Extraction of cellulose nanocrystals (CNCs) from wastes is a valuable strategy from the environmental and economical points of view. Herein, a novel and cost-effective method for the preparation of superhydrophobic, environmentally friendly, and recyclable bio-aerogel by freeze-drying the aqueous suspension of CNCs extracted from waste tissue paper and polyvinyl alcohol (PVA) in the presence of hydrolyzed tetraethyl orthosilicate (TEOS) sol has been developed for the first time. The highly porous (98.42 %), ultralow density (0.017 g/cm3), and superhydrophobic (WCA of 154.93◦±4.14) CNCs/PVA/TEOS aerogel can selectively remove oily contaminants from water (BET surface area of 76 m2/g). The aerogel showed a high sorption capacity in the range of 69−168 g/g for 6 oils and 8 organic solvents. The reusability experiments showed the aerogel could maintain more than 92 % of its sorption capacity even after 20 cycles of sorption-squeezing. The cyclic compressive stress-strain tests confirmed the good mechanical properties of the aerogel with 89 % of shape recovery after 50 cycles. The CNCs/PVA/TEOS aerogel can be used as a recyclable sorbent for removing oils/organic solvents from water.

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