Different titration methods were applied with the purpose to determine the dissociation properties of a natural (cotton) and regenerated (viscose, modal and lyocell) cellulose fibers. Potentiometric and conductometric titration were used to determine the content of acidic groups. pK values were determined by potentiometric titration. Polyelectrolyte adsorption was used for surface and total charge determination, and to obtain information about charge location and accessibility of charged groups. It was found that the average content of acidic groups is higher in cotton fibers than in regenerated fibers. The fiber charge of cotton is due to the dissociation of two type of acidic groups, one with pK Ϸ3.5 and the other with pK Ϸ5.5. In regenerated fibers there is only one type of acidic groups (pK Ϸ3.5). The pK value of the stronger acid is typical for carboxyl group in uronic acids. The polyelectrolyte adsorption indicates that most of the carboxyl groups are located in an inner region of all cellulose samples (cotton and regenerated fibers). It is concluded that titration methods are powerful tools for monitoring the content, strength, and distribution of acidic groups, as well as the total charge of natural and regenerated cellulose fibers. The three methods give similar results on all analyzed samples and show good repeatability. The results of investigation make it quite clear that combination of all titrations yields relevant information about content and strength of acidic groups in both natural and regenerated cellulose fibers used in the manufacture of textiles.
The oxidation reaction of regenerated cellulose fibers mediated by N-hydroxyphthalimide (NHPI) and various cocatalysts at room temperature for different time intervals and various amounts of low concentration sodium hypochlorite solution has been investigated to produce oxidized cellulose (OC), a biocompatible and bioresorbable polymer. The results revealed that the nonpersistent phthalimide-N-oxyl (PINO) radical generated in situ from NHPI in both, metallic or metal-free systems, is a powerful agent in this kind of transformation. Moreover, the reaction converts highly selectively C(6) primary hydroxyl groups to carboxylic groups under mild reaction conditions and shorter reaction times than previously reported. The amounts of negatively charged groups in OC were determined by means of potentiometric titration. Further characterization of the products were accomplished by using Fourier transform infrared spectroscopy/attenuated total internal reflection spectroscopy (FT-IR/ATR), environmental scanning electron microscopy (ESEM), and X-ray and energy-dispersive X-ray (EDX) spectroscopy. Notably, water retention values of the oxidized fibers increased by 30% in comparison with the original nonoxidized sample, as a result of the introduction of hydrophilic carboxylate groups.
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