Analytical Pyrolysis Pathways of Guaiacyl Glycerol-β-guaiacyl Ether by Py-GC/MS
Analytical Pyrolysis Pathways of Guaiacyl Glycerol-β-guaiacyl Ether by Py-GC/MS
复制标题
Py-GC/MS 分析愈创木基甘油-β-愈创木基醚的热解途径
DOI：
10.15376/biores.11.3.5816-5828
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发表时间：
2016-08-01
期刊：
影响因子：
1.5
通讯作者：
Lucia, Lucian A.
中科院分区：
文献类型：
--
作者：
Liu, Yu;Liu, Yu;Lucia, Lucian A.
以愈创木酚为原料，经5步反应，合成了β-O-4结构的木质素模型化合物愈创木基甘油-β-愈创木基醚。该合成方法的关键步骤是4-（α-溴乙酰基）-愈创木酚（III）与愈创木酚（I）的缩合反应。通过核磁共振氢谱（H-1-NMR）和二维核磁共振（2D-NMR）对化合物进行了表征。采用裂解-气相色谱/质谱联用技术（Py-GC/MS）研究了愈创木基甘油-β-愈创木基醚的裂解行为。研究了愈创木基甘油-β-愈创木基醚热解过程中的热行为和主要挥发性碎片的演化规律。愈创木酚是C-β-O在低温下均解的主要产物。C-beta-O均裂和C-beta-O协同分解在中等温度下发生，产生愈创木酚、2-羟基苯甲醛、2-甲氧基苯甲醛和各种酚类化合物。在高温下，C-β-O均解和C-β-O协同分解产物发生二次热裂解，生成大量小分子产物，增加了热解产物的复杂性。
A synthetic method for obtaining a lignin model compound of beta-O-4 structure, guaiacyl glycerol-beta-guaiacyl ether, was researched through five reaction steps from guaiacol. The key step of this synthetic method was the condensation reaction between 4-(alpha-bromoacetyl)-guaiacol (III) and guaiacol (I). The compounds were characterized by H-1 nuclear magnetic resonance spectroscopy (H-1-NMR) and two-dimensional nuclear magnetic resonance (2D-NMR). Pyrolysis behaviors of guaiacyl glycerol-beta-guaiacyl ether were investigated by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). The thermal behavior and the evolution profiles of major volatile fragments from the guaiacyl glycerol-beta-guaiacyl ether pyrolysis were evaluated. Guaiacol is the major product through C-beta-O homolysis at low temperatures. C-beta-O homolysis and C-beta-O concerted decomposition occurred at moderate temperatures, producing guaiacol, 2-hydroxybenzaldehyde, 2-methoxybenzaldehyde, and various phenolic compounds. At high temperatures, the products obtained from C-beta-O homolysis and C-beta-O concerted decomposition experienced secondary thermal cracking, generating a large number of small molecule products, which increased the complexity of the pyrolytic products.