Search Results (75)

UiO-66-NH₂ is a metal–organic framework (MOF) with open metal sites, making it a promising candidate for adsorption and catalysis. However, the powdery texture of MOFs and the use of toxic solvents during synthesis limit their application. A novel solution to this issue is to create a layered porous composite by encasing the MOF within a flexible and structurally robust aerogel substrate using safe, eco-friendly, and green solvents such as ethanol. The fibrous MOF aerogels, characterized by a desirable macroscopic shape of cylindrical block and hierarchical porosity, were synthesized by two approaches: in situ growth of amine-functionalized UiO-66-NH₂ crystals on a TEMPO-oxidized cellulose nanofiber (TOCNF) and ex situ crosslinking of UiO-66-NH₂ crystals onto a TOCNF network to form UiO-66-NH₂/TOCNF. The incorporation of MOF into the cellulose nanofibrils via the in situ method reduces their aggregation potential, alters the nucleation/growth balance to produce smaller MOF crystals, and enhances mechanical flexibility, as evidenced by SEM images. The three adsorbents, including UiO-66-NH₂, ex situ UiO-66-NH₂/TOCNF, and in situ UiO-66-NH₂/TOCNF, were synthesized and used in this study. The effects of pH, time, temperature, and initial concentration were studied. A maximum adsorption capacity (Qmax) of 549.45 mg/g for Congo Red (CR) and 171.23 mg/g for Orange II (ORII) was observed at pH 6, using 10 mg of in situ UiO-66-NH₂/TOCNF at 40 °C with a contact time of 75 min for CR and 2 h for ORII. The adsorption of both dyes primarily occurs through monolayer chemisorption on the in situ UiO-66-NH₂/TOCNF. The main removal mechanisms were hydrogen bonding and surface complexation. The noteworthy adsorption capacity of in situ UiO-66-NH₂/TOCNF coupled with environment-friendly fabrication techniques indicates its potential applications on a large scale in real wastewater systems. Full article

To address the pollution issues of industrial oily wastewater and catering industry wastewater, a series of Ti₃C₂T_x/TEMPO oxidized cellulose nanofibers composite aerogels with varying Ti₃C₂T_x content were successfully prepared using liquid nitrogen non-directional and directional freezing methods, with Ti₃C₂T_x and TEMPO oxidized cellulose nanofibers (TOCNF) as the main raw materials. The prepared samples were then hydrophobically modified using methyltrichlorosilane (MTCS) via chemical vapor deposition (CVD). The results showed that the directional Ti₃C₂T_x/TOCNF composite aerogel had the most orderly SEM morphology. The hydrophobic Ti₃C₂T_x/TOCNF composite aerogels exhibited efficient adsorption separation capabilities, with an adsorption capacity ranging from 21.5 to 78.2 times their own mass. Notably, the oil absorption performance was optimal when the mass fraction of Ti₃C₂T_x was 33.3%. After five adsorption cycles, the adsorption capacity of M5C10 (with a mass ratio of Ti₃C₂T_x to TOCNF of 5:10) only decreased by around 11%. M5C10 exhibits highly efficient oil absorption performance, which is of considerable significance for the research on oil-water separation treatment of industrial wastewater, domestic wastewater, and sewage from the catering industry. Full article

Cellulose nanofibers (NF) were extracted from kapok fibers using TEMPO oxidation, followed by a combination of mechanical grinding and ultrasonic processing. The TEMPO-mediated oxidation significantly impacted the mechanical disintegration behavior of the kapok fibers, resulting in a high NF yield of 98%. This strategy not only improved the fibrillation efficiency but also reduced overall energy consumption during NF preparation. An ultralight and highly porous NF-based aerogel was successfully prepared using a simple ice-templating technique. It had a low density in the range of 3.5–11.2 mg cm⁻³, high compressional strength (160 kPa), and excellent thermal insulation performance (0.024 W m⁻¹ K⁻¹). After silane modification, the aerogel displayed an ultralow density of 7.9 mg cm⁻³, good hydrophobicity with a water contact angle of 128°, and excellent mechanical compressibility with a high recovery of 92% at 50% strain. Benefiting from the silene support structure, it showed a high oil absorptive capacity (up to 71.4 g/g for vacuum pump oil) and a remarkable oil recovery efficiency of 93% after being reused for 10 cycles. These results demonstrate that our strategy endows nanocellulose-based aerogels with rapid shape recovery and high liquid absorption capabilities. Full article

