Individual Cellulose Research Articles

Evaluation of chemical treatments to tensile properties of cellulosic bamboo fibers

Acidified sodium chlorite (NaClO2) and sodium hydroxide (NaOH) solutions were successfully used to eliminate lignin and hemicellulose, respectively, from isolated bamboo fibers to investigate their microstructures, composition and micro-tensile properties in individual cellulose fibers. The results demonstrated that isolated fibers and chemically treated fibers clearly displayed different wrinkles, pores and microfibril aggregations on the cell wall surface. Field emission environmental scanning electron microscope images together with confocal scanning laser microscope measurements revealed that chemical treatments have a reduction effect on micro-tensile strength and modulus. Two methods of freeze-drying and air-drying produced varying interfaces and pores in microfibril aggregations and resulted in different tensile behavior. Notably, the reductions of Young’s modulus and tensile strength in freeze-drying (52.99 and 13.32%) fibers are larger than that (18.21 and 10.93%) in air-drying samples. These results suggest that most fractures occur in the weak interspaces or pores that are caused by the loss of matrix materials during chemical treatments.

Multimethod approach to understand the assembly of cellulose fibrils in the biosynthesis of bacterial cellulose

The production of controlled bacterial cellulose structures for various applications requires a better understanding on the mechanism of cellulose biosynthesis as well as proper tools for structural characterization of the materials. In this work, bacterial celluloses synthesized by an Asaia bogorensis strain known to produce fine cellulose fibrils and a commonly used Komagataeibacter xylinus strain were characterized using a comprehensive set of methods covering multiple levels of the hierarchical structure. FT-IR spectroscopy and x-ray diffraction were used to analyse the crystal structure and crystallite dimensions, whereas scanning and transmission electron microscopy, atomic force microscopy, and small-angle x-ray and neutron scattering were employed to obtain information on the higher-level fibrillar structures. All methods yielded results consistent with the A. bogorensis cellulose fibrils being thinner than the K. xylinus fibrils on both the level of individual cellulose microfibrils and bundles or ribbons thereof, even though the exact values determined for the lateral fibril dimensions depended slightly on the method and sample preparation. Particularly, the width of microfibril bundles determined by the microscopy methods differed due to shrinkage and preferred orientation caused by drying, whereas the microfibril diameter remained unaffected. The results were used to understand the biological origin of the differences between the two bacterial celluloses.

What cell wall components are the best indicators for Miscanthus digestibility and conversion to ethanol following variable pretreatments?

BackgroundEnergy crops including Miscanthus provide a storable, portable energy source which can be used to complement a wide range of products and energy generation systems. Miscanthus is predominantly used in Europe as a combustion material for electricity generation but also has the potential for biochemical conversion due to its high yield and low-nutrient requirements. The ratio of holocellulose (hemicellulose and cellulose combined) to acid detergent lignin (H:L) within the senesced material has previously been shown to indicate the relative suitability of Miscanthus accessions for thermochemical conversion. In this study, the ratio was assessed to examine its use as a selection aid for biochemical conversion. 20 highly-characterised Miscanthus accessions were saccharified using an enzyme mix to determine optimum sugar release. Nine of these accessions spanning high, medium and low H:L ratios were then autoclaved with dilute acid, alkali or water, and enzymically hydrolysed and fermented to produce ethanol. Samples taken throughout the process allowed assessments of released sugars.ResultsEnzymic degradation of the biomass showed a relationship between H:L ratio and glucose release, with high glucose release for high H:L ratio accessions and vice versa. Xylose release showed no such relationship. This relationship was maintained following pretreatments and enzyme saccharification, where compound analysis showed that following all pretreatments, accessions with high H:L ratios repeatedly had the highest releases of glucose, xylose and arabinose, and produced more ethanol. Release of all measured compounds increased with the pretreatment severity and ethanol yields from each pretreatment correlated with the respective glucose yield, providing assurance that any inhibitory compounds generated were tolerated by the fermentation yeast. Strong correlations were also seen between glucose release, ethanol and cell wall components, with cellulose showing the highest correlations with ethanol yields for some treatments and H:L ratio with others.ConclusionsThe H:L ratio is a good predictor of ethanol yields and sugar release from Miscanthus in this study but individual components lignin and cellulose also correlate well, especially for hot water and mild acid pretreatments. In conclusion, use of the H:L ratio does not provide any advantages over the concentration of individual cell wall components for predicting sugar release and ethanol yields.

