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木质素的久万川法和索氏溶剂分级分离：对化学结构的影响

Kumagawa and Soxhlet Solvent Fractionation of Lignin: The Impact on the Chemical Structure.

作者信息

D'Orsi Rosarita, Lucejko Jeannette J, Babudri Francesco, Operamolla Alessandra

机构信息

Dipartimento di Chimica e Chimica Industriale, Università di Pisa, Via Giuseppe Moruzzi 13, I-56124 Pisa, Italy.

Interuniversity Consortium of Chemical Reactivity and Catalysis (CIRCC), Via Celso Ulpiani 27, I-70126 Bari, Italy.

出版信息

ACS Omega. 2022 Jul 11;7(29):25253-25264. doi: 10.1021/acsomega.2c02170. eCollection 2022 Jul 26.

DOI:10.1021/acsomega.2c02170
PMID:35910110
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9330082/
Abstract

We investigated the effects of solvent fractionation on the chemical structures of two commercial technical lignins. We compared the effect of Soxhlet and Kumagawa extraction. The aim of this work was to compare the impact of the methods and of the solvents on lignin characteristics. Our investigation confirmed the potentialities of fractionation techniques in refining lignin properties and narrowing the molecular weight distribution. Furthermore, our study revealed that the Kumagawa process enhances the capacity of oxygenated solvents (ethanol and tetrahydrofuran) to extract lignin that contains oxidized groups and is characterized by higher average molecular weights. Furthermore, the use of tetrahydrofuran after ethanol treatment enabled the isolation of lignin with a higher ratio between carbonyl and other oxidized groups. This result was confirmed by attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), C NMR and two-dimensional (2D) NMR spectroscopies, gel permeation chromatography (GPC), and analytical pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) analysis. Ultraviolet-visible (UV-vis) spectra evidenced the enrichment in the most conjugated species observed in the extracted fractions. Elemental analyses pointed at the cleavage of C-heteroatom bonds enhanced by the Kumagawa extraction.

摘要

我们研究了溶剂分级对两种商业工业木质素化学结构的影响。我们比较了索氏提取法和熊川提取法的效果。这项工作的目的是比较这些方法和溶剂对木质素特性的影响。我们的研究证实了分级技术在改善木质素性能和缩小分子量分布方面的潜力。此外，我们的研究表明，熊川工艺提高了含氧溶剂（乙醇和四氢呋喃）提取含有氧化基团且平均分子量较高的木质素的能力。此外，在乙醇处理后使用四氢呋喃能够分离出羰基与其他氧化基团比例更高的木质素。衰减全反射傅里叶变换红外光谱（ATR-FTIR）、碳核磁共振（C NMR）和二维（2D）核磁共振光谱、凝胶渗透色谱（GPC）以及分析热解-气相色谱-质谱（Py-GC-MS）分析证实了这一结果。紫外可见（UV-vis）光谱证明了在提取级分中观察到的最共轭物种的富集。元素分析表明熊川提取增强了碳-杂原子键的断裂。

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