Dye/salt separation has gained increasing attention in recent years, prompting the quest to find cost-effective and environmentally friendly raw materials for synthesizing high performance nanofiltration (NF) membrane for effective dye/salt separation. Herein, a high-performance loose-structured NF membrane was fabricated via a simple vacuum filtration method using a green nanomaterial, 2,2,6,6-tetramethylpiperidine-1-oxide radical (TEMPO)-oxidized cellulose nanofiber (TOCNF), by sequentially filtrating larger-sized and finer-sized TOCNFs on a microporous substrate, followed by crosslinking with trimesoyl chloride. The resulting TCM membrane possessed a separating layer composed entirely of pure TOCNF, eliminating the need for other polymer or nanomaterial additives. TCM membranes exhibit high performance and effective dye/salt selectivity. Scanning Electron Microscope (SEM) analysis shows that the TCM membrane with the Fine-TOCNF layer has a tight layered structure. Further characterizations via Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) confirmed the presence of functional groups and chemical bonds of the crosslinked membrane. Notably, the optimized TCM-5 membrane exhibits a rejection rate of over 99% for various dyes (Congo red and orange yellow) and 14.2% for NaCl, showcasing a potential candidate for efficient dye wastewater treatment. Full article

Nanocellulose fiber materials were considered promising biomaterials due to their excellent biodegradability, biocompatibility, high hydrophilicity, and cost-effectiveness. However, their low proton conductivity significantly limited their application as proton exchange membranes. The methods previously reported to increase their proton conductivity often introduced non-biodegradable groups and compounds, which resulted in the loss of the basic advantages of this natural polymer in terms of biodegradability. In this work, a green and sustainable strategy was developed to prepare cellulose-based proton exchange membranes that could simultaneously meet sustainability and high-performance criteria. Adenine and thymine were introduced onto the surface of tempo-oxidized nanocellulose fibers (TOCNF) to provide many transition sites for proton conduction. Once modified, the proton conductivity of the TOCNF membrane increased by 31.2 times compared to the original membrane, with a specific surface area that had risen from 6.1 m²/g to 86.5 m²/g. The wet strength also increased. This study paved a new path for the preparation of environmentally friendly membrane materials that could replace the commonly used non-degradable ones, highlighting the potential of nanocellulose fiber membrane materials in sustainable applications such as fuel cells, supercapacitors, and solid-state batteries. Full article

Nanocellulose materials have been widely used in biomedicine, food packaging, aerospace, composite material, and other fields. In this work, cellulose obtained from Camellia shells through alkali boiling and subbleaching was micro-dissolved and regenerated using the DMAc (N,N-Dimethylacetamide)/LiCl system, and TOCNs (TEMPO-oxidized cellulose nanofibers) with different degrees of oxidation. The membrane was prepared by filtration of polytetrafluoroethylene (pore size 0.1 μm), and the oxidized nanocellulose film was obtained after drying, Then, the crystallinity, mechanical properties and oxygen barrier properties of the TOCN film were investigated. Furthermore, based on TS (tea saponin) from Camellia oleifera seed cake and TOCNs, TS-TOCN film was prepared by the heterogeneous reaction. The TS-TOCN film not only shows excellent oxygen barrier properties (the oxygen permeability is 2.88 cc·m⁻²·d⁻¹) but also has good antibacterial effects on both Gram-negative and Gram-positive bacteria. The antibacterial property is comparable to ZnO-TOCN with the same antibacterial content prepared by the in-situ deposition method. Antioxidant activity tests in vitro showed that TS-TOCN had a significant scavenging effect on DPPH (2,2-Diphenyl-1-picrylhydrazyl) radicals. This design strategy makes it possible for inexpensive and abundant Camellia oleifera remainders to be widely used in the field of biobased materials. Full article

