Textile production has doubled in the last 20 years, but only 1% is recycled into new fibers. It is the third largest contributor to water pollution and land use, accounting for 10% of global carbon emissions and 20% of clean water pollution. A key challenge in textile recycling is blended yarns, such as polycotton blends, which consist of polyester and cotton. Chemical recycling offers a solution, in particular, alkali treatment, which hydrolyzes polyester (PET) into its components while preserving cotton fibers. However, conventional methods require high temperatures, long durations, or catalysts. Our study presents, for the first time, the heated high-ethanol alkaline aqueous (HHeAA) process that efficiently hydrolyzes PET from polycotton at lower temperatures and without a catalyst. A near-complete PET hydrolysis was achieved in 20 min at 90 °C, while similar results were obtained at 70 °C and 80 °C with longer reaction times. The process was successfully scaled at 90 °C for 20 min, and complete PET hydrolysis was achieved, with a significantly reduced liquid-to-solid ratio, from 40 to 7 (L per kg), signifying its potential to be implemented in an industrial context. Additionally, the cotton maintained most of its properties after the treatment. This method provides a more sustainable and efficient approach to polycotton recycling.