Initiation, Elongation, and Termination of Bacterial Cellulose Synthesis.

Cellulose is the major component of the plant cell wall and composed of β-linked glucose units. Use of cellulose is greatly impacted by its physical properties, which are dominated by the number of individual cellulose strand within each fiber and the average length of each strand. Our work described herein provides a complete mechanism for cellulose synthase accounting for its processivity and mechanism of initiation. Using ionic liquids and gel permeation chromatography, we obtain kinetic constants for initiation, elongation, and termination (release of the cellulose strand from the enzyme) for two bacterial cellulose synthases (Gluconacetobacter hansenii and Rhodobacter sphaeroides). Our results show that initiation of synthesis is primer-independent. After initiation, the enzyme undergoes multiple cycles of elongation until the strand is released. The rate of elongation is much faster than that of steady-state turnover. Elongation requires cyclic addition of glucose (from uridine diphosphate-glucose) and then strand translocation by one glucose unit. Translocations greater than one glucose unit result in termination requiring reinitiation. The rate of the strand release, relative to the rate of elongation, determines the processivity of the enzyme. This mechanism and the measured rate constants were supported by kinetic simulation. With the experimentally determined rate constants, we are able to simulate steady-state kinetics and mimic the size distribution of the product. Thus, our results provide for the first time a mechanism for cellulose synthase that accounts for initiation, elongation, and termination.

Assessing the potential of quartz crystal microbalance to estimate water vapor transfer in micrometric size cellulose particles

This study aims at assessing the use of a quartz crystal microbalance (QCM) coupled with an adsorption system to measure water vapor transfer properties in micrometric size cellulose particles. This apparatus allows measuring successfully water vapor sorption kinetics at successive relative humidity (RH) steps on a dispersion of individual micrometric size cellulose particles (1 μg) with a total acquisition duration of the order of one hour. Apparent diffusivity and water uptake at equilibrium were estimated at each step of RH by considering two different particle geometries in mass transfer modeling, i.e. sphere or finite cylinder, based on the results obtained from image analysis. Water vapor diffusivity values varied from 2.4 × 10−14 m2 s−1 to 4.2 × 10−12 m2 s−1 over the tested RH range (0–80%) whatever the model used. A finite cylinder or spherical geometry could be used equally for diffusivity identification for a particle size aspect ratio lower than 2.

Development of completely dispersed cellulose nanofibers.

Plant cellulose fibers of width and length ∼0.03 mm and ∼3 mm, respectively, can be completely converted to individual cellulose nanofibers of width and length ∼3 nm and ∼1 µm, respectively, by 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO)-mediated oxidation under aqueous conditions and subsequent gentle mechanical disintegration of the oxidized cellulose in water. The obtained TEMPO-oxidized cellulose nanofibers (TOCNs) are new bio-based, crystalline nanomaterials with applications in the high-tech and commodity product industries. Sodium carboxylate groups, which are densely, regularly, and position-selectively present on the crystalline TOCN surfaces, can be efficiently ion-exchanged with other metal and alkylammonium carboxylate groups in water to control the biodegradable/stable and hydrophilic/hydrophobic properties of the TOCNs. TOCNs are therefore promising nanomaterials that can be prepared from the abundant wood biomass resources present in Japan. Increased production and use of TOCNs would stimulate a new material stream from forestry to industries, helping to establish a sustainable society based on wood biomass resources.

Cellulose Nanocrystals with Tethered Polymer Chains: Chemically Patchy versus Uniform Decoration

The site-specific surface modification of colloidal substrates, yielding "patchy" nanoparticles, is a rapidly expanding area of research as a result of the new complex structural hierarchies that are becoming accessible to chemists and materials scientists through colloidal self-assembly. The inherent directionality of cellulose chains, which feature a nonreducing and a reducing end, within individual cellulose nanocrystals (CNCs) renders them an interesting experimental platform for the synthesis of asymmetric nanorods with end-tethered polymer chains. Here, we present water-tolerant reaction pathways toward patchy and uniformly modified CNC hybrids based on atom transfer radical polymerization (ATRP) and initiators that were linked to the CNCs with carbodiimide-mediated coupling and Fischer esterification, respectively. Various monomers, including N-isopropylacrylamide (NIPAM), [2-(methacryloyloxy)ethyl]trimethylammonium chloride (METAC), and sodium 4-vinylbenzenesulfonate (4-SS), were polymerized from both types of initiator-modified CNCs, yielding chemically patchy and uniform CNC hybrids, via surface-initiated ATRP (SI-ATRP). Interestingly, the stereochemistry of tethered PNIPAM was affected by the precise location of ATRP initiating sites, as evidenced by 1H NMR and circular dichroism (CD) spectroscopy. This effect may be related to the inherent right-handed chirality of CNCs. CNC/PMETAC hybrids were labeled with gold nanoparticles (AuNPs) in order to visualize the precise location of polymer tethers via cryo-electron microscopy. In some instances, the AuNPs were indeed concentrated at the end groups of the patchy CNC hybrids.

