Dataset Information

Efficient Mild Organosolv Lignin Extraction in a Flow-Through Setup Yielding Lignin with High ?-O-4 Content.

ABSTRACT: Current lignin fractionation methods use harsh conditions that alter the native lignin structure, resulting in a recalcitrant material which is undesired for downstream processing. Milder fractionation processes allow for the isolation of lignins that are high in ?-aryl ether (?-O-4) content, however, at reduced extraction efficiency. The development of improved lignin extraction methods using mild conditions is therefore desired. For this reason, a flow-through setup for mild ethanosolv extraction (120 °C) was developed. The influence of acid concentration, ethanol/water ratio, and the use of other linear alcohol co-solvents on the delignification efficiency and the ?-O-4 content were evaluated. With walnut shells as model feedstock, extraction efficiencies of over 55% were achieved, yielding lignin with a good structural quality in terms of ?-O-4 linking motifs (typically over 60 per 100 aromatic units). For example, lignin containing 66 ?-O-4 linking motifs was obtained with an 80:20 n-propanol/water ratio, 0.18 M H₂SO₄ with overall a good extraction efficiency of 57% after 5 hours. The majority of the lignin was extracted in the first 2 hours and this lignin showed the best structural quality. Compared to batch extractions, both higher lignin extraction efficiency and higher ?-O-4 content were obtained using the flow setup.

SUBMITTER: Zijlstra DS

PROVIDER: S-EPMC6960700 | biostudies-literature | 2019 Nov

REPOSITORIES: biostudies-literature

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Publications

Efficient Mild Organosolv Lignin Extraction in a Flow-Through Setup Yielding Lignin with High β-O-4 Content.

Zijlstra Douwe S DS Analbers Coen A CA Korte Joren de J Wilbers Erwin E Deuss Peter J PJ

Polymers 20191120 12

Current lignin fractionation methods use harsh conditions that alter the native lignin structure, resulting in a recalcitrant material which is undesired for downstream processing. Milder fractionation processes allow for the isolation of lignins that are high in β-aryl ether (β-O-4) content, however, at reduced extraction efficiency. The development of improved lignin extraction methods using mild conditions is therefore desired. For this reason, a flow-through setup for mild ethanosolv extract ...[more]

PMID: 31757013

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Project description:Innovative biomass fractionation is of major importance for economically competitive biorefineries. Lignin is currently severely underutilized due to the use of high severity fractionation methodologies that yield complex condensed lignin that limits high-value applicability. Mild lignin fractionation conditions can lead to lignin with a more regular C-O bonded structure that has increased potential for higher value applications. Nevertheless, such extraction methodologies typically suffer from inadequate lignin extraction efficiencies and yield. (Semi)-continuous flow extractions are a promising method to achieve improved extraction efficiency of such C-O linked lignin. Here we show that optimized organosolv extraction in a flow-through setup resulted in 93-96% delignification of 40 g walnut shells (40 wt% lignin content) by applying mild organosolv extraction conditions with a 2 g/min flowrate of a 9:1 n-butanol/water mixture with 0.18 M H2SO4 at 120°C in 2.5 h. 85 wt% of the lignin (corrected for alcohol incorporation, moisture content and carbohydrate impurities) was isolated as a powder with a high retention of the β-aryl ether (β-O-4) content of 63 linking motifs per 100 C9 units. Close examination of the isolated lignin showed that the main carbohydrate contamination in the recovered lignin was butyl-xyloside and other butoxylate carbohydrates. The work-up and purification procedure were investigated and improved by the implementation of a caustic soda treatment step and phase separation with a continuous integrated mixer/separator (CINC). This led to a combined 75 wt% yield of the lignin in 3 separate fractions with 3% carbohydrate impurities and a very high β-O-4 content of 67 linking motifs per 100 C9 units. Analysis of all the mass flows showed that 98% of the carbohydrate content was removed with the inline purification step, which is a significant improvement to the 88% carbohydrate removal for the traditional lignin precipitation work-up procedure. Overall we show a convenient method for inline extraction and purification to obtain high β-O-4 butanosolv lignin in excellent yields.

Dataset Information

Efficient Mild Organosolv Lignin Extraction in a Flow-Through Setup Yielding Lignin with High ?-O-4 Content.

Publications

Efficient Mild Organosolv Lignin Extraction in a Flow-Through Setup Yielding Lignin with High β-O-4 Content.

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