Hendro Sat Setijo Tomo, Mutya Parahita Mahanani, Fathya Putri Fajriani, Nurul Jamilah, Heru Santoso, Dody Andi Winarto, Chandra Liza, Asep Riswoko
ABSTRACT This study introduces a novel interface engineering strategy for high‐performance cellulose/poly (vinyl alcohol) (PVA) aerogels derived from coir fiber waste. To address structural fragility, postsynthesis reinforcement was achieved through conformal liquid epoxy–acrylate infiltration. Quantitative Barrett–Joyner–Halenda (BJH) analysis confirmed the existence of a pore‐wall thickening mechanism that preserved the internal mesoporous network (radius: 1.9–2.6 nm) without interstitial blockage. The functionalized scaffold demonstrated significant thermal stabilization, with the maximum degradation temperature ( T max ) shifting from 283°C to 307°C, coupled with superior mechanical resilience and a bulk density of 0.051 g/cm 3 . Methylene blue (MB) adsorption tests achieved 97.3% removal at pH 10, accurately modeled by pseudo‐second‐order kinetics and the Freundlich isotherm ( R 2 = 0.980, RMSE = 1.507, and Χ 2 = 0.884), indicating spontaneous and endothermic multilayer physisorption. Furthermore, regeneration studies established 70% capacity retention over three cycles while maintaining full macroscopic integrity. These findings indicate that strategic resin infiltration provides a robust and sustainable pathway for the development of durable adsorbents for industrial wastewater remediation.