Retention of metal and sulphate ions from acidic mining water by anionic nanofibrillated cellulose

We carried out an adsorption experiment to investigate the ability of anionic nanofibrillated cellulose (NFC) to retain metal and SO42− ions from authentic highly acidic (pH3.2) mining water. Anionic NFC gels of different consistencies (1.1-%, 1.4-% and 1.8-% w/w) were allowed to react for 10min with mining water, after which NFC-induced changes in the metal and SO42− concentrations of the mining water were determined. The sorption capacities of the NFC gels were calculated as the difference between the element concentrations in the untreated and NFC-treated mining water samples. All the NFCs efficiently co-adsorbed both metals and SO42−. The retention of metals was concluded to take place through formation of metal-ligand complexes. The reaction between the NFC ligand and the polyvalent cations renders the cellulose nanofibrils positively charged and, thus, able to retain SO42− electrostatically. Adsorption capacity of the NFC gels substantially increased upon decreasing DM content as a result of the dilution-induced weakening of the mutual interactions between individual cellulose nanofibrils. This outcome reveals that the dilution of the NFC gel not only increases its purification capacity but also reduces the demand for cellulosic raw material. These results suggest that anionic NFC made of renewable materials serves as an environmentally sound and multifunctional purification agent for acidic multimetal mining waters or AMDs of high ionic strength. Unlike industrial minerals traditionally used to precipitate valuable metals from acidic mining effluents before their permanent disposal from the material cycle, NFC neither requires mining of unrenewable raw materials nor produces inorganic sludges.

Nanocelluloses obtained by ammonium persulfate (APS) oxidation of bleached kraft pulp (BKP) and bacterial cellulose (BC) and their application in biocomposite films together with chitosan

Abstract Bleached birch kraft pulp (BKP, Södra Cell AB, Sweden) and unmodified bacterial cellulose (BC) pellicles, biosynthesized by the bacterium Komagataeibacter rhaeticus, were converted to cellulose nanofibers via ammonium persulfate (APS) oxidation. Fiber dimensions were investigated in an atomic force microscope, and the crystallite size was calculated by Rietveld analysis. Saos-2 osteosarcoma cell line served to assess the in vitro cytocompatibility of the biocomposite films. Results showed that individual cellulose nanofibers with an average width of 80±15 nm and a length between 600 and 1200 nm are formed by APS oxidation. The obtained BC nanofibers can be promising constituents in nanocellulose films and in chitosan-matrix films with improved physical-mechanical and biological properties. Good cellular biocompatibility was found for chitosan/oxidized cellulose films; the viability of Saos-2 osteosarcoma cells was higher on chitosan/oxidized BC films compared to chitosan/oxidized BKP films.

Surface-Induced Frustration in Solid State Polymorphic Transition of Native Cellulose Nanocrystals.

The presence of an interface generally influences crystallization of polymers from melt or from solution. Here, by contrast, we explore the effect of surface immobilization in a direct solid state polymorphic transition on individual cellulose nanocrystals (CNCs), extracted from a plant-based origin. The conversion from native cellulose I to cellulose III crystal occurred via a host-guest inclusion of ethylene diamine inside the crystal. A 60% reduction in CNC width (height) in atomic force microscopy images suggested that when immobilized on a flat modified silica surface, the stresses caused by the inclusion or the subsequent regeneration resulted in exfoliation, hypothetically, between the van der Waals bonded sheets within the crystal. Virtually no changes in dimensions were visible when the polymorphic transition was performed to nonimmobilized CNCs in bulk dispersion. With reservations and by acknowledging the obvious dissimilarities, the exfoliation of cellulose crystal sheets can be viewed as analogous to exfoliation of 2D structures like graphene from a van der Waals stacked solid. Here, the detachment is triggered by an inclusion of a guest molecule inside a host cellulose crystal and the stresses caused by the firm attachment of the CNC on a solid substrate, leading to detachment of molecular sheets or stacks of sheets.

