Search Results (26)

Cellulose is a versatile biopolymer increasingly applied in medicine and industry due to its biodegradability and biocompatibility, along with the renewability and large availability of source materials. However, finding simple, eco-friendly, and effective methods to modify cellulose to provide it with new functionalities remains a challenge. This work presents a new, inexpensive, and eco-friendly method to chemically modify microcrystalline cellulose (MCC) by the submerged cold plasma treatment of an aqueous suspension of MCC containing different oxidizing agents, such as hydrogen peroxide (H₂O₂), sodium hypochlorite (NaClO), or sodium periodate (NaIO₄). Fourier-transform Infrared (FTIR) and X-ray photoelectron spectroscopy (XPS) showed that plasma treatment intensified the oxidizing effect of H₂O₂, NaClO, and NaIO₄, with plasma-assisted NaClO treatment yielding the highest MCC oxidation level. XPS indicated that the plasma-assisted oxidations also resulted in different degrees of chemical degradation of MCC, a finding further supported by the thermogravimetric analysis (TGA) results. X-ray diffraction (XRD) data revealed a different effect of the oxidizing agents on the crystalline and amorphous regions in MCC. Scanning electron microscopy (SEM) images showed that the combined treatment with plasma and chemical oxidizing agents led to MCC fragmentation and varying degrees of defibrillation into nanofibers. Full article

Blackcurrant pomace (BCP) is an example of an annual, high-volume, under-utilized renewable resource with potential to generate chemicals, materials and bioenergy within the context of a zero-waste biorefinery. Herein, the microwave-assisted isolation, characterization and potential application of defibrillated lignocelluloses from depectinated blackcurrant pomace are reported. Depectination was achieved using citric acid (0.2–0.8 M, 80 °C, 2 h, conventional heating) and compared with acid-free hydrothermal microwave-assisted processing (1500 W, 100–160 °C, 30 min). The resultant depectinated residues were subjected to microwave-assisted hydrothermal defibrillation to afford two classes of materials: namely, (i) hydrothermal acid-free microwave-assisted (1500 W, 160 °C, 30 min; DFC-M1-M4), and (ii) hydrothermal citric acid microwave-assisted (1500 W, 160 °C, 30 min; DFC-C1–C4). Thermogravimetric analysis (TGA) revealed that the thermal stability with respect to native BCP (T_d = 330 °C) was higher for DFC-M1-M4 (T_d = 345–348 °C) and lower for DFC-C1–C4 (322–325 °C). Both classes of material showed good propensity to hold water but failed to form stable hydrogels (5–7.5 wt% in water) unless they underwent bleaching which removed residual lignin and hemicellulosic matter, as evidenced by ¹³C solid-state NMR spectroscopy. The hydrogels made from bleached DFC-C1–C4 (7.5 wt%) and bleached DFC-M1-M4 (5 wt%) exhibited rheological viscoelastic, shear thinning, and time-dependent behaviour, which highlights the potential opportunity afforded by microwave-assisted defibrillation of BCP for food applications. Full article

Cellulose produced by bacteria (BC) is considered a promising material for the textile industry, but the fragile and sensitive nature of BC membranes limits their broad applicability. Production of all-cellulose biocomposites, in which the BC is cultivated in situ on a cotton fabric, could solve this problem, but here a new issue arises, namely poor adhesion. To overcome this challenge, cotton fabric was modified with low-pressure oxygen plasma in either afterglow, E-mode, or H-mode. All-cellulose biocomposites were prepared in situ by placing the samples of cotton fabric in BC culture medium and incubating for 7 days to allow BC microfibril networks to form on the fabric. Modification of cotton fabric with oxygen plasma afterglow led to additional functionalization with polar groups, and modification with oxygen plasma in H-mode led also to etching and surface roughening of the cotton fibers, which improved the adhesion within the biocomposite. In addition, these biocomposites showed higher deformation capacities. Modification of the cotton fabric over a longer period in E-mode was found to be unsuitable, as this caused strong etching, which led to the defibrillation of cotton fibers and poor adhesion of BC. This study highlights the potential of low-pressure plasma treatment as an environmentally friendly method to improve the performance of cellulose-based biocomposites. Full article

