Search Results (676)

Lignin used in this work was isolated from sapele (Entandrophragma cylindricum) wood through a hybrid pulping process using soda/ethanol as pulping liquor and denoted soda-oxyethylated lignin (SOL). SOL was mixed with a polyethylene glycol (PEG)–glycerol mixture (80/20 v/v) as liquefying solvent with 98% wt. sulfur acid as catalyst, and the mixture was taken to boil at 140 °C for 2, 2.5, and 3 h. Three bio-polyols LBP1, LBP2, and LBP3 were obtained, and each of them exhibited a high proportion of -OH groups. Lignin-based polyurethane foams (LBPUFs) were prepared using the bio-polyols obtained with a toluene diisocyanate (TDI) prepolymer by the one-shot method. Gel permeation chromatography (GPC), Fourier transform infrared spectroscopy (FTIR), and carbon-13 nuclear magnetic resonance spectroscopy (¹³C NMR) were used characterize lignin in order to determine viscosity, yield, and composition and to characterize their structure. The PEG-400–glycerol mixture was found to react with the lignin bio-polyols’ phenolic -OHs. The bio-polyols’ viscosity was found to increase as the liquefaction temperature increased, while simultaneously their molecular weights decreased. All the NCO groups were eliminated from the samples, which had high thermal stability as the liquefaction temperature increased, leading to a decrease in cell size, density, and crystallinity and an improvement in mechanical performance. Based on these properties, especially the presence of some aromatic rings in the bio-polyols, the foams produced can be useful in automotive applications and for floor carpets. Full article

Segregative phase separation technology demonstrates substantial potential for precise molecular fractionation in food and biomaterial applications. The investigation elucidates the causal relationship between viscosity variations and phase separation dynamics, which govern molecular fractionation in GA/HPMC composite systems. By conducting a comparative analysis of two GA subtypes (CGA and SGA) and three HPMC grades with controlled viscosity gradients, we utilized gel permeation chromatography-multi-angle laser light scattering (GPC-MALLS) coupled with rheological characterization to elucidate the critical relationship between continuous phase viscosity and fractionation efficiency. Notably, increasing HPMC viscosity significantly intensified phase separation, resulting in selective enrichment of arabinogalactan-protein complexes: from 6.3% to 8.5% in CGA/HPMC systems and from 27.3% to 36.5% in SGA/HPMC systems. Further mechanistic investigation revealed that elevated HPMC viscosity enhances thermodynamic incompatibility while slowing interfacial mass transfer, synergistically driving component redistribution. These findings establish a quantitative viscosity–fractionation relationship, offering theoretical insights for optimizing GA/HPMC systems in emulsion stabilization, microencapsulation, and functional biopolymer purification via viscosity-mediated phase engineering. Full article

Polysodiumoxy(methyl)siloxane is a highly functional polymer matrix that can be used for the preparation of both functional and non-functional polymers, including molecular brushes. To determine the molecular weight parameters of the matrix, as well as its chemical structure, it is necessary to develop an effective method of blocking functional (in our case, sodiumoxy) groups due to their high reactivity. At the same time, the blocking product should represent a complete non-functionalized replica of polysodiumoxy(methyl)siloxane. Since the obtained polysodiumoxy(methyl)siloxane can contain both sodium- and hydroxy groups in its composition, the presence of both types of functional groups should be considered in the blocking process. In this work, we investigated the blocking process of polysodiumoxy(methyl)siloxane and the influence of blocking conditions on the blocked product. We carried out several variants of blocking, which differed in the order and method of introduction of reagents, as well as in the temperature regime. The chemical structure and molecular weight characteristics of the obtained polymers were analyzed by ¹H NMR spectroscopy and gel permeation chromatography (GPC), respectively. According to the blocking results, only in one case, complete non-functionalized replicas of polysodiumoxy(methyl)siloxane were obtained, which allows this technique to be used as a tool for the analysis of complex, highly functionalized organosilicon systems. Full article

