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A Novel Method for Analysis of Xanthate Group Distribution in Viscoses
Author(s) -
Rußler Axel,
Lange Thomas,
Potthast Antje,
Rosenau Thomas,
BergerNicoletti Elena,
Sixta Herbert,
Kosma Paul
Publication year - 2005
Publication title -
macromolecular symposia
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.257
H-Index - 76
eISSN - 1521-3900
pISSN - 1022-1360
DOI - 10.1002/masy.200550513
Subject(s) - xanthate , viscose , lability , chemistry , cellulose , organic chemistry , polymer chemistry , inorganic chemistry
Abstract Analytical monitoring of xanthation in the viscose process along with xanthate group analysis in the viscose material is a long‐debated problem in cellulose chemistry. The task is rendered extremely intricate by the lability of the starting material and the harshness of the reaction medium, which adds to a lack of suitable analytical approaches. In a four‐years' endeavor in our lab, a method is being developed which allows to analyze the distribution of xanthate groups in viscoses relative to the anhydroglucose units and along the cellulose chain. In a first step the xanthate groups are stabilized by alkylation, which was optimized towards quantitative conversion. In a second step, the remaining free hydroxyl groups are protected by carbanilation, followed by selective removal of the stabilized xanthate groups. Steps two and three thus generate an inverse image of the initial xanthate pattern. In the forth and fifth step, the liberated hydroxyl groups are methylated, and the carbanilates are removed, so that in the overall process the xanthates were replaced by methyl groups. All reaction steps have been comprehensively tested with regard to completeness of conversion and orthogonality of the protecting groups.