Sustainability of cellulose dissolution and regeneration in 1,5-diazabicyclo[4.3.0]non-5-enium acetate : a batch simulation of the IONCELL-F process

The recyclability of 1,5-diazabicyclo[4.3.0] non-5-enium acetate ([DBNH][OAc]), as a direct dissolution solvent for cellulose, was evaluated during laboratory scale recycling trials. The main objective was to simulate the conditions of a spinning bath from a Lyocell-type air-gap spinning process, called the IONCELL-F process. The saline solution was then concentrated, recycled and reused as many times as possible before cellulose dissolution was no longer possible. The chemical compositions of the ionic liquid and pulp were recorded throughout the experiments. The results of the experiments showed that [DBNH][OAc] can be recycled from aqueous media with an average recovery rate of 95.6 wt% using basic laboratory equipment, without any further process intensification or optimisation. The recycling of the ionic liquid did not change the chemical composition or degree of polymerisation of the recovered pulp but the colour of the regenerated pulps gradually darkened as the recycling times increased. The ionic liquid was found to hydrolyse 6.0-13.6 mol% per cycle, under these conditions. The build-up of the hydrolysis product, 3-( aminopropyl)-2-pyrrolidonium acetate, killed the dissolution feature at between 30.6-45.6 wt% hydrolysis product. The enzymatic digestibility of the regenerated pulp samples was studied with both a monocomponent endoglucanase and a cellulase mixture. The amount of residual [DBNH][OAc] in the regenerated pulps was determined, by both NMR and capillary electrophoresis. Although hydrolysis of the ionic liquid occurs, this study clearly shows potential for industrial application, with appropriate process equipment and recycling conditions.Peer reviewe

Large-scale production of cellulose-binding domains : adsorption studies using CBD-FITC conjugates

A method for the gram-scale production of cellulose-binding domains (CBD) through the proteolytic digestion of a commercial nzymatic preparation (Celluclast) was developed. The CBD obtained, isolated from Trichoderma reesei cellobiohydrolase I, is highly pure and heavily glycosylated. The purified peptide has a molecular weight of 8.43 kDa, comprising the binding module, a part of the linker, and about 30% glycosidic moiety. Its properties may thus be different from recombinant ones expressed in bacteria. CBDfluorescein isothiocyanate conjugates were used to study the CBD-cellulose interaction. The presence of fluorescent peptides adsorbed on crystalline and amorphous cellulose fibers suggests that amorphous regions have a higher concentration of binding sites. The adsorption is reversible, but desorption is a very slow process.Fundação para a Ciência e a Tecnologia (FCT