The repair efficiency of various self-healing materials often depends on the ability of the prepolymer and curing agent to form mixtures. This paper presents a synthesis and study of the properties of modified self-healing polyurethanes using the Diels–Alder reaction (DA reaction), obtained from a maleimide-terminated preform and a series of furan–urethane curing agents. The most commonly used isocyanates (4,4′-methylene diphenyl diisocyanate (MDI), 2,4-tolylene diisocyanate (TDI), and hexamethylene diisocyanate (HDI)) and furan derivatives (furfurylamine, difurfurylamine, and furfuryl alcohol) were used as initial reagents for the synthesis of curing agents. For comparative analysis, polyurethanes were also obtained using the well-known “traditional” approach—from furan-terminated prepolymers based on mono- and difurfurylamine, as well as furfuryl alcohol and the often-used bismaleimide curing agent 1,10-(methylenedi-1,4-phenylene)bismaleimide (BMI). The structure and composition of all polymers were studied using spectroscopic methods. Molecular mass was determined using gel permeation chromatography (GPC). Thermal properties were studied using TGA, DSC, and TMA methods. The mechanical and self-healing properties of the materials were investigated via a uniaxial tensile test. Visual assessment of the completeness of damage restoration after the self-healing cycle was carried out using a scanning electron microscope. It was shown that the proposed modified approach helps obtain more durable polyurethanes with a high degree of self-healing of mechanical properties after damage. Full article

This study systematically investigates the impact of hydrolytic degradation on the crystallization kinetics and morphology of poly(butylene succinate-co-adipate) (PBSA). Gel Permeation Chromatography (GPC) confirmed extensive chain scission, significantly reducing the polymer’s weight-average molecular weight (M_w from ~103,000 to ~16,000 g/mol) and broadening its polydispersity index (PDI from ~2 to 7 after 64 days). Differential scanning calorimetry (DSC) analysis revealed that hydrolytic degradation dramatically accelerated crystallization rates, reducing crystallization time roughly 10-fold (e.g., from ~3000 s to ~300 s), and crystallinity increased from 34% to 63%. Multiple melting peaks suggested the presence of lamellae with varying thicknesses, consistent with the Gibbs–Thomson equation. Isothermal crystallization kinetics were evaluated using the Avrami equation (with n ≈ 3), reciprocal half-time of crystallization, and a novel inflection point slope method, all confirming accelerated crystallization; for instance, the slope increased from 0.00517 to 0.05203. Polarized optical microscopy (POM) revealed evolving spherulite morphologies, including hexagonal and flower-like dendritic spherulites with diamond-shape ends, while wide-angle X-ray diffraction (WAXD) showed a crystallization range shift to higher temperatures (e.g., from 72–61 °C to 82–71 °C) and a 14% increase in crystallite diameter, aligning with increased melting point and lamellar thickness and overall increased crystallinity. Full article

In this study, we designed an injectable skin-rejuvenating formulation based on polyethylene glycol–polycaprolactone–polyethylene glycol (PEG-PCL-PEG) copolymers to provide a synergistic combination of biocompatibility, antioxidative capacity, and regenerative potential. Through the systematic optimization of the precursor molar ratio and molecular weight, well-defined PEG-PCL-PEG copolymers were synthesized and structurally characterized using gel permeation chromatography (GPC), proton nuclear magnetic resonance (¹H-NMR), and Fourier transform infrared (FT-IR) spectroscopy. An optimized precipitation and drying protocol effectively reduced residual solvents, as confirmed by gas chromatography (GC). Idebenone was incorporated as an antioxidant to prevent skin aging, while hyaluronic acid (HA), L-arginine, and glycerin were included to promote collagen regeneration. In vitro assays demonstrated that idebenone-loaded samples exhibited prolonged intracellular antioxidant activity with low cytotoxicity. The collagen-promoting formulation, containing HA, glycerin, and L-arginine, enhanced the expression of transforming growth factor-β (TGF-β) and type III collagen (COL3) while suppressing inflammatory genes, suggesting a favorable environment for extracellular matrix remodeling. In vivo evaluation corroborated these outcomes, showing angiogenesis, collagen reorganization, and progressive dermal thickness. Histological analysis further confirmed sustained matrix regeneration and tissue integration. These results highlight the potential of PEG-PCL-PEG-based injectables as a multifunctional platform for collagen regeneration, offering a promising strategy for both cosmetic and clinical applications. Full article

