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Heavy metals in water are critical global environmental problems. In particular, the anionic heavy metal chromium (Cr) has carcinogenic and genotoxic risks on human health. To this end, an ultralight and flexible nanofibrillated cellulose (NFC)/chitosan (CS) aerogel was developed only by freeze-drying combined with physical thermal cross-linking for efficient one step co-removal of Cr(VI) and Cr(III). The maximum adsorption capacity of Cr(VI) and total Cr calculated according to the Langmuir model was 197.33 and 134.12 mg/g, respectively. Even in the presence of competing soluble organics, anions and oil contaminants, the resulting NFC/CS-5 aerogels showed excellent selectivity. The aerogel exhibited outstanding mechanical integrity, remaining intact after 17 compressions in air and underwater. Meanwhile, after 5 adsorption-desorption cycles, the aerogel was easy to regenerate and maintained a high regeneration efficiency of 80.25%. Importantly, self-assembled NFC/CS-5 aerogel filter connected with the peristaltic pump could purify 752 mL of industrial wastewater with Cr(VI) pre-concentration capacity of 49.71 mg/g. XPS and FT-IR verified that electrostatic interactions, reduction and complexation acted as the main driving forces for the adsorption process. Moreover, such aerogel possessed broad application prospects for alleviating heavy metal pollution in agriculture. [Display omitted] • An ultralight & flexible nanofibrillated cellulose/chitosan aerogel was synthesized. • The maximum adsorption capacities of Cr(VI) and total Cr were 197.33 and 134.12 mg/g. • Aerogels exhibited superior antifouling, selectivity and recyclability. • Self-assembled aerogel filter could purify 752 mL of industrial wastewater. • Adsorption coupled reduction and chelation mechanism was revealed by FTIR and XPS. [ABSTRACT FROM AUTHOR]