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22 pages, 5942 KiB  
Protocol
Development of an Application Method for Volatile Compounds Derived from Mushroom Fungi Beds as Plant Growth-Promoting Biostimulants
by Clever N. Kanga, Yui Okisaka, Shigeru Hanamata, Daijiro Ueda, Tsutomu Sato, Toshiaki Mitsui and Kimiko Itoh
Methods Protoc. 2025, 8(2), 29; https://doi.org/10.3390/mps8020029 - 7 Mar 2025
Viewed by 305
Abstract
Volatile compounds (VCs) from fungi can promote plant growth, but their application methods are limited. Edible mushroom fungi beds (FBs) provide a readily available alternative source of fungal VCs, although their biostimulatory functions remain unvalidated. In this study, a novel, non-contact exposure method [...] Read more.
Volatile compounds (VCs) from fungi can promote plant growth, but their application methods are limited. Edible mushroom fungi beds (FBs) provide a readily available alternative source of fungal VCs, although their biostimulatory functions remain unvalidated. In this study, a novel, non-contact exposure method for applying VCs emitted from FBs to rice seedlings was developed. This marks the first evaluation of mushroom FBs as a direct source of bioactive VCs for plant growth promotion. Volatiles from two different edible mushroom FBs promoted shoot growth and increased biomass for rice seedlings. VCs from shiitake FBs significantly increased biomass by 67.4% while VCs from enokitake FBs by 39.5% compared to the control. The biomass-increasing effects were influenced by the quantity of shiitake FBs applied, with significant increases at 15 g, 30 g and 60 g applications. The VCs effects remained significant even when the FBs were covered with two types of gas-permeable polymer film. Chemical analysis of VCs from FBs identified several organic compounds and subsequent bioassays using synthetic VCs determined key bioactive VCs contributing to biomass increase at specific concentrations. This study presents a utilization method of waste mushroom FBs as sustainable, scalable, and cost-effective agricultural biostimulants. Full article
(This article belongs to the Section Biochemical and Chemical Analysis & Synthesis)
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<p>An overview of the schematic workflow of non-contact VCs exposure on rice seedlings experimental design and conditions. (<b>1</b>) Rice seeds were sterilized with 1% sodium hypochlorite. After 4 days of germination, rice seedlings were transplanted into a plant box with culture soil. Seedlings are exposed to mushroom fungi bed-derived VCs (+VCs) in a non-contact setup, while control seedlings remain unexposed (−VCs). Growth conditions include a 13 h light/11 h dark photoperiod, 123 ± 6 μmol m⁻<sup>2</sup> s⁻<sup>1</sup> and 122 ± 9 μmol m⁻<sup>2</sup> s⁻<sup>1</sup> PPFD, and around 60% relative humidity for 14 days. (<b>2</b>) HS-SPME-GC-TOF-MS analysis identified 3-octanone, 1-octen-3-ol, 1-octen-3-one, and 3-octanol as key fungal VCs present in shiitake mushroom FBs. Illustration was created using Biorender; <a href="https://BioRender.com" target="_blank">https://BioRender.com</a> (accessed on 3 March 2025).</p>
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<p>Effect of VCs emitted from enokitake and shiitake fungi beds on rice seedling growth and biomass accumulation. (<b>A</b>) Representative images of rice seedlings exposed to VCs from enokitake and shiitake fungi beds compared to control seedlings (scale bar = 5 cm is shown as white bar at the left). (<b>B</b>) Dry weight (mg) of rice seedlings after 14 days of exposure. (<b>C</b>) Plant height (cm) of rice seedlings. (<b>D</b>) Root length (cm) of rice seedlings. Distinct letters (a, b, c) denote statistically significant differences (<span class="html-italic">p</span> &lt; 0.05) among the treatments. The data are presented as mean ± standard deviation (SD) with n = 5. Error bars represent the standard deviation (±SD).</p>
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<p>Dose–response effects of shiitake fungi bed VCs on rice seedling growth and biomass accumulation. (<b>A</b>) Representative images of rice seedlings after 14 days of non-contact exposure to varying quantities (0–60 g) of shiitake fungi bed substrates (scale bar = 5 cm is shown as white bar at the right). (<b>B</b>) Dry weight of rice seedlings. (<b>C</b>) Plant height. (<b>D</b>) Root length. Different letters (a, b, c, d) indicate statistically significant differences between treatments (Tukey’s test, <span class="html-italic">p</span> &lt; 0.05). Data are presented as mean ± SD (n = 5). Error bars indicate the standard deviation (±SD).</p>
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<p>Effect of different exposure methods of shiitake fungi bed-derived VCs on rice seedling growth and biomass accumulation. (<b>A</b>) Representative image of rice seedlings exposed to shiitake fungi beds (60 g) using HDPE wrapping (HDPE), PVC wrapping (PVC), and open Petri dish (OPD) methods compared to the control (scale bar = 5 cm is shown as white bar at the right). (<b>B</b>) Dry weight (mg) of rice seedlings. (<b>C</b>) Plant height (cm) of rice seedlings. (<b>D</b>) Root length (cm) of rice seedlings. Different letters (a