The dependence of conventional epoxy resins on fossil fuels and the environmental and health hazards associated with bisphenol A (BPA) demand the creation of sustainable alternatives. Because lignin is a natural resource and has an aromatic ring skeleton structure, it could be used as an alternative to fossil fuels. This study effectively resolved this challenge by utilizing a sustainable one-step epoxidation process to transform lignin into a bio-based epoxy resin. The results verified the successful synthesis of epoxidized bamboo lignin through systematic characterization employing Fourier transform infrared spectroscopy, hydrogen spectroscopy/two-dimensional heteronuclear single-quantum coherent nuclear magnetic resonance, quantitative phosphorus spectroscopy, and gel permeation chromatography. Lignin-based epoxy resins had an epoxy equivalent value of 350–400 g/mol and a weight-average molecular weight of 4853 g/mol. Studies on the curing kinetics revealed that polyetheramine (PEA-230) demonstrated the lowest apparent activation energy (46.2 kJ/mol), signifying its enhanced curing efficiency and potential for energy conservation. Mechanical testing indicated that the PEA-230 cured network demonstrated the maximum tensile strength (>25 MPa), whereas high-molecular-weight polyetheramine (PEA-2000) imparted enhanced elongation to the material. Lignin-based epoxy resins demonstrated superior heat stability. This study demonstrates the conversion of bamboo lignin into bio-based epoxy resins using a simple, environmentally friendly synthesis process, demonstrating the potential to reduce fossil resource use, efficiently use waste, develop sustainable thermosetting materials, and promote a circular bioeconomy. Full article

The recycling of plastics collected from household waste to produce post-consumer recycled (PCR) materials is a critical step of sustainable waste management. However, the processing of PCR materials presents unique challenges, particularly in the context of seasonal input stream fluctuations and resulting PCR material composition variations. Within this paper, the influence of batch-to-batch fluctuations on the processing stability and product properties of high-density polyethylene (HDPE) PCR from the German municipal waste system is analysed. It examines how variations in batch composition affect key parameters such as processing data (injection pressure, torque), mechanical properties (tensile strength, E-modulus, impact strength), and product quality (gel formation, part dimensions, part weight). Therefore, six consecutive household HDPE PCR material batches are analysed regarding their composition, contaminations, and rheological characteristics through ashing, differential scanning calorimetry, high-temperature gel permeation chromatography, and high-pressure capillary rheometry. The batches are then processed using blown- and cast-film extrusion as well as injection moulding, and the resulting process stability and product quality are analysed. The results show a strong correlation between thermal properties, such as crystallisation enthalpy, molecular weight, polypropylene (PP) content, varying batch viscosities, and changes in processing data as well as the resulting product properties. Full article

This study aims to identify the chemical structure and immunomodulatory activity of exopolysaccharides (EPSs) from Acetilactobacillus jinshanensis BJ01 and suggest its potential applications in the pharmaceutical field and as functional food additives. The EPS-1 produced by A. jinshanensis BJ01 was purified using column chromatography. The lyophilized powder obtained by vacuum freeze-drying was used for structural characterization and immunomodulatory activity analysis. Gel permeation chromatography (GPC) determined its molecular weight as 156.58 kDa. High-performance anion-exchange chromatography (HPAEC) identified that the EPS-1 is composed of mannose, xylose, and glucose. The structural characterization of EPS-1 by gas chromatography–mass spectrometry (GC-MS) and 1D/2D nuclear magnetic resonance (NMR) spectroscopy demonstrated that EPS-1 is primarily composed of α-D-Manp-(1→, →2,6)-α-D-Manp-(1→, →2)-α-D-Manp-(1→, and →3)-α-D-Manp-(1→. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) illustrated that EPS-1 exhibited a round, flake-like morphology. In vitro experiments with RAW264.7 macrophages demonstrated the high immunomodulatory activity of EPS-1. Significant upregulation of iNOS, IL-6, and TNF-α mRNA levels was confirmed by qRT-PCR (p < 0.05). Western blotting revealed that EPS-1 (6.25 μg/mL) induced phosphorylation of NF-κB (p65, IκBα) and MAPK (ERK) signaling proteins. This study provides the first structural and immunomodulatory characterization of an exopolysaccharide from A. jinshanensis BJ01, highlighting its potential as a novel immune adjuvant. Full article

