A value-adding robust and sequential synthetic pathway was elaborated to produce hydrogel structures with ionic character from crude acetylated galactoglucomannan-rich wood hydrolysate (WH). The WH was first-step liquor originating from a sulphite cracking pulp process for dissolving pulp. The synthetically modified WH fractions were verified at each step by NMR and FTIR, and the hydrogels were characterized with respect to their swelling and mechanical properties. Altering the crosslinking chemistry and the content of ionic moieties resulted in hydrogels with various swelling ratios and mechanical properties. Renewable hydrogel formulations with swelling ratios as high as Qeq = 270 were achieved.

A one-pot synthetic methodology for the thiolation of O-acetyl-galactoglucomannan (AcGGM) was developed to merge hemicellulose chemistry with "click" chemistry. This was realized by the AcGGM-mediated nucleophilic ring-opening of γ-thiobutyrolactone via the activation of the polysaccharide pendant hydroxyl groups. The incorporation of thiol functionalities onto the hemicellulose backbone was visualized by 1H and 13C NMR spectroscopy and was assessed by an Ellman's reagent assay of the thiol groups. The versatility of the thiolated AcGGM was elaborated and demonstrated by conducting several postmodification reactions together with hydrogel formation utilizing thiol-ene and thiol-Michael addition "click" reactions. The one-pot synthesis of thiolated AcGGM is a straightforward approach that can expand the applications of hemicelluloses derived from biomass by employing "click" chemistry.