Synthesis of β-O-4-type artificial lignin polymers and their analysis by NMR spectroscopy

Synthesis of β-O-4-type artificial lignin polymers and their analysis by NMR spectroscopy
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DOI:
10.1039/b805460f
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发表时间:
2008-08-21
影响因子:
3.2
通讯作者:
Ubukata, Makoto
Ubukata, Makoto
中科院分区:
化学3区
文献类型:
--
作者:
Kishimoto, Takao;Uraki, Yasumitsu;Ubukata, Makoto

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我们描述了仅含有 β-O-4 子结构的三种人造木质素聚合物的合成和核磁共振波谱分析:紫丁香基型均聚物、对羟基苯基型均聚物和愈创木基/紫丁香基型杂聚物。使用凝胶渗透色谱法,测得三种聚合物的重均聚合度(DPw)为19.2。分别为 38.6 和 13.9。该聚合物是基于愈创木基型均聚物的合成方法制备的,并使用乙酰化和非乙酰化形式的 H-1-、C-13-和 H-1-C-13 NMR 光谱进行了充分表征。愈创木基/紫丁香基型杂聚物的光谱与从日本白桦硬木中获得的磨碎木质素的β-O-4亚结构的光谱非常一致。
We describe the synthesis and NMR spectroscopic analysis of three artificial lignin polymers containing only the beta-O-4 substructure: syringyl-type homopolymer, p-hydroxyphenyl-type homopolymer and guaiacyl/syringyl-type heteropolymer. Using gel permeation chromatography, the weight-average degree of polymerization (DPw) of the three polymers was determined as 19.2. 38.6, and 13.9, respectively. The polymers were prepared based on the synthetic methodology of guaiacyl-type homopolymer, and were fully characterized using H-1-, C-13-, and H-1-C-13 NMR spectroscopy of the acetylated and non-acetylated forms. The spectra of guaiacyl/syringyl-type heteropolymers were in good agreement with those of the beta-O-4 substructure of milled wood lignin obtained from the hardwood of Japanese white birch.