To investigate the immunomodulatory activity of polysaccharides derived from the rhizome of Imperata cylindrica, polysaccharides (IRPs-H) were extracted using hot water extraction and further purified via DEAE-52 ion-exchange chromatography, yielding three fractions: IRPs-H1, IRPs-H2, and IRPs-H3. The structural features of these fractions were characterized by Fourier-transform infrared spectroscopy (FT-IR), high-performance gel permeation chromatography (HPGPC), atomic force microscopy (AFM), and thermogravimetric analysis (TGA). Their immunological activities were evaluated in vitro. All three fractions were identified as neutral pyranose-type polysaccharides, primarily composed of glucose and xylose, exhibiting good thermal stability and lacking long-chain structures. In vitro assays using RAW264.7 macrophages demonstrated that these polysaccharides promoted cell proliferation (50–800 μg/mL), enhanced phagocytic activity, and induced morphological changes characteristic of macrophage activation, including irregular shapes and pseudopod formation. ELISA and flow cytometry analyses revealed dose-dependent increases in nitric oxide (NO), interleukin-6 (IL-6), tumor necrosis factor-α (TNF-α), and reactive oxygen species (ROS) levels. Notably, the IRPs-H3 fraction stimulated TNF-α and IL-6 production to levels of 438.02 ± 14.14 pg/mL and 30.13 ± 1.27 pg/mL, respectively, which were comparable to those induced by lipopolysaccharide (LPS), the positive control (460.83 ± 16.10 pg/mL and 31.87 ± 1.72 pg/mL, respectively). These results suggest that polysaccharides extracted from the rhizome of Imperata cylindrica possess significant immunostimulatory properties and hold potential for development as functional food ingredients or immune-enhancing agents. Full article

The functionalisation of lignin-derived phenolics (guaiacol, 4-propylguaiacol, eugenol, isoeugenol, phenol, m-cresol, catechol, syringol, syringaldehyde, and vanillin) for the synthesis of thermoplastic polyurethanes (PUs) and polyester (PE) resins is herein described. Diols were synthesised from phenolics in a one-step reaction using either glycerol carbonate or ethylene carbonate as a greener, solvent-free synthetic route. Nine of the diols were selected for the synthesis of Pus, and two of the diols were used for the synthesis of PE resins, with their physical and thermal properties characterised. Analysis of the PUs by differential scanning calorimetry (DSC) confirmed their amorphous nature, while thermogravimetric analysis (TGA) suggested improved thermal stability for all PUs with the addition of an alkyl or aldehyde substituent on the benzene ring regardless of the diisocyanate used. However, lower PU thermal stabilities were observed with the use of an aliphatic diisocyanate over an aromatic diisocyanate in the absence of an additional substituent. Analysis of the PEs by DSC also confirmed that the clear resins were all amorphous, and gel permeation chromatography (GPC) revealed significantly higher molecular weights and dispersities when an aliphatic diacid was utilised over an aromatic diacid. Full article