Biodegradable mulching films are a very attractive solution to agronomical practices intended to achieve more successful crop results. And, in this context, the employment of agricultural and industrial food residues as starting material for their production is an alternative with economic and environmental advantages. This work reports the preparation of bilayer films having two different wettability characteristics from three bio-derived biopolymers: TEMPO-oxidized cellulose nanofibers isolated from infused Yerba Mate residues, Chitosan and Polylactic acid. The infused Yerba Mate residues, the isolated and oxidized cellulose nanofibers, and the films were characterized. Nanofibrillation yield, optical transmittance, cationic demand, carboxyl content, intrinsic viscosity, degree of polymerization, specific surface area and length were studied for the (ligno)cellulose nanofibers. Textural and chemical analysis, thermal and mechanical properties studies, as well as water and light interactions were included in the characterization of the films. The bilayer films are promising materials to be used as mulching films. Full article

In this study, the wear resistance of nickel (Ni)–cellulose nanofiber (CNF) composite electroplated films on steel plates (JIS SPCC, cold-rolled steel) was evaluated, including their surface and microstructural properties. In the CNF sample, 2,2,6,6-tetramethylpiperidine 1-oxyl (TEMPO)-oxidized CNF was used. As a result of the ball-on-disk abrasion test, in which steel (SUJ2) balls were used as the counterpart material, the plated film obtained with the addition of 1 g/L of CNF to the plating solution showed the highest wear resistance in this study. Compared to the conventional Ni-plated film without CNF, the abrasion loss volume on the plated side was reduced by approximately 79%, and that on the ball side was reduced remarkably by 94%. A microstructural analysis of the abrasion scars showed areas where co-deposited CNFs were stretched in the direction of abrasion, suggesting that the wear reduction effect was caused by sliding between the individual CNFs within the aggregates. Moreover, the hardness of the plated film increased when the Ni crystallite size became finer. It was confirmed that the co-deposition of fine CNFs is effective in improving hardness, whereas the co-deposition of a certain degree of aggregated CNFs is effective in exhibiting the wear reduction effect. Full article

(1) Background: Nanostructured cellulose has emerged as an efficient bio-adsorbent aerogel material, offering biocompatibility and renewable sourcing advantages. This study focuses on isolating (ligno)cellulose nanofibers ((L)CNFs) from barley straw and producing aerogels to develop sustainable and highly efficient decontamination systems. (2) Methods: (Ligno)cellulose pulp has been isolated from barley straw through a pulping process, and was subsequently deconstructed into nanofibers employing various pre-treatment methods (TEMPO-mediated oxidation process or PFI beater mechanical treatment) followed by the high-pressure homogenization (HPH) process. (3) Results: The aerogels made by (L)CNFs, with a higher crystallinity degree, larger aspect ratio, lower shrinkage rate, and higher Young’s modulus than cellulose aerogels, successfully adsorb and remove organic dye pollutants from wastewater. (L)CNF-based aerogels, with a quality index (determined using four characterization parameters) above 70%, exhibited outstanding contaminant removal capacity over 80%. The high specific surface area of nanocellulose isolated using the TEMPO oxidation process significantly enhanced the affinity and interactions between hydroxyl and carboxyl groups of nanofibers and cationic groups of contaminants. The efficacy in adsorbing cationic dyes in wastewater onto the aerogels was verified by the Langmuir adsorption isotherm model. (4) Conclusions: This study offers insights into designing and applying advanced (L)CNF-based aerogels as efficient wastewater decontamination and environmental remediation platforms. Full article

