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Structural Analysis of Alfa Grass (<i>Stipa tenacissima</i> L.) Lignin Obtained by Acetic Acid/Formic Acid Delignification
Alfa grass lignin obtained by the acetic acid/formic
acid/water CIMV pulping process was characterized by FTIR and <sup>1</sup>H, <sup>13</sup>C–<sup>1</sup>H 2D HSQC, and <sup>31</sup>P NMR spectroscopies. Lignin samples purified by further dissolution/precipitation
or basic hydrolysis steps were also analyzed. The CIMV alfa lignin
is a mixture of low molar mass compounds (<i>M</i><sub>n</sub> = 1500 g/mol) of <b>SGH</b> type with β-O-4 ether bonds as the major
interunit linkage. The crude lignin contains fatty acids and residual
polysaccharides. It also contains large amounts of acetate and hydroxycinnamates,
mostly in the γ-position of β-O-4 interunit linkages.
Although partial acetylation induced by the process cannot be excluded,
the absence of aromatic acetates and acetylated polysaccharides in
crude lignin demonstrates the mildness of the process. By combining
smooth alkaline hydrolysis and dissolution/precipitation steps to
the CIMV pulping, it is possible to produce a purified lignin with
a composition and a structure quite analogous to that of the native
polymer in the plant