2D NMR characterization of wheat straw residual lignin after dilute acid pretreatment with different severities
-
Anders Jensen
,
Yohanna Cabrera
,
Chia-Wen Hsieh
Abstract
The chemical characteristics of wheat straw lignin pretreated under dilute acid conditions were compared. After pretreatment, the lignin content of the solid residue increased as temperature increased (from 160°C to 190°C) and with the amount of acid added (0%, 0.25%, or 1% H2SO4). Pretreatment at 190°C with increasing concentrations of acid catalyst led to a decrease in glucan content, whereas the glucan content remained almost constant at 160°C pretreatment regardless of the acid concentration. The xylan content decreased in proportion with increased acid concentration and pretreatment temperature. The residual lignins were characterized by solution-state, two-dimensional (2D) nuclear magnetic resonance (NMR) spectroscopy and size-exclusion chromatography (SEC). Results showed that more ether bonds were cleaved with increased pretreatment temperature and lower pH, whereas the levels of carbon-carbon bonded structures (e.g. phenylcoumaran and resinol units) were hardly affected. With a pretreatment of 160°C and 1% H2SO4, the majority of the β-O-4 bonds were cleaved. In addition, lignin depolymerization was more evident than repolymerization at higher pretreatment temperatures and lower pH. Documenting lignin structural changes as a function of pretreatment parameters provides a tool for biorefineries to gain flexibility in processing parameters with full control over the final properties of the products.
Acknowledgments
The authors would like to thank the Innovation Fund Denmark for funding under the Biomass for the 21st century project. JR was funded by the DOE Great Lakes Bioenergy Research Center (DOE BER Office of Science, DE-FC02–07ER64494).
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©2017 Walter de Gruyter GmbH, Berlin/Boston
Articles in the same Issue
- Frontmatter
- Effects of thermo-hygro-mechanical (THM) treatment on the viscoelasticity of in-situ lignin
- 2D NMR characterization of wheat straw residual lignin after dilute acid pretreatment with different severities
- Determination of inorganic element distribution in the freeze-fixed stem of Al2(SO4)3-treated Hydrangea macrophylla by TOF-SIMS and ICP-AES
- NMR determination of sorption isotherms in earlywood and latewood of Douglas fir. Identification of bound water components related to their local environment
- The combined effects of initial microfibrillar angle and moisture contents on the tensile mechanical properties and angle alteration of wood foils during tension
- Fatigue behavior of Japanese cypress (Chamaecyparis obtusa) under repeated compression loading tests perpendicular to the grain
- Influence of strain rate, temperature and fatigue on the radial compression behaviour of Norway spruce
- Effect of conditioning history on the characterization of hardness of thermo-mechanical densified and heat treated poplar wood
- An innovative composite plywood for the acoustic improvement of small closed spaces
- Antioxidant activity of Scots pine heartwood and knot extractives and implications for resistance to brown rot
- Quantitative observation of the foraging tunnels in Sitka spruce and Japanese cypress caused by the drywood termite Incisitermes minor (Hagen) by 2D and 3D X-ray computer tomography (CT)
Articles in the same Issue
- Frontmatter
- Effects of thermo-hygro-mechanical (THM) treatment on the viscoelasticity of in-situ lignin
- 2D NMR characterization of wheat straw residual lignin after dilute acid pretreatment with different severities
- Determination of inorganic element distribution in the freeze-fixed stem of Al2(SO4)3-treated Hydrangea macrophylla by TOF-SIMS and ICP-AES
- NMR determination of sorption isotherms in earlywood and latewood of Douglas fir. Identification of bound water components related to their local environment
- The combined effects of initial microfibrillar angle and moisture contents on the tensile mechanical properties and angle alteration of wood foils during tension
- Fatigue behavior of Japanese cypress (Chamaecyparis obtusa) under repeated compression loading tests perpendicular to the grain
- Influence of strain rate, temperature and fatigue on the radial compression behaviour of Norway spruce
- Effect of conditioning history on the characterization of hardness of thermo-mechanical densified and heat treated poplar wood
- An innovative composite plywood for the acoustic improvement of small closed spaces
- Antioxidant activity of Scots pine heartwood and knot extractives and implications for resistance to brown rot
- Quantitative observation of the foraging tunnels in Sitka spruce and Japanese cypress caused by the drywood termite Incisitermes minor (Hagen) by 2D and 3D X-ray computer tomography (CT)
