| 1. |
- Alves, Luis, et al.
(författare)
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Dissolution state of cellulose in aqueous systems. 1. Alkaline solvents
- 2016
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Ingår i: Cellulose. - : Springer Science and Business Media LLC. - 0969-0239 .- 1572-882X. ; 23:1, s. 247-258
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Tidskriftsartikel (refereegranskat)abstract
- The understanding of the state of dissolution of cellulose in a certain solvent is a critical step forward in the development of new efficient solvent systems for cellulose. Nevertheless, obtaining such information is not trivial. Recently, polarization transfer solid-state NMR (PTssNMR) was shown to be a very promising technique regarding an efficient and robust characterization of the solution state of cellulose. In the present study, combining PTssNMR, microscopic techniques and X-ray diffraction, a set of alkaline aqueous systems are investigated. The addition of specific additives, such as urea or thiourea, to aqueous NaOH based systems as well as the use of an amphiphilic organic cation, is found to have pronounced effects on the dissolution efficiency of cellulose. Additionally, the characteristics of the regenerated material are strongly dependent on the dissolution system; typically less crystalline materials, presenting smoother morphologies, are obtained when amphiphilic solvents or additives are used.
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| 2. |
- Alves, Luis, et al.
(författare)
-
Dissolution state of cellulose in aqueous systems. 2. Acidic solvents
- 2016
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Ingår i: Carbohydrate Polymers. - : Elsevier BV. - 0144-8617 .- 1879-1344. ; 151, s. 707-715
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Tidskriftsartikel (refereegranskat)abstract
- Cellulose is insoluble in water but can be dissolved in strong acidic or alkaline conditions. How well dissolved cellulose is in solution and how it organizes are key questions often neglected in literature. The typical low pH required for dissolving cellulose in acidic solvents limits the use of typical characterization techniques. In this respect, Polarization Transfer Solid State NMR (PT ssNMR) emerges as a reliable alternative. In this work, combining PT ssNMR, microscopic techniques and X-ray diffraction, a set of different acidic systems (phosphoric acid/water, sulfuric acid/glycerol and zinc chloride/water) is investigated. The studied solvent systems are capable to efficiently dissolve cellulose, although degradation occurs to some extent. PT ssNMR is capable to identify the liquid and solid fractions of cellulose, the degradation products and it is also sensitive to gelation. The materials regenerated from the acidic dopes were found to be highly sensitive to the solvent system and to the presence of amphiphilic additives in solution.
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