TENCEL fiber is a new generation of biocompatible green fiber with excellent flexibility and toughness, and its wet strength is much better than common cotton fibers. In this work, TENCEL fiber was used as the original cellulose fiber. Sodium hydroxide was dissolved in 50% ethyl alcohol solution to prepare a sodium hydroxide solution with a mass fraction of 8%. TENCEL fibers were immersed into the solution at room temperature for 1 h. Then, 10% sodium chloroacetate solution was added, and the mixture was gently stirred in an oil bath at 35 °C for 30 min. Then the temperature was raised and the mixture was stirred at 75 °C for 30 min, 60 min and 90 min, respectively. After the mixture cooled down, the fibers were taken out and washed several times with a 75% ethanol solution containing acetic acid until neutral. Finally, the fibers were dehydrated with absolute ethyl alcohol and dried at 40 °C for 2 h to obtain the carboxymethylated cellulose fibers. According to reaction time, from 30 min to 90 min, the fibers were named CMC1, CMC2, and CMC3 in order.

Calcium chloride solution with concentration of 0.1 mol/L was dropwise added on the surface of CMC until CMC reached a fully swelling state. The CMC and Ca2+ mixture with different mass fractions were added into a 10% PVA aqueous solution to prepare a gel-like mixture. The mixture was stirred and left standing for 30 min to obtain even distribution of the components. Aldehyde (molar ratio of PVA/aldehyde was 1) solution and a small amount of acid were subsequently added to the mixture at room temperature until well mixed. Then, the mixture was foamed through supercritical fluid technology, with supercritical CO2 as the foaming agent. Finally, the foamed mixture was directly placed into molds and underwent vacuum freeze drying. The as-prepared porous composite with different CMC content (5, 10 and 15 wt%) were named as CMCP-1, CMCP-2 and CMCP-3, respectively.

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