Amphiphilic diblock copolymers comprising polyethylene glycol (PEG) and 1-vinyl imidazole (VIM) were synthesized using reversible addition–fragmentation chain transfer (RAFT) polymerization. The study focused on the synthesis of well-defined nanostructures with tunable composition and their functional modification for biomedical applications. The successful polymerization of PEG-b-PVIM diblock copolymers was confirmed via ¹H NMR spectroscopy, and their molecular weights were analyzed using gel permeation chromatography (GPC). The copolymers exhibited pH-responsive behavior, with effective pK values of approximately 4.2. To facilitate radiolabeling and in vivo tracking, a post-polymerization modification enabled the conjugation of a 1,4,7-Triazacyclononane-1,4,7-triacetic acid (NOTA) chelator via aminolysis. The final conjugates were purified and characterized, confirming successful functionalization. These findings highlight the potential of PEG_x-b-PVIM_y diblock copolymers for biomedical applications. Full article

To develop efficient utilization technologies for lignite, HyperCoal was prepared from the depolymerization of Shengli lignite by reacting it with NaOH and methanol. A series of HyperCoal extracts were obtained using different solvents and characterized using elemental analysis, Fourier-transform infrared spectroscopy, gel permeation chromatography, and synchronous fluorescence spectroscopy. The results indicate that solvent polarity is the primary factor influencing both the extraction yield and the structure of the extracts as polar solvents can disrupt or break hydrogen bonds within the extracts. The extraction yield increases with the polarity of the extraction solvent. HyperCoal is a complex mixture of aromatic derivatives containing alkyl substituents and oxygen-containing functional groups. The O/C ratio and molecular size of the extracts, the amount of oxygen-containing functional groups, the proportion of aromatic structures, and the size of aromatic nuclei in the extracts increase with increasing solvent polarity, while the H/C ratio and proportion of aliphatic structures decrease. These findings aid developing methods for producing high-value-added chemicals from HyperCoal through staged conversion. Full article

The degradation of polypropylene (PP) through thermal and mechanical stress, as well as the influence of oxygen, are unavoidable when processing on a co-rotating twin-screw extruder. In previous studies, a mathematical model was developed to predict the degradation while compounding on different twin-screw extruder sizes. Additionally, the examination of filled PPs was conducted. To this end, a range of operating parameters and extruder sizes were used to process PP, and the molar mass was then determined by melt flow rate (MFR) and gel permeation chromatography (GPC) measurements to derive the degree of degradation. The model was then modified by adjusting the sensitivity parameters to allow the degradation behavior of the PPs to be described independently of extruder size. Consistent with prior research, comprehensive measurements of a PP/titanium dioxide (TiO₂) compound revealed that, with a few exceptions, increasing temperatures and screw speeds and decreasing throughputs generally resulted in higher degradation. However, the application of the model to the compounds did not achieve good agreement with the measured degradation, indicating different degradation conditions due to the different thermodynamic and rheological properties of the compounds. Full article

Biochemical monomer upcycling of plastic waste and its conversion into value-added products is deemed necessary, as it provides a greener and more sustainable solution to plastic waste management. In the current study, the polystyrene (PS) biodegradation potential of the fungus Phanerochaete chrysosporium NA3 was evaluated using various analytical techniques, such as Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), gel permeation chromatography (GPC), and high-performance liquid chromatography (HPLC). The biodegradation capacity of the fungal strain was further evaluated using a carbon dioxide (CO₂) evolution test, which showed that the PS films treated with NA3 produced more CO₂, indicating the strain’s ability to successfully utilize PS as a carbon source. The FTIR analysis of the PS films treated with NA3 showed modifications in the polymer chemical structure, including the formation of carbonyl and hydroxyl groups, which suggests the enzymatic dissociation of the polymer and the associated biodegradation mechanism. Pretreatments were found to be effective in modifying the polymer’s properties, making it more susceptible to microbial degradation, thus further accelerating the biodegradation process. The current study strongly advocates that P. chrysosporium (NA3) can be effectively used for the biochemical monomer recovery of PS waste and could be further utilized in the upcycling of plastic waste for its conversion into value-added products under the concept of circular economy. Full article