Alkaline Delignification of Cactus Fibres for Pulp and Papermaking Applications

Stable aqueous suspensions with high cellulosic contents and low fractions of lignin have been prepared from Cactus fibres via chemical delignification of the Cactus biomass feedstock with a sodium hydroxide–anthraquinone (soda–AQ) mixture. In order to optimize the reaction parameters, various temperatures between 120 and 170 °C and reaction times between 60 and 180 min were examined. The optimal yield of the resulting alkaline pulps (corresponding to the complete reaction of the raw materials) was equal to 41.4%, while the morphological parameters of individual cellulose fibres (such as length, width, and fraction of fine elements) were determined using a MorFi analyser. The estimated degree of polymerization, water retention value, total charge, and drainability of the produced pulps confirmed their suitability for papermaking applications; as a result, paper sheets were manually prepared using a Rapid-Kothen sheet former apparatus. The morphological analysis of the produced paper was conducted using a scanning electron microscopy technique, and its structural and mechanical properties were evaluated with the standard laboratory testing equipment. The obtained results indicate that the paper fabricated from Cactus fibres via the soda–AQ delignification process exhibits homogenous morphology as well as satisfactory mechanical and structural properties.

Spin Probe Multi-Frequency EPR Study of Unprocessed Cotton Fibers.

Known since the ancient times, cotton continues to be one of the essential materials for the human civilization. Cotton fibers are almost pure cellulose and contain both crystalline and amorphous nanodomains with different physicochemical properties. While understanding of interactions between the individual cellulose chains within the crystalline phase is important from a perspective of mechanical properties, studies of the amorphous phase lead to characterization of the essential transport parameters, such as solvent diffusion, dyeing, drug release, and toxin absorption, as well as more complex processes of enzymatic degradation. Here, we describe the use of spin probe electron paramagnetic resonance methods to study local polarity and heterogeneous viscosity of two types of unprocessed cotton fibers, G. hirsutum and G. barbadense, harvested in the State of North Carolina, USA. These fibers were loaded with two small molecule nitroxide probes that differ in polarity-Tempo and its more hydrophilic derivative Tempol-using a series of polar and non-polar solvents. The electron paramagnetic resonance spectra of the nitroxide-loaded cotton fibers were analyzed both semi-empirically and by least-squares simulations using a rigorous stochastic theory of electron paramagnetic resonance spectra developed by Freed and coworkers. A software package and least-squares fitting protocols were developed to carry out automatic simulations of multi-component electron paramagnetic resonance spectra in both first-derivative and the absorption forms at multiple resonance frequencies such as X-band (9.5 GHz) and W-band (94.3 GHz). The results are compared with the preceding electron paramagnetic resonance spin probe studies of a commercial bleached cotton sheeting carried out by Batchelor and coworkers. One of the results of this study is a demonstration of a co-existence of cellulose nanodomains with different physicochemical properties such as polarity and microviscosity that are affected by solvents and temperature. Spin labeling studies also revealed a macroscopic heterogeneity in the domain distribution along the cotton fibers and a critical role the cuticular layer is playing as a barrier for spin probe penetration. Finally but not lastly, the simultaneous multi-component least-squares simulation method of electron paramagnetic resonance spectra acquired at different resonant frequencies and the display forms (e.g., absorption and first-derivative displays) and the strategy of spectral parameter sharing could be potentially applicable to other heterogeneous biological systems in addition to the cotton fibers studies here.

A single heterologously expressed plant cellulose synthase isoform is sufficient for cellulose microfibril formation in vitro

Plant cell walls are a composite material of polysaccharides, proteins, and other noncarbohydrate polymers. In the majority of plant tissues, the most abundant polysaccharide is cellulose, a linear polymer of glucose molecules. As the load-bearing component of the cell wall, individual cellulose chains are frequently bundled into micro and macrofibrils and are wrapped around the cell. Cellulose is synthesized by membrane-integrated and processive glycosyltransferases that polymerize UDP-activated glucose and secrete the nascent polymer through a channel formed by their own transmembrane regions. Plants express several different cellulose synthase isoforms during primary and secondary cell wall formation; however, so far, none has been functionally reconstituted in vitro for detailed biochemical analyses. Here we report the heterologous expression, purification, and functional reconstitution of Populus tremula x tremuloides CesA8 (PttCesA8), implicated in secondary cell wall formation. The recombinant enzyme polymerizes UDP-activated glucose to cellulose, as determined by enzyme degradation, permethylation glycosyl linkage analysis, electron microscopy, and mutagenesis studies. Catalytic activity is dependent on the presence of a lipid bilayer environment and divalent manganese cations. Further, electron microscopy analyses reveal that PttCesA8 produces cellulose fibers several micrometers long that occasionally are capped by globular particles, likely representing PttCesA8 complexes. Deletion of the enzyme's N-terminal RING-finger domain almost completely abolishes fiber formation but not cellulose biosynthetic activity. Our results demonstrate that reconstituted PttCesA8 is not only sufficient for cellulose biosynthesis in vitro but also suffices to bundle individual glucan chains into cellulose microfibrils.

