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Construction of monolithic cryogels that can efficiently adsorb proteins is of great significance in biotechnological and pharmaceutical industries. Herein, a novel approach is presented to fabricate microfibrillated cellulose (MFC)/sodium alginate (SA) cryogels by using freezing-induced oxa-Michael reaction at -12 °C. Thanks to the controllable reactiveness of divinyl sulfone (DVS), cryo-concentrated pH increase activates the oxa-Michael reaction between DVS and hydroxyl groups of MFCs and SAs. The obtained composite cryogel exhibits outstanding underwater shape recovery and excellent fatigue resistance. Moreover, the MFC/SAs reveal a high lysozyme adsorption capacity of 294.12 mg/g, surpassing most of absorbent materials previously reported. Furthermore, the cryogel-packed column can purify lysozyme continuously from chicken egg white, highlighting its outstanding practical application performance. Reuse experiments indicated that over 90% of lysozyme extraction capacity was retained after 6 cycles. This work provides a new avenue to design and develop next-generation chromatographic media of natural polysaccharide-based cryogel for protein purification., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Interconnected macro-porous cryogels with robust and pore-tunable structures have been fabricated using chemically crosslinked microfibrillated cellulose (MFC). Periodate oxidation was initially conducted to introduce aldehyde groups into the MFC surface, followed by the freeze-induced chemical crosslinking via the formation of hemiacetal bonds between aldehyde and hydroxyl at −12 °C. The cryogels with pore-tunable structures and sharply enhanced mechanical strengths were finally achieved by re-assembly of MFCs through soaking in NaIO 4 solution. Furthermore, the MFC cryogels were post-crosslinked by polyethyleneimine (PEI), bestowing the cryogels with the capability of adsorbing anionic dyes. The stress of the PEI-MFC cryogel at the 80% strain was determined to be 304.5 kPa, which is the maximum value for the nanocellulose-based cryogels reported so far. Finally, the adsorption performances of PEI-MFC cryogels for methyl orange (MO) were evaluated. Maximum adsorption capacity of 500 mg/g could be obtained by the Langmuir model, outperforming that of previous absorbent materials. Reuse experiments indicated that over 90% of adsorption capacity was retained after 6 cycles. Continuous clean-up experiments demonstrated excellent MO removal abilities of the PEI-MFC cryogel. This study shows that the novel, green strategy to fabricate the robust cryogel extends the practical applications of nanocellulose adsorbents for environmental remediation. [Display omitted] • A novel strategy of freeze-induced crosslinking and reassembly to fabricate MFC cryogels is developed. • Pore-tunable MFC cryogels exhibit high mechanical strengths, super-elasticity, and shape recovery. • Mechanisms of freeze-induced chemical crosslinking and reassembly of MFCs are explored. • PEI-MFC cryogels show high binding, remarkable reusability, and continuous removal ability for MO. [ABSTRACT FROM AUTHOR]