• Journal of the Korean Wood Science and Technology
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• v.50 no.6
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• pp.436-447
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• 2022

Lignocellulose nanofibrils (LCNFs) were prepared using a two-step deep eutectic solvent (DES) and enzymatic pretreatment followed by mechanical defibrillation, and we examined the effects of enzymatic pretreatment conditions on different characteristics of the LCNFs thus obtained. The LCNFs yielded using the two-step DES pretreatment (Enz-LCNF) exhibited a well-defibrillated entangled web-like structure with an average fiber diameter ranging from 15.7 to 20.4 nm. Furthermore, we found that the average diameter and filtration time of the Enz-LCNFs decreased with an increase in enzyme concentration and enzymatic treatment time, whereas we detected a concomitant reduction in the tensile strength of the Enz-LCNF sheets. The Enz-LCNFs were characterized by a typical cellulose I structure, thereby indicating that the enzymatic treatment causes very little damage to the crystalline form.

• Journal of the Korean Wood Science and Technology
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• v.39 no.3
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• pp.197-205
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• 2011

Cellulose nanofibrils (CNF) with 50~100 nm diameter were manufactured from micro-size cellulose by an application of a high-pressure homogenizer at 1,400 bar. High strength nanopapers were prepared over a filter paper by a vacuum filtration from CNF suspension. After reinforcing and dispersing CNF suspension, hydroxypropyl cellulose (HPC) and polyvinyl alcohol (PVA)-based composites were tailored by solvent- and film-casting methods, respectively. After 2, 4, 6 and 8 passes through high-pressure homogenizer, the tensile strength of the nanopapers were extremely high and increased linearly depending upon the pass number. Chemical modification of 1H, 1H, 2H, 2H-perfluorodecyl-triethoxysilane (PFDTES) on the nanopapers significantly increased the mechanical strength and water repellency. The reinforcement of 1, 3, and 5 wt% CNF to HPC and PVA resins also improved the mechanical properties of the both composites.

• Toxicological Research
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• v.35 no.1
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• pp.45-63
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• 2019

In view of the growing industrial use of Bacterial cellulose (BC), and taking into account that it might become airborne and be inhaled after industrial processing, assessing its potential pulmonary toxic effects assumes high relevance. In this work, the murine model was used to assess the effects of exposure to respirable BC nanofibrils (nBC), obtained by disintegration of BC produced by Komagataeibacter hansenii. Murine bone marrow-derived macrophages ($BMM{\Phi}$) were treated with different doses of nBC (0.02 and 0.2 mg/mL, respectively 1 and $10{\mu}g$ of fibrils) in absence or presence of 0.2% Carboxymethyl Cellulose (nBCMC). Furthermore, mice were instilled intratracheally with nBC or nBCMC at different concentrations and at different time-points and analyzed up to 6 months after treatments. Microcrystaline $Avicel-plus^{(R)}$ CM 2159, a plant-derived cellulose, was used for comparison. Markers of cellular damage (lactate dehydrogenase release and total protein) and oxidative stress (hydrogen peroxidase, reduced glutathione, lipid peroxidation and glutathione peroxidase activity) as well presence of inflammatory cells were evaluated in brochoalveolar lavage (BAL) fluids. Histological analysis of lungs, heart and liver tissues was also performed. BAL analysis showed that exposure to nBCMC or CMC did not induce major alterations in the assessed markers of cell damage, oxidative stress or inflammatory cell numbers in BAL fluid over time, even following cumulative treatments. $Avicel-plus^{(R)}$ CM 2159 significantly increased LDH release, detected 3 months after 4 weekly administrations. However, histological results revealed a chronic inflammatory response and tissue alterations, being hypertrophy of pulmonary arteries (observed 3 months after nBCMC treatment) of particular concern. These histological alterations remained after 6 months in animals treated with nBC, possibly due to foreign body reaction and the organism's inability to remove the fibers. Overall, despite being a safe and biocompatible biomaterial, BC-derived nanofibrils inhalation may lead to lung pathology and pose significant health risks.

• International Journal of Industrial Entomology and Biomaterials
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• v.26 no.2
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• pp.81-88
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• 2013

Wet-spun silk fibers have attracted the attention of many researchers because of 1) the unique properties of silk as a biomaterial, including good biocompatibility and cyto-compatability and 2) the various methods available to control the structure and properties of the fiber. Cellulose nanofibrils (CNFs) have typically been used as a reinforcing material for natural and synthetic polymers. In this study, CNF-embedded silk fibroin (SF) nanocomposite fibers were prepared for the first time. The effects of CNF content on the rheology of the dope solution and the characteristics of wet-spun CNF/SF composite fibers were also examined. A 5% SF formic acid solution that contained no CNFs showed nearly Newtonian fluid behavior, with slight shear thinning. However, after the addition of 1% CNFs, the viscosity of the dope solution increased significantly, and apparent shear thinning was observed. The maximum draw ratio of the CNF/SF composite fibers decreased as the CNF content increased. Interestingly, the crystallinity index for the silk in the CNF/SF fibers was sequentially reduced as the CNF content was increased. This phenomenon may be due to the fact that the CNFs prevent ${\beta}$-sheet crystallization of the SF by elimination of formic acid from the dope solution during the coagulation process. The CNF/SF composite fibers displayed a relatively smooth surface with stripes, at low magnification (${\times}500$). However, a rugged nanoscale surface was observed at high magnification (${\times}10,000$), and the surface roughness increased with the CNF content.