Alpha-cellulose, a unique, natural, and essential polymer for the fiber industry, was isolated in an ecofriendly manner using eleven novel systems comprising recycling, defibrillation, and delignification of prosenchyma cells (vessels and fibers) of ten lignocellulosic resources. Seven hardwood species were selected, namely Conocorpus erectus, Leucaena leucocephala, Simmondsia chinensis, Azadirachta indica, Moringa perigrina, Calotropis procera, and Ceiba pentandra. Moreover, three recycled cellulosic wastes were chosen due to their high levels of accumulation annually in the fibrous wastes of Saudi Arabia, namely recycled writing papers (RWPs), recycled newspapers (RNPs), and recycled cardboard (RC). Each of the parent samples and the resultant alpha-cellulose was characterized physically, chemically, and anatomically. The properties examined differed significantly among the ten resources studied, and their mean values lies within the cited ranges. Among the seven tree species, L. leucocephala was the best cellulosic precursor due to its higher fiber yield (55.46%) and holocellulose content (70.82%) with the lowest content of Klasson lignin (18.86%). Moreover, RWP was the best α-cellulose precursor, exhibiting the highest holocellulose (87%) and the lowest lignin (2%) content. Despite the high content of ash and other additives accompanied with the three lignocellulosic wastes that were added upon fabrication to enhance their quality (10%, 11%, and 14.52% for RWP, RNP, and RC, respectively), they can be considered as an inexhaustible treasure source for cellulose production due to the ease and efficiency of discarding their ash minerals using the novel CaCO₃-elimination process along with the other innovative techniques. Besides its main role for adjusting the pH of the delignification process, citric acid serves as an effective and environmentally friendly additive enhancing lignin breakdown while preserving cellulose integrity. Comparing the thermal behavior of the ten cellulosic resources, C. procera and C. pentandra exhibited the highest moisture content and void volume as well as having the lowest specific gravity, crystallinity index, and holocellulose content and were found to yield the highest mass loss during their thermal degradation based on thermogravimetric and differential thermal analysis in an inert atmosphere. However, the other resources used were found to yield lower mass losses. The obtained results indicate that using the innovative procedures of recycling, defibrillation, and delignification did not alter or distort either the yield or structure of the isolated α-cellulose. This is a clear indicator of their high efficiency for isolating cellulose from lignocellulosic precursors. Full article

Cellulose-based aerogel has attracted considerable attention for its excellent adsorption capacity, biodegradability, and renewability. However, it is considered eco-unfriendly due to defibrillation of agriculture waste and requires harmful/expensive chemical agents. In this study, cornstalk rind-based aerogel was obtained via the following steps: green H₂O₂/HAc delignification of cornstalk rind to obtain cellulose fibers, binding with carboxymethyl cellulose (CMC)/polyvinyl alcohol (PVA) and freeze-drying treatment, and hydrophobic modification with stearic acid. The obtained aerogel showed high compressive strength (200 KPa), which is apparently higher (about 32 kPa) than NaClO-delignified cornstalk-based cellulose/PVA aerogel. Characterization of the obtained aerogel through SEM, water contact angle, etc., showed high porosity (95%), low density (0.0198 g/cm⁻³), and hydrophobicity (water contact angle, 159°), resulting in excellent n-hexane adsorption capacity (35 g/g), higher (about 29.5 g/g) than NaClO-delignified cornstalk-based cellulose/PVA aerogel. The adsorbed oil was recovered by the extrusion method, and the aerogel showed excellent recyclability in oil adsorption. Full article

