Superabsorbent polymers (SAPs) were prepared from carboxymethyl chitosan (CMCS) cross-linked to a gel, concentrated by partial dehydration in a rotary evaporator (at 70, 85, and 100 °C), frozen at −5, −20, and −196 °C, and then freeze dried. A 0.9% aqueous solution of CMCS was gelled by addition of glutaraldehyde and partially dehydrated to 1.3−16.8% dry matter (DM) before freeze drying. The water binding capacity (WBC) of the products was up to 171 g/g of superabsorbent. The best results were obtained when 32−81% of the water in the gel was removed in the evaporator at 85−100 °C, and the concentrated gel (1.3−4.7% DM) was frozen in liquid nitrogen at −196 °C before freeze drying. On average, these SAPs, according to SEM micrographs, had a porous sponge-like structure and absorbed 35 and 32 g/g of saline and urine solutions after 10 min exposure, respectively. The corresponding WBC of two commercial polyacrylate-based SAPs was 34−57 g/g for saline and 30−37 g/g for urine solutions.