Recently, the ambient drying method for the preparation of xerogels has attracted great attention due to its low cost and high drying efficiency. However, the strong capillary forces existing during ambient drying cause severe shrinkage or even collapse of the aerogels (called xerogels). Although chemical cross-linking or displacement of water by organic solvents have been tried to solve the problem, extensive usage of chemicals and time-consuming displacement processes seem to be environmentally unfriendly and complex. Herein, we reported a green and efficient method for the preparation of a lignocellulosic xerogel. The xerogel was fabricated by alkali freezing of unbleached eucalyptus fibers followed by water washing and ambient drying. The alkali freezing promoted fiber swelling and enhanced the hydrogen bonds among the fibers, resulting in the gelation of lignocellulosic fibers. In particular, the residual lignin in the fibers reduced the capillary force during the drying process. The resulting lignocellulosic xerogel achieved a low shrinkage rate (27.50%), low density (0.039 g cm−3), high porosity (97.57%), and excellent mechanical strength (782.23 kPa) as well as environmental stability, and low thermal conductivity (44.76 mW m−1 K−1). Similarly structured xerogels could be generated using recycled NaOH solution. This technique was suitable for production using various kinds of plant fibers, which shows its great scalable production prospects.
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