Structural Changes of Lignin in the Soda-AQ Pulping Process Studied Using the Carbon-13 Tracer Method

Haitao Yang, Xing Zheng, Lan Yao, Yimin Xie


To reveal the structural changes of lignin during the soda–AQ cooking process and chemical bonds between lignin and xylan of wheat straw, 13C isotope-labeled technology was used in this study. First, 13C isotope-labeled xylose was injected into the living wheat straw. The success of 13C isotope-labeling was confirmed by the results of 13C abundance determination. Then, milled wood lignin-13C was extracted from wheat straw. The wheat straw, which had already been labeled by xylose-13C, was cooked by the soda-AQ process. Soda-AQ Lignin-13C and Residual Lignin-13C were extracted from black liquor and residual pulp. FT-IR, 13C-NMR, and 2D HSQC NMR analyses indicated that all lignin preparations were HGS-type lignin. The main lignin linkages were β-O-4’ units, β-β’ units, β-5’ units, and β-1 units, with the highest content of β-O-4’. Furthermore, 82.8% of β-O-4’ units, 77.2% of β-β’ units, 75.4% of β-5’ units, and 75.4% of β-1 units were degraded during the cooking process. LC bonds between lignin and xylan were at C2 and C5 positions of xylan. It was found that the C-2 position of xylan in wheat straw could be mainly connected to lignin by γ-ester bonds, and C-5 position of xylan in wheat straw was possibly linked with lignin by benzyl ether bonds.


Isotope-labeled; Lignin; Lignin-carbohydrate complexes (LCCs); 13C-NMR; 2D-HSQC

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