Defibrillating cellulose through various grinding steps and incorporating it into hydrogels introduces unique properties that warrant thorough exploration. This study investigates cellulose defibrillation at different steps (15–120) using an ultra-fine friction grinder, blended with high-molecular-weight polyvinyl alcohol (PVA), and crosslinked via freeze–thawing. A critical discovery is the influence of defibrillation on the hydrogel structure, as evidenced by reduced crystallinity, thermal degradation, and the enhanced swelling of PVA chains. Despite an increased elastic modulus of up to 120 steps, the synthesized material maintains remarkable strength under hydrated conditions, holding significant promise in biomaterial applications. Full article

This work proposes a biorefinery approach for utilizing tomato pomace (TP) through a top-down deconstructing strategy, combining mild chemical hydrolysis with high-pressure homogenization (HPH). The objective of the study is to isolate cellulose pulp using different combinations of chemical and physical processes: (i) direct HPH treatment of the raw material, (ii) HPH treatment following acid hydrolysis, and (iii) HPH treatment following alkaline hydrolysis. The results demonstrate that these isolation routes enable the production of cellulose with tailored morphological properties from TP with higher yields (up to +21% when HPH was applied before hydrolysis and approximately +6% when applied after acid or after alkaline hydrolysis). Additionally, the side streams generated by this cascade process show a four-fold increase in phenolic compounds when HPH is integrated after acid hydrolysis compared to untreated sample, and they also contain nanoparticles composed of hemicellulose and lignin, as shown by FT-IR and SEM. Notably, the further application of HPH treatment enables the production of nanostructured cellulose from cellulose pulp derived from TP, offering tunable properties. This approach presents a sustainable pathway for the extraction of cellulose and nanocellulose, as well as the valorization of value-added compounds found in residual biomass in the form of side streams. Full article

The exploitation of unavoidable food supply chain wastes resulting from primary and secondary processing for chemicals, materials, and bioenergy is an important concept in the drive towards circular-based, resource-efficient biorefineries rather than petroleum refineries. The potential production of hydrogels (materials) from unavoidable food supply chain wastes, which are naturally rich in biopolymers such as cellulose, hemicellulose, pectin, and lignin, represents an interesting opportunity. However, these intertwined and interconnected biopolymers require separation and deconstruction prior to any useful application. Thus, this study aims to explore the formation of hydrogels from defibrillated celluloses (MW-DFCs) produced via acid-free stepwise microwave hydrothermal processing of blackcurrant pomace residues. Initially, pectin was removed from blackcurrant pomace residues (MW, 100–160 °C), and the resultant depectinated residues were reprocessed at 160 °C. The pectin yield increased from 2.36 wt.% (MW, 100 °C) to 3.07 wt.% (MW, 140 °C) and then decreased to 2.05 wt.% (MW, 160 °C). The isolated pectins were characterized by attenuated total reflectance infrared spectroscopy (ATR-IR), thermogravimetric analysis (TGA), and ¹³C NMR (D₂O). The cellulosic-rich residues were reprocessed (MW, 160 °C) and further characterized by ATR-IR, TGA, and Klason lignin analysis. All the MW-DFCs contained significant lignin content, which prevented hydrogel formation. However, subsequent bleaching (H₂O₂/OH⁻) afforded off-white samples with improved gelling ability at the concentration of 5% w/v. Confocal laser microscopy (CLSM) revealed the removal of lignin and a more pronounced cellulosic-rich material. In conclusion, the microwave-assisted defibrillation of blackcurrant pomace, an exploitable unavoidable food supply chain waste, affords cellulosic-rich materials with the propensity to form hydrogels which may serve useful applications when put back into food products, pharmaceuticals, cosmetics, and home and personal care products. Full article