• Applied Chemistry for Engineering
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• v.27 no.4
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• pp.380-385
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• 2016

Nanocelluloses, mainly cellulose nanofibrils (CNF) and cellulose nanocrystals (CNC, i.e., defect-free, rod-like crystalline residues after acid hydrolysis of fibers), have been the subject of recent interest. Due to the presence of hydroxyl groups on the surface of nanocelluloses, their surfaces are reactive, making them suitable candidates for reinforcing materials for manufacturing polymer composites. In this study, CNF was used as a reinforcing material for manufacturing cement composites. CNF was prepared by TEMPO (2,2,6,6,-tetramethyl piperidine-1-oxyl radical) oxidation procedure combined with extensive homogenization and ultrasonication. Transmission electron microscopy (TEM) analysis of the suspension showed the width of CNF between 10 and 15 nm. The compressive strength of cement composites containing 0.5% CNF was comparable to that of conventional cement composites. On the other hand, the tensile and flexural strength were improved by 49.7% and 38.8%, respectively, compared to those of conventional cement composites. Also, at an ambient condition, the degree of self-shrinkage reduction reached to 18.9% in one day, followed by 5.9% in 28 days after molding.

• Current Research on Agriculture and Life Sciences
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• v.31 no.4
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• pp.250-255
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• 2013

As a renewable nanomaterial, cellulose nanocrystal (CNC) isolated from wood grants excellent mechanical properties in developing high performance nanocomposites. This study was undertaken to compare the reinforcing efficiency of two different CNCs, i.e., cellulose nanowhiskers (CNWs) and cellulose nanofibrils (CNFs) from hardwood bleached kraft pulp (HW-BKP) as reinforcing agent in polyvinyl alcohol (PVA)-based nanocomposite. The CNWs were isolated by sulfuric acid hydrolysis while the CNFs were isolated by 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO)-mediated oxidation. Based on measurements using transmission electron microscopy, the individual CNWs were about $6.96{\pm}0.87nm$ wide and $178{\pm}55nm$ long, while CNFs were $7.07{\pm}0.99nm$ wide. The incorporation of CNWs and CNFs into the PVA matrix at 5% and 1% levels, respectively, resulted in the maximum tensile strength, indicating different efficiencies of these CNCs in the nanocomposites. Therefore, these results suggest a relationship between the reinforcing potential of CNCs and their physical characteristics, such as their morphology, dimensions, and aspect ratio.

• Journal of the Korean Wood Science and Technology
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• v.49 no.2
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• pp.169-180
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• 2021

Inherent crystalline domains present in low formaldehyde to urea (F/U) molar ratio urea-formaldehyde (UF) resins are responsible for their poor adhesion in wood-based composite panels. To modify the crystallinity of low molar ratio (LMR) UF resins, this study investigates the additional effect of cellulose nanomaterials (CNMs), such as cellulose microfibrils (CMFs), cellulose nanofibrils (CNFs), and TEMPO-oxidized CNFs (TEMPO-CNFs) on the crystallinity of modified LMR UF resins. First, two modification methods (post-mixing and in situ) were compared for modified LMR UF resins with TEMPO-CNFs. The modified UF resins with TEMPO-CNFs decreased the nonvolatile solid contents, while increasing the viscosity and gel time. However, the in situ modification of UF resins with TEMPO-CNFs showed lower crystallinity than that of post-mixing. Then, the in situ method was compared for all CNMs to modify LMR UF resins. The modified UF resins with CMFs using the in situ method increased nonvolatile solid contents and viscosity but decreased the gel time. The crystallinity of UF resins modified with TEMPO-CNFs was the lowest even though the crystalline domains were not significantly changed for all modified UF resins. These results suggest that these CNMs should be modified to prevent the formation of crystalline domains in LMR UF resins.

• Journal of Microbiology and Biotechnology
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• v.32 no.11
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• pp.1479-1484
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• 2022

Bacterial cellulose (BC) is gaining attention as a carbon-neutral alternative to plant cellulose, and as a means to prevent deforestation and achieve a carbon-neutral society. However, the high cost of fermentation media for BC production is a barrier to its industrialization. In this study, chestnut shell (CS) hydrolysates were used as a carbon source for the BC-producing bacteria strain, Gluconacetobacter xylinus ATCC 53524. To evaluate the suitability of the CS hydrolysates, major inhibitors in the hydrolysates were analyzed, and BC production was profiled during fermentation. CS hydrolysates (40 g glucose/l) contained 1.9 g/l acetic acid when applied directly to the main medium. As a result, the BC concentration at 96 h using the control group and CS hydrolysates was 12.5 g/l and 16.7 g/l, respectively (1.3-fold improved). In addition, the surface morphology of BC derived from CS hydrolysates revealed more densely packed nanofibrils than the control group. In the microbial BC production using CS, the hydrolysate had no inhibitory effect during fermentation, suggesting it is a suitable feedstock for a sustainable and eco-friendly biorefinery. To the best of our knowledge, this is the first study to valorize CS by utilizing it in BC production.

• Journal of the Korean Wood Science and Technology
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• v.45 no.3
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• pp.268-277
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• 2017

In this study, lignocellulose nanofibrils (LCNFs) were prepared from Pussy willow wood powder by disk-milling after pretreatment using the cosolvent of 1-ethyl-3-methylimidazolium acetate ([EMIM]Ac) and N,N-dimethylformamide (DMF) with different mixing ratios for different time. All pretreated samples showed native cellulose I polymorph and cellulose crystallinity was lowest when cosolvent of DMF with 30% [EMIM]Ac was used. Average crystallite size of raw material and the pretreated product by MDF and its cosolvent with 10% [EMIM]Ac was found to be about 3.2 nm and decreased with increasing pretreatment time at the DMF cosolvent with 30% [EMIM]Ac. Defibrillation efficiency was improved by loosening wood cell wall structure by the pretreatment using co-solvent system of [EMIM]Ac and DMF.