Abstract
An integrated approach, based on quantitative transmission mode powder X-ray diffraction (PXRD) combined with multivariate statistical analysis, has been applied to cellulose obtained from three different sources to correlate the mercerization degree and crystallinity with the cellulose type, temperature, and reaction time. The effects of the experimental conditions on the two outcomes were studied by design of experiments (DoE) and surface responding analysis (SRA) combined with principal component analysis (PCA). SRA showed a marked influence of the type of cellulose (wood cellulose from the kraft vs. sulfite process, WCK vs. WCS) on the conversion of cellulose I to cellulose II (CII%) during mercerization. A counterintuitive simultaneous effect of temperature and cellulose type was also highlighted. The data elaboration in the form of response surface plots provided an easy predictive tool for the optimum conditions to maximize the conversion. The simulation reported for WCK showed maximum conversion (96%) at 70 °C in 24 h with 18%wt NaOH.
Highlights
Cellulose, the most abundant polysaccharide in nature, is formed of anhydroglucopyranose (AGU)repeat units linked by β(1→4) glyosidic bonds
To demonstrate the power of the multivariate approach, we have reported the analysis of mercerization involving only wood celluloses WCK and WCS
A set of analytical tools for estimating and improving the efficiency of the mercerization process applied to industrial cellulose samples was presented
Summary
The most abundant polysaccharide in nature, is formed of anhydroglucopyranose (AGU)repeat units linked by β(1→4) glyosidic bonds. The most abundant polysaccharide in nature, is formed of anhydroglucopyranose (AGU). Cellulose can be obtained from several plant fibres and through the delignification of woody plants [1]. It is characterized by a complex supramolecular structure that is known to affect both the reactivity and macroscopic properties of the cellulose polymer [2]. Native cellulose is a mixture of two crystalline forms, Iα and Iβ. Cellulose Iα has a triclinic unit cell containing one chain (P1 space group) and is present in algae and bacteria, while cellulose Iβ has a two-chain monoclinic cell (P21 space group) and is found in higher plants [3].
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