In order to enhance the performance of the epoxy resin-prepared materials, straw fiber was used as the reinforcing base in this study. The principle of this study is to use the cellulose component exposed after the defibrillation of straw fiber can be further combined with the epoxy group. Firstly, the degree of defibrillation of straw fiber under three different pretreatment methods of acid, alkali and moist heat treatment was explored, and a control test was conducted with untreated straw fiber, which showed that the defibrillation of the straw fiber after alkali treatment was better than the other two methods. Secondly, to prove the comprehensive effect of the pretreatment method and straw fiber filling amount on the composite material performance, this paper carried out a tensile, bending, density and water absorption test. The results showed that when the straw fiber filling was 15%, the best performance of the composites was achieved by the alkali treatment, with tensile strength and tensile modulus reaching 1.89 KN and 3.92 MPa, bending strength and bending modulus reaching 2.00 KN and 81.65 MPa, average water absorption reaching 2.77%, and density reaching 0.957 g/cm³. Finally, the results were verified using Image J software was used for verification. After comparison, the material meets the basic requirements of high-density fiberboard material and provides a reference for preparing straw epoxy resin composites. Full article

In this work, cellulose nanofibers (CNF) were surface treated by plasma and grafted with poly(ethylene glycol)methyl ether methacrylate (PEGMMA) for increasing mechanical strength and hydrophobicity. The surface characteristics of the sponges were studied by scanning electron microscopy, micro-computed tomography, and Fourier transform infrared spectroscopy, which demonstrated successful surface modification. Plasma treatment applied to CNF suspension led to advanced defibrillation, and the resulting sponges (CNFpl) exhibited smaller wall thickness than CNF. The grafting of PEGMMA led to an increase in the wall thickness of the sponges and the number of larger pores when compared with the non-grafted counterparts. Sponges with increased hydrophobicity demonstrated by an almost 4 times increase in the water contact angle and better mechanical strength proved by 2.5 times increase in specific compression strength were obtained after PEGMMA grafting of plasma treated CNF. Cells cultivated on both neat and PEGMMA-grafted CNF sponges showed high viability (>99%). Remarkably, CNF grafted with PEGMMA showed better cell viability as compared with the untreated CNF sample; this difference is statistically significant (p < 0.05). In addition, the obtained sponges do not trigger an inflammatory response in macrophages, with TNF-α secretion by cells in contact with CNFpl, CNF-PEGMMA, and CNFpl-PEGMMA samples being lower than that observed for the CNF sample. All these results support the great potential of cellulose nanofibers surface treated by plasma and grafted with PEGMMA for biomedical applications. Full article

Carbotrace 480 is a commercially available fluorescent optotracer that specifically binds to cellulose’s glycosidic linkages. Herein, the use of Carbotrace 480 is reported as an analytical tool for linking cellulose content to hydrogel formation capability in defibrillated celluloses obtained from proprietary microalgae. Defibrillated celluloses obtained from acid-free hydrothermal microwave processing at low temperature (160 °C) showed poor hydrogel formation attributed to a low cellulose concentration as evidenced through the lack of Carbotrace fluorescence. High temperature (220 °C) processing afforded reasonable gels commensurate with a higher cellulose loading and stronger response to Carbotrace. Full article

This work proposes a biorefinery approach for the utilization of agri-food residues, such as tomato pomace (TP), through combining chemical hydrolysis with high-pressure homogenization (HPH), aiming to achieve the isolation of cellulose with tailored morphological properties from underused lignocellulose feedstocks, along with the valorization of the value-added compounds contained in the biomass. Cellulose was isolated from TP using sequential chemical hydrolysis in combination with mechanical pretreatment through HPH. The chemical and structural features of cellulose isolated from TP pretreated by HPH were compared with cellulose isolated from untreated TP through light scattering for particle size distribution, optical and scanning electron microscopy, and Fourier-transform infrared spectroscopy (FT-IR) analysis. HPH pretreatment (80 MPa, 10 passes) not only promoted a slight increase in the yield of cellulose extraction (+9%) but contributed to directly obtaining defibrillated cellulose particles, characterized by smaller irregular domains containing elongated needle-like fibers. Moreover, the selected mild chemical process produced side streams rich in bioactive molecules, evaluated in terms of total phenols and reducing activity. The liquors recovered from acid hydrolysis of TP exhibited a higher biological activity than those obtained through a conventional extraction (80% v/v acetone, 25 °C, 24 h at 180 rpm). Full article