Preparation and Characterization of Polyvinyl Alcohol-Chitosan Composite Films Reinforced with Cellulose Nanofiber.

In this study microcrystalline cellulose (MCC) was oxidized by 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO)-mediated oxidation. The treated cellulose slurry was mechanically homogenized to form a transparent dispersion which consisted of individual cellulose nanofibers with uniform widths of 3–4 nm. Bio-nanocomposite films were then prepared from a polyvinyl alcohol (PVA)-chitosan (CS) polymeric blend with different TEMPO-oxidized cellulose nanofiber (TOCN) contents (0, 0.5, 1.0 and 1.5 wt %) via the solution casting method. The characterizations of pure PVA/CS and PVA/CS/TOCN films were performed in terms of field emission scanning electron microscopy (FESEM), tensile tests, thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD). The results from FESEM analysis justified that low loading levels of TOCNs were dispersed uniformly and homogeneously in the PVA-CS blend matrix. The tensile strength and thermal stability of the films were increased with the increased loading levels of TOCNs to a maximum level. The thermal study indicated a slight improvement of the thermal stability upon the reinforcement of TOCNs. As evidenced by the FTIR and XRD, PVA and CS were considered miscible and compatible owing to hydrogen bonding interaction. These analyses also revealed the good dispersion of TOCNs within the PVA/CS polymer matrix. The improved properties due to the reinforcement of TOCNs can be highly beneficial in numerous applications.

Measurements of hydrogen, oxygen and carbon isotope variability inSphagnummoss along a micro‐topographical gradient in a southern Patagonian peatland

ABSTRACTPeat archives offer a diverse range of physical and chemical proxies from which it is possible to study past environmental and ecological changes. Direct numerical calibration and verification is difficult so process‐based and mechanistic studies are therefore required to establish and quantify links between environmental changes and their associated proxy‐responses. Traditional ‘space‐for‐time’ calibrations provide a solution to this calibration problem, but are often unable to isolate a single environmental variable from other potentially confounding variables. In this study, we explored the potential of a site‐specific ‘space‐for‐time’ approach applied to a hummock‐hollow transect on an ombrotrophic raised bog in Patagonia, southern Chile. Coupled stable carbon, oxygen and hydrogen isotopic measurements were made on individual samples ofSphagnummoss cellulose and compared with plant‐associated waters, local hydrology, temperature and relative humidity, sampled at the same points along the study transect. Results reveal a range of environmental responses, which were supported by plant‐physiological models in the case of carbon and oxygen isotopes. For hydrogen isotopes, the results obtained from cellulose indicated a need for further research into hydrogen isotope fractionation inSphagnum. We recommend conducting site‐specific characterization of plant response to support the development of peat‐based isotope records for palaeoenvironmental research, and where logistically possible, that monitoring is conducted over timescales appropriate to the time‐integrative nature of theSphagnumrecord.

A versatile method for producing functionalized cellulose nanofibers and their application.

A facile method was developed to produce functionalized cellulose nanofibers in one step by ball milling. Through the synergy of mechanical and chemical actions, the produced cellulose nanofibers are ca. 20 nm wide and several micrometers long, with surface properties tailored by choice of modifying reagent. Modified by succinic anhydride, a cellulose nanofiber shows enhanced hydrophilicity, can be readily dispersed in water or DMSO, and gives a zeta potential of -38.7 mV due to carboxyl groups on the surface. Modified by dodecyl succinic anhydride, a cellulose nanofiber has excellent dispersibility in o-xylene and good compatibility with polyethylene. The polyethylene-cellulose nanofiber composite presents overall enhancement of mechanical properties. This method opens a new way to the production of functionalized cellulose nanofibers.

