Theory, practice and prospects of X-ray and neutron scattering for lignocellulosic biomass characterization: towards understanding biomass pretreatment
Abstract:Efficient deconstruction of lignocelluosic biomass into fermentable sugar depends largely on the development of advanced biomass pretreatment technologies. Due to the highly heterogeneous nanoand microstructure of the plant cell walls, there is a lack of understanding with regards to interactions 10
“…To this end, different pretreatment strategies are being developed to improve sugar yield from lignocellulosic biomass samples by increasing accessibility of enzymes to cellulose fibers (Meng & Ragauskas, 2014), decreasing lignin content (Singh, Shukla, Tiwari & Srivastava, 2014;Zeng, Zhao, Yang & Ding, 2014) or transforming native cellulose crystalline structure into less recalcitrant forms (Cheng et al, 2011;da Costa Sousa et al, 2016). However, suitable pretreatment technologies have not been established due in part to complex interactions between plant cell walls and biomass pretreatment as well as coupling between the biomass recalcitrant factors (Cheng, Zhang, Simmons & Singh, 2015). This requires further study of pretreatment processes to identify efficient ways to deconstruct biomass.…”
“…To this end, different pretreatment strategies are being developed to improve sugar yield from lignocellulosic biomass samples by increasing accessibility of enzymes to cellulose fibers (Meng & Ragauskas, 2014), decreasing lignin content (Singh, Shukla, Tiwari & Srivastava, 2014;Zeng, Zhao, Yang & Ding, 2014) or transforming native cellulose crystalline structure into less recalcitrant forms (Cheng et al, 2011;da Costa Sousa et al, 2016). However, suitable pretreatment technologies have not been established due in part to complex interactions between plant cell walls and biomass pretreatment as well as coupling between the biomass recalcitrant factors (Cheng, Zhang, Simmons & Singh, 2015). This requires further study of pretreatment processes to identify efficient ways to deconstruct biomass.…”
“…Although pure cellulose showed a small peak at 2θ of 34.5°, a reflection of the 004 plane of the periodic structure of the crystallite along the axial direction, 37 the peak disappeared in all four fractions. The loss of 004 peaks did not indicate the crystal structure change, as this peak is sensitive to the twisting and alignment of microfibrils and even the moisture content.…”
Section: Acs Sustainable Chemistry and Engineeringmentioning
Rice
straw cellulose was completely defibrillated via aqueous counter
collision (ACC) at a low energy input of 15 kWh/kg, then fractionated
by differential centrifugation into four increasing weight fractions
of progressively thinner cellulose nanofibrils (CNFs): 6.9% in 80–200
nm, 14.4% in 20–80 nm, 20.3% in 5–20 nm, and 58.4% in
less than 5 nm thickness. The 93.1% less than 80 nm or 78.7% less
than 20 nm thick CNFs yields were more than double those from wood
pulp by other mechanical means but at a lower energy input. The smallest
(3.7 nm thick and 5.5 nm wide) CNFs were only a third or less in lateral
dimensions than those obatined through ACC processed from wood pulp,
bamboo, and microbial cellulose pellicle. The less than 20 nm thick
CNFs could self-assemble into continuous submicron (136 nm) wide fibers
by freezing and freeze-drying or semitransparent (13–42% optical
transmittance) film by ultrafiltration and air-drying with excellent
mechanical properties (164 MPa tensile strength, 4 GPa Young’s
modulus, and 16% strain at break). ACC defibrillated CNFs retained
essentially the same chemical and crystalline structures and thermal
stability as the original rice straw cellulose and therefore were
much more thermally stable than TEMPO oxidized CNFs and sulfuric acid
hydrolyzed cellulose nanocrystals from the same rice straw cellulose.
“…Small-angle X-ray scattering (SAXS) as a method capable of averaging over the volume in the X-ray beam is one of the very few techniques that can provide statistical information about the morphology, porosity and specific surface area of materials on the nanometre scale (Lichtenegger et al 2002(Lichtenegger et al , 2003Rennhofer et al 2014;Cheng et al 2015). SAXS patterns from wood can be regarded as arising from the electron density contrast in a two-phase composite, cellulose fibrils in a hemicellulose-lignin matrix, and with contributions from pores and other cavities at very small scattering angles (Jakob et al 1996).…”
Tracking the changes of cellulose crystallites upon thermo-hygro-mechanical treatment is essential to understand the response of wood cell walls to steam and compression. In this paper the influence of Compression combined with Steam (CS) treatment on wood cellulose crystallites and pores structure of Chinese fir (Cunninghamia lanceolata) was studied under different steaming temperatures and compression ratios. Small-angle X-ray scattering and wide-angle X-ray scattering were used to investigate the changes of cellulose crystallites dimension, aspect ratio, fibril diameter distribution, non-crystalline fraction, the number of chains in each microfibril, as well as the fractal dimension and size of pores in response to CS treatment conditions. Results indicate that the crystallinity increased due to CS treatment, but did not show alteration with varying CS treatment conditions, i.e. seemed nearly unaffected by higher temperatures or compression ratio, both for earlywood and latewood. The cellulose crystallite diameter depended on processing parameters: it increased with increasing treatment temperature. No considerable differences were found for earlywood and latewood. We interpret our findings as a rearrangement of adjacent cellulose chains towards higher crystalline perfection attributing to the increase in crystallinity. The same effect allows a larger coherence length of crystalline order and therefore features an increasing cross-sectional dimension. In general we can state that the CS treatment leads to higher crystallinity and more perfectly arranged cellulose crystals, while it does not greatly affect the microfibril diameter but rather the amorphous regions of the microfibrils and the surrounding hemicellulose and lignin.
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