Cellulose nanofibers (CNFs) are the most advanced bio-nanomaterial utilized in various applications due to their unique physical and structural properties, renewability, biodegradability, and biocompatibility. It has been isolated from diverse sources including plants as well as textile wastes using different isolation techniques, such as acid hydrolysis, high-intensity ultrasonication, and steam explosion process. Here, we planned to extract and isolate CNFs from carpet wastes using a supercritical carbon dioxide (Sc.CO₂) treatment approach. The mechanism of defibrillation and defragmentation caused by Sc.CO₂ treatment was also explained. The morphological analysis of bleached fibers showed that Sc.CO₂ treatment induced several longitudinal fractions along with each fiber due to the supercritical condition of temperature and pressure. Such conditions removed th fiber’s impurities and produced more fragile fibers compared to untreated samples. The particle size analysis and Transmission Electron Microscopes (TEM) confirm the effect of Sc.CO₂ treatment. The average fiber length and diameter of Sc.CO₂ treated CNFs were 53.72 and 7.14 nm, respectively. In comparison, untreated samples had longer fiber length and diameter (302.87 and 97.93 nm). The Sc.CO₂-treated CNFs also had significantly higher thermal stability by more than 27% and zeta potential value of −38.9± 5.1 mV, compared to untreated CNFs (−33.1 ± 3.0 mV). The vibrational band frequency and chemical composition analysis data confirm the presence of cellulose function groups without any contamination with lignin and hemicellulose. The Sc.CO₂ treatment method is a green approach for enhancing the isolation yield of CNFs from carpet wastes and produce better quality nanocellulose for advanced applications. Full article

In the present study, agro-food waste derived rice straw (RS) was valorized into cellulose microfibers (CMFs) using a green process of combined ultrasound and heating treatments and were thereafter used to improve the physical properties of thermoplastic starch films (TPS). Mechanical defibrillation of the fibers gave rise to CMFs with cumulative frequencies of length and diameters below 200 and 5–15 µm, respectively. The resultant CMFs were successfully incorporated at, 1, 3, and 5 wt% into TPS by melt mixing and also starch was subjected to dry heating (DH) modification to yield TPS modified by dry heating (TPSDH). The resultant materials were finally shaped into films by thermo-compression and characterized. It was observed that both DH modification and fiber incorporation at 3 and 5 wt% loadings interfered with the starch gelatinization, leading to non-gelatinized starch granules in the biopolymer matrix. Thermo-compressed films prepared with both types of starches and reinforced with 3 wt% CMFs were more rigid (percentage increases of ~215% for TPS and ~207% for the TPSDH), more resistant to break (~100% for TPS and ~60% for TPSDH), but also less extensible (~53% for TPS and ~78% for TPSDH). The incorporation of CMFs into the TPS matrix at the highest contents also promoted a decrease in water vapor (~15%) and oxygen permeabilities (~30%). Finally, all the TPS composite films showed low changes in terms of optical properties and equilibrium moisture, being less soluble in water than the TPSDH films. Full article

Lignocellulose nanofibrils (LCNFs) with different lignin contents were prepared using choline chloride (ChCl)/lactic acid (LA), deep eutectic solvent (DES) pretreatment, and subsequent mechanical defibrillation. The LCNFs had a diameter of 15.3–18.2 nm, which was similar to the diameter of commercial pure cellulose nanofibrils (PCNFs). The LCNFs and PCNFs were wet-spun in CaCl₂ solution for filament fabrication. The addition of sodium alginate (AL) significantly improved the wet-spinnability of the LCNFs. As the AL content increased, the average diameter of the composite filaments increased, and the orientation index decreased. The increase in AL content improved the wet-spinnability of CNFs but deteriorated the tensile properties. The increase in the spinning rate resulted in an increase in the orientation index, which improved the tensile strength and elastic modulus. Full article