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A mixture of aqueous sodium hydroxide and a cosolvent was applied to a polycotton pre-consumer fabric to promote the chemical separation of polyester (PES) and cotton (CO). The feasibility of reusing the hydrolytic solutions was tested, where dimethyl sulfoxide (DMSO) and 2-propanol allowed the reusage of the hydrolytic solution for up to 3 consecutive cycles when applied to pristine material. The recovery of pure terephthalic acid (TPA), after treatment at 50\u00a0\u00b0C followed by vacuum filtration, achieved yields ranging from 65 to 69%. No further purification was required in 75% of the tested conditions. Through this environmentally sustainable procedure, a method was proposed that could facilitate the development of a scalable process for the TPA recovery from polycotton textiles. 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