating magnetic nanomaterial (magnetite) within a sodium alginate matrix were synthesized and evaluated for their effectiveness in purifying water from THF mixtures. Both Pervaporation (PV) and Vapor Permeation (VP) processes were employed, with thorough analysis conducted on the impact of magnetite content on permeate purity. The study identified optimal magnetite content for industrial wastewater treatment and developed a new membrane composition based on these findings. The VP process’s performance was evaluated by determining the permeation flux and separation factor. The highest separation factor of 460 was obtained for an 80% wt. THF-water solution in the VP process. Using these findings, the optimal magnetite content for industrial wastewater treatment was identified, and a new membrane composition was developed. The activation energies for the permeation of THF through the NaAlg-Fe20 membrane were found to be 10.50 kcal/mol and 7 kcal/mol for the VP and PV processes, respectively.