Nanofibrillated cellulose was extracted from potato peel waste using a fast and green method with a simple process. To extract cellulose and eliminate non-cellulosic constituents, alkaline and hydrogen peroxide treatments were performed under microwave irradiation. The nanofibrillated cellulose was extracted from purified cellulose via TEMPO oxidation followed by ultrasonication. The TEM, FTIR, XRD, and TGA experiments were used to evaluate the structural, crystalline, and thermal properties of cellulose fiber and nanofiber. The chemical and FTIR analysis of bleached fibers indicates that almost all non-cellulosic components of biomass have been eliminated. The diameter of the extracted nanofibers is in the range of 4 to 22 nm. In terms of crystallinity, extracted nanocellulose had 70% crystallinity, compared to 17% for unprocessed lignocellulose fibers, which makes it an excellent choice for use as a reinforcement phase in biobased composites. Thermogravimetric analysis reveals that cellulose nanofibers are less thermally stable than potato peel pure cellulose, but it has a higher char content (28%) than pure cellulose (6%), which signifies that the carboxylate functionality acts as a flame retardant. The comparison between cellulose derived from microwave and conventional extraction methods confirmed that their impact on the removal of non-cellulosic materials is nearly identical. Full article

An innovative colloidal approach is proposed here to carry out the customized functionalization of TEMPO-Oxidized Cellulose Nanofibers (CNF) incorporating non-noble inorganic nanoparticles. A heterocoagulation process is applied between the delignified CNF and as-synthetized CuO nanoparticles (CuO NPs) to formulate mixtures which are used in the preparation of aerogels with antibacterial effect, which could be used to manufacture membranes, filters, foams, etc. The involved components of formulated blending, CNF and CuO NPs, were individually obtained by using a biorefinery strategy for agricultural waste valorization, together with an optimized chemical precipitation, assisted by ultrasounds. The optimization of synthesis parameters for CuO NPs has avoided the presence of undesirable species, which usually requires later thermal treatment with associated costs. The aerogels-based structure, obtained by conventional freeze-drying, acted as 3D support for CuO NPs, providing a good dispersion within the cross-linked structure of the nanocellulose and facilitating direct contact of the antibacterial phase against undesirable microorganisms. All samples showed a positive response against Escherichia coli and Staphylococcus aureus. An increase of the antibacterial response of the aerogels, measured by agar disk diffusion test, has been observed with the increase of CuO NPs incorporated, obtaining the width of the antimicrobial “halo” (nw_halo) from 0 to 0.6 and 0.35 for S. aureus and E. coli, respectively. Furthermore, the aerogels have been able to deactivate S. aureus and E. coli in less than 5 h when the antibacterial assays have been analyzed by a broth dilution method. From CNF-50CuO samples, an overlap in the nanoparticle effect produced a decrease of the antimicrobial kinetic. Full article

Inspired by the principles of the circular economy, using vineyard pruning residues as a source of raw materials for producing nanocellulose is a promising approach to transforming vineyard resources into value-added products. This study aimed to obtain and characterize cellulose and cellulose nanofibers from such sources. The cellulose collected from different fractions of micronized stems (500, 300, 150 μm, and retain) of vines was submitted to autohydrolysis and finally bleached. Soon, it underwent treatment via (2,2,6,6-tetrametil-piperidi-1-nil)oxil (TEMPO) oxidation and ultrasonic to obtain nanocellulose fibers. The cellulose films were obtained at a microscale thickness of 0.05 ± 0.00; 0.37 ± 0.03; 0.06 ± 0.01 e 0.030 ± 0.01 mm, with the following particle size: 500 µm, 300 µm, 150 µm, and retain (<150 µm). The bleaching efficiency of the cellulose fibers of each particle size fraction was evaluated for color through a colorimeter. In addition, the extraction of cellulose fibers was assessed by infrared with Fourier transform, and size and shape were assessed by microscopy. Differential scanning calorimetry and X-ray diffraction were performed to confirm the thermal and crystalline properties. Combining autohydrolysis with a bleaching step proved to be a promising and ecological alternative to obtain white fractions rich in cellulose. It was possible to perform the extraction of cellulose to obtain nanocellulose fibers from vine pruning residues for the development of coatings for the conservation of heritage buildings from environmental conditions through an environmentally friendly process. Full article

