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    Multi-scale processes of beech wood disintegration and pretreatment with 1-ethyl-3-methylimidazolium acetate/water mixtures
    (London : BioMed Central, 2016) Viell, Jörn; Inouye, Hideyo; Szekely, Noemi K.; Frielinghaus, Henrich; Marks, Caroline; Wang, Yumei; Anders, Nico; Spiess, Antje C.; Makowski, Lee
    Background: The valorization of biomass for chemicals and fuels requires efficient pretreatment. One effective strategy involves the pretreatment with ionic liquids which enables enzymatic saccharification of wood within a few hours under mild conditions. This pretreatment strategy is, however, limited by water and the ionic liquids are rather expensive. The scarce understanding of the involved effects, however, challenges the design of alternative pretreatment concepts. This work investigates the multi length-scale effects of pretreatment of wood in 1-ethyl-3-methylimidazolium acetate (EMIMAc) in mixtures with water using spectroscopy, X-ray and neutron scattering. Results: The structure of beech wood is disintegrated in EMIMAc/water mixtures with a water content up to 8.6 wt%. Above 10.7 wt%, the pretreated wood is not disintegrated, but still much better digested enzymatically compared to native wood. In both regimes, component analysis of the solid after pretreatment shows an extraction of few percent of lignin and hemicellulose. In concentrated EMIMAc, xylan is extracted more efficiently and lignin is defunctionalized. Corresponding to the disintegration at macroscopic scale, SANS and XRD show isotropy and a loss of crystallinity in the pretreated wood, but without distinct reflections of type II cellulose. Hence, the microfibril assembly is decrystallized into rather amorphous cellulose within the cell wall. Conclusions: The molecular and structural changes elucidate the processes of wood pretreatment in EMIMAc/water mixtures. In the aqueous regime with >10.7 wt% water in EMIMAc, xyloglucan and lignin moieties are extracted, which leads to coalescence of fibrillary cellulose structures. Dilute EMIMAc/water mixtures thus resemble established aqueous pretreatment concepts. In concentrated EMIMAc, the swelling due to decrystallinization of cellulose, dissolution of cross-linking xylan, and defunctionalization of lignin releases the mechanical stress to result in macroscopic disintegration of cells. The remaining cell wall constituents of lignin and hemicellulose, however, limit a recrystallization of the solvated cellulose. These pretreatment mechanisms are beyond common pretreatment concepts and pave the way for a formulation of mechanistic requirements of pretreatment with simpler pretreatment liquors. © 2016 Viell et al.
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    Biorefinery Concept Employing Bacillus coagulans: LX-Lignin and L-(+)-Lactic Acid from Lignocellulose
    (Basel : MDPI, 2021) Schroedter, Linda; Streffer, Friedrich; Streffer, Katrin; Unger, Peter; Venus, Joachim
    A new biorefinery concept is proposed that integrates the novel LX-Pretreatment with the fermentative production of L-(+)-lactic acid. Lignocellulose was chosen as a substrate that does not compete with the provision of food or feed. Furthermore, it contains lignin, a promising new chemical building material which is the largest renewable source for aromatic compounds. Two substrates were investigated: rye straw (RS) as a residue from agriculture, as well as the fibrous digestate of an anaerobic biogas plant operated with energy corn (DCS). Besides the prior production of biogas from energy corn, chemically exploitable LX-Lignin was produced from both sources, creating a product with a low carbohydrate and ash content (90.3% and 88.2% of acid insoluble lignin). Regarding the cellulose fraction of the biomass, enzymatic hydrolysis and fermentation experiments were conducted, comparing a separate (SHF), simultaneous (SSF) and prehydrolyzed simultaneous saccharification and fermentation (PSSF) approach. For this purpose, thermophilic B. coagulans 14-300 was utilized, reaching 38.0 g L−1 LA in 32 h SSF from pretreated RS and 18.3 g L−1 LA in 30 h PSSF from pretreated DCS with optical purities of 99%.