Unveiling the Structural Heterogeneity of Bamboo Lignin by In Situ HSQC NMR Technique

Wen, Jia‐Long; Xue, Bai-Liang; Xu, Feng; Sun, Run‐Cang

doi:10.1007/s12155-012-9203-5

Cited by 96 publications

(71 citation statements)

References 35 publications

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“…Bamboo biomass primarily consists of Stype and G-type lignin, as well as a small amount of H-type lignin (Lou et al 2010;Wen et al 2012Wen et al , 2013a. In the present study, the BL sample was in overall agreement with published reports, as shown in Table 4.…”

Section: D-hsqc Nmr Spectra Of the Lignin Samplessupporting

confidence: 92%

“…This may have been due to the demethoxylation at the 3-position of G units or the 3,5-position of S units at higher temperatures. Another reasonable explanation for this could be that bamboo is a gramineous biomass and a large amount of PCA is associated with its lignin (Wen et al 2012), which was detected by the 2D-HSQC analysis. As a result, the total phenolic OH evidently increased, which was beneficial for the self-bonding of lignin.…”

Section: D-hsqc Nmr Spectra Of the Lignin Samplesmentioning

confidence: 98%

“…The weight-average (Mw) and number-average (Mn) molecular weights of all lignin samples were determined by gel permeation chromatography (GPC, Agilent 1200 series, Agilent Technologies Inc. USA) with an ultraviolet detector (UV) at 280 nm according to a previous report (Wen et al 2012). NMR spectra were recorded on a Bruker AVIII 400 MHz (Bruker, Germany) spectrometer at 25 °C in DMSO-d6.…”

Section: Characterization Of the Lignin Samplesmentioning

confidence: 99%

“…For the quantitative 2D-HSQC spectra, approximately 90 mg of lignin was dissolved in 0.5 mL of DMSO-d6. Quantitative 31 P NMR spectra were recorded according to published procedures (Yuan et al 2011;Wen et al 2012).…”

Section: Characterization Of the Lignin Samplesmentioning

confidence: 99%

“…As compared to the BL, however, the proportion of G-type and H-type lignin was increased in the PBL1 and PBL2. There are two possible explanations for this result: (1) the AL (S/G/H, 43/25/32) includes a small amount of Htype lignin, which was one of sources for the PBL1 and PBL2 samples isolated from the compound board; or (2) the S-type and G-type lignin could become transformed into H units as a result of demethoxylation (Wen et al 2012). A more interesting result was that the rate of demethoxylation was probably faster in S-type than G-type lignin at higher temperatures.…”

Section: D-hsqc Nmr Spectra Of the Lignin Samplesmentioning

confidence: 99%

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Effect of Lignin on Bamboo Biomass Self-Bonding During Hot-Pressing: Lignin Structure and Characterization

Li¹,

Wu²,

Peng³

et al. 2015

BioResources

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To achieve high value-added utilization of lignin extracted from the biorefinery process in the wood composite industry, binderless particle boards were manufactured by bamboo materials combined with alkaline lignin (AL) in various proportions under various hot-pressing conditions. To elucidate the reactivity and chemical transformations of lignin macromolecules during the hot-pressing process, lignin samples were isolated from the corresponding boards and characterized by highperformance anion-exchange chromatography (HPAEC), gel permeation chromatography (GPC), quantitative 31 P-NMR, and 2D-HSQC NMR. The best bonding strength (1.36 MPa) of the binderless particle boards was obtained under the conditions of 180 °C, pressure 5 MPa, and lignin/bamboo mass ratio 0.4. The molecular weight of the lignin samples decreased from 3260 to 1420 g/mol during hot-pressing. The NMR results showed that the contents of β-O-4' and β-β' linkages were reduced and β-5' linkages were increased as the hot-pressing temperature rose. Simultaneously, the percentage of G-type and H-type lignins as well as the content of phenolic OH increased.

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Section: D-hsqc Nmr Spectra Of the Lignin Samplessupporting

confidence: 92%

Section: D-hsqc Nmr Spectra Of the Lignin Samplesmentioning

confidence: 98%

Section: Characterization Of the Lignin Samplesmentioning

confidence: 99%

Section: Characterization Of the Lignin Samplesmentioning

confidence: 99%

Section: D-hsqc Nmr Spectra Of the Lignin Samplesmentioning

confidence: 99%

See 3 more Smart Citations

Effect of Lignin on Bamboo Biomass Self-Bonding During Hot-Pressing: Lignin Structure and Characterization

Li¹,

Wu²,

Peng³

et al. 2015

BioResources

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Hydrothermal liquefaction of lignin

Dunn

Hobson

2016

Sugarcane‐Based Biofuels and Bioproducts

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Efficient solid‐phase synthesis of acetylated lignin and a comparison of the properties of different modified lignins

Zhao

Huang

Zhang

et al. 2016

J of Applied Polymer Sci

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The chemical modification of lignin can greatly enhance its functionality and exploit its application areas. To avoid the difficulties of separation and environmental pollution in the traditional liquid-phase method, we prepared acetylated lignin by a mechanical-activation-assisted solid-phase synthesis (MASPS) technology with a customized stirring ball mill as a reactor and studied its structure and properties. Ultraviolet-visible analysis showed that the degree of esterification (DE) of the acetylated lignin produced by the MASPS technique was 77.59%, whereas the DEs of those produced by traditional liquid-phase synthesis (LPS) and thermal solid-phase synthesis (TSPS) were only 42.29 and 27.54%, respectively. Fourier transform infrared spectroscopy and NMR analyses indicated that both phenolic hydroxyls and aliphatic hydroxyls participated in the reaction, and the reactivity of the phenolic hydroxyls was higher than that of the aliphatic hydroxyl groups. The acetylation of aliphatic hydroxyl mainly happened at the g of arylglycerol-b-aryl ether (b-O-4). Scanning electron microscopy analysis showed that the acetylated lignins prepared by MASPS and TSPS were irregular blocks with coarse surfaces and loose structures, whereas the lignin prepared by LPS consisted mostly of regular balls with a smooth surface and a compact structure. Differential scanning calorimetry and thermogravimetric analyses indicated that the glass-transition temperatures and thermal stability of the acetylated lignin increased by orders with the processing techniques of MASPS, TSPS, and LPS. MASPS integrated the activation and reaction in the same equipment without the use of a solvent and showed advantages of a high efficiency, environmental protection, and easy operation. V C 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017, 134, 44276.

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Unveiling the Structural Heterogeneity of Bamboo Lignin by In Situ HSQC NMR Technique

Cited by 96 publications

References 35 publications

Effect of Lignin on Bamboo Biomass Self-Bonding During Hot-Pressing: Lignin Structure and Characterization

Effect of Lignin on Bamboo Biomass Self-Bonding During Hot-Pressing: Lignin Structure and Characterization

Hydrothermal liquefaction of lignin

Efficient solid‐phase synthesis of acetylated lignin and a comparison of the properties of different modified lignins

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