The cost-effective implementation of nanofibrillated cellulose (CNF) at industrial scale requires optimizing the quality of the nanofibers according to their final application. Therefore, a portfolio of CNFs with different qualities is necessary, as well as further knowledge about how to obtain each of the main qualities. This paper presents the influence of various production techniques on the morphological characteristics and properties of CNFs produced from a mixture of recycled fibers. Five different pretreatments have been investigated: a mechanical pretreatment (PFI refining), two enzymatic hydrolysis strategies, and TEMPO-mediated oxidation under two different NaClO concentrations. For each pretreatment, five high-pressure homogenization (HPH) conditions have been considered. Our results show that the pretreatment determines the yield and the potential of HPH to enhance fibrillation and, therefore, the final CNF properties. These results enable one to select the most effective production method with the highest yield of produced CNFs from recovered paper for the desired CNF quality in diverse applications. Full article

The surface modification of cellulose nanofibers (CNFs) using a 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO)/sodium bromide (NaBr)/sodium hypochlorite (NaClO) system was successful in improving their hydrophilicity. Following that, we fabricated hydrogels containing carboxylated cellulose nanofibers (c-CNFs) and loaded them with polyhexamethylene biguanide (PHMB) using a physical crosslinking method, aiming for efficient antimicrobial uses. The morphological and physicochemical properties of all hydrogel formulations were characterized, and the results revealed that the 7% c-CNFs-2 h loaded with PHMB formulation exhibited desirable characteristics such as regular shape, high porosity, good mechanical properties, suitable gel content, and a good maximum swelling degree. The successful integration of PHMB into the c-CNF matrix was confirmed by FTIR analysis. Furthermore, the 7% c-CNFs-2 h loaded with the PHMB formulation demonstrated PHMB contents exceeding 80% and exhibited a prolonged drug release pattern for up to 3 days. Moreover, this formulation displayed antibacterial activity against S. aureus and P. aeruginosa. In conclusion, the novel approach of c-CNF hydrogels loaded with PHMB through physical crosslinking shows promise as a potential system for prolonged drug release in topical drug delivery while also exhibiting excellent antibacterial activity. Full article

Beeswax is a bio-sourced, renewable, and even edible material that stands as a convincing option to provide paper-based food packaging with moisture resistance. Nonetheless, the difficulty of dispersing it in water limits its applicability. This work uses oxidized, negatively charged cellulose nanofibers along with glycerol to stabilize beeswax-in-water emulsions above the melting point of the wax. The synergistic effects of nanocellulose and glycerol granted the stability of the dispersion even when it cooled down, but only if the concentration of nanofibers was high enough. This required concentration (0.6–0.9 wt%) depended on the degree of oxidation of the cellulose nanofibers. Rheological hindrance was essential to prevent the buoyancy of beeswax particles, while the presence of glycerol prevented excessive aggregation. The mixtures had yield stress and showed pseudoplastic behavior at a high enough shear rate, with their apparent viscosity being positively influenced by the surface charge density of the nanofibers. When applied to packaging paper, the nanocellulose-stabilized beeswax suspensions not only enhanced its barrier properties towards liquid water (reaching a contact angle of 96°) and water vapor (<100 g m⁻² d⁻¹), but also to grease (Kit rating: 5) and airflow (>1400 Gurley s). While falling short of polyethylene-coated paper, this overall improvement, attained using only one layer of a biobased coating suspension, should be understood as a step towards replacing synthetic waxes and plastic laminates. Full article