Surface energy of cellulosic materials: The effect of particle morphology, particle size, and hydroxyl number

Understanding the surface properties of cellulose materials is important for proper commercial applications. The effect of particle size, particle morphology, and hydroxyl number on the surface energy of three microcrystalline cellulose (MCC) preparations and one nanofibrillated cellulose (NFC) preparation were investigated using inverse gas chromatography at column temperatures ranging from 30ºC to 60ºC. The mean particle sizes for the three MCC samples and the NFC sample were 120.1, 62.3, 13.9, and 9.3 μm. The corresponding dispersion components of surface energy at 30°C were 55.7 ± 0.1, 59.7 ± 1.3, 71.7 ± 1.0, and 57.4 ± 0.3 mJ/m2. MCC samples are agglomerates of small individual cellulose particles. The different particle sizes and morphologies of the three MCC samples resulted in various hydroxyl numbers, which in turn affected their dispersion component of surface energy. Cellulose samples exhibiting a higher hydroxyl number have a higher dispersion component of surface energy. The dispersion component of surface energy of all the cellulose samples decreased linearly with increasing temperature. MCC samples with larger agglomerates had a lower temperature coefficient of dispersion component of surface energy.

Analyzing three‐dimensional structure and geometrical shape of individual cellulose nanocrystal from switchgrass

The three‐dimensional morphology, size distribution, and structure of individual cellulose nanocrystals (CNCs) isolated from switchgrass (Panicumvirgatum L), a representative raw biomass material, were investigated in this research. Width and height evolutions along the individual CNC longitudinal direction were statistically and quantitatively characterized using transmission electron microscopy (TEM) and atomic force microscopy (AFM). Lognormal distribution was identified as the most likely for cellulose nanocrystals’ size distribution. Height and width dimensions were shown to decrease toward the ends from the midpoint of individual CNCs, implying a spindle shape. The observed rough surfaces of CNCs were explainable as the results of acid etching of the subcrystalline and disordered region located at the surface. X‐ray diffraction analysis of crystallite size accompanied with TEM and AFM measurements revealed that the cross‐sectional dimensions of individual switchgrass CNC were either rectangularly or elliptically shaped, with an approximately 3–5 nm lateral element length range. POLYM. COMPOS., 38:2368–2377, 2017. © 2015 Society of Plastics Engineers

Fractionation of organic substances from the South African Eucalyptus grandis biomass by a combination of hot water and mild alkaline treatments

An alternative way of fractionating lignocellulose biomass into its individual components, hemicelluloses, lignin and cellulose, was investigated. South African Eucalyptus grandis wood chips were fractionated using a combination of hot water and alkaline treatments with or without AQ. Initially, the biomass samples were treated in hot water to remove hemicelluloses. At optimum pre-fraction conditions, the data acquired revealed that almost 12 % of the E. grandis wood biomass could be recovered as hemicelluloses. When the hemicelluloses pre-extracted biomass was further treated using sodium hydroxide with or without AQ, the data indicated that the amount of lignin and cellulose that could be recovered was 22 and 36 %, respectively (as % of the wood mass). The substrate was characterised by a higher amount of α-cellulose (91–93 %), lower kappa no (12–13), viscosity (327–450 η mg/L) and DP (1078–1536). It was then presumed that such pulp could meet end-user requirement of the dissolving pulps. Industrial acceptance of this biomass fractionation concept, however, will further require careful assessments of various options for treating and purifying the hemicelluloses and lignin in their respect streams.

Mesoporous structures in never-dried softwood cellulose fibers investigated by nitrogen adsorption

Nitrogen adsorption was used to characterize mesoporous structures in never-dried softwood cellulose fibers. Distinct inflections in desorption isotherms were observed over the relative vapor pressure (P/P0) range of 0.5–0.42 for never-dried cellulose fibers and partially delignified softwood powders. The reduction in N2 adsorption volume was attributed to cavitation of condensed N2 present in mesopores formed via lignin removal from wood cell walls during delignification. The specific surface areas of significantly delignified softwood powders were ~150 m2 g−1, indicating that in wood cell walls 16 individual cellulose microfibrils, each 3–4 nm in width, form one cellulose fibril bundle surrounded with a thin layer of lignin and hemicelluloses. Analysis of N2 adsorption isotherms indicates that mesopores in the softwood cellulose fibers and partially delignified softwood powders had peaks ranging from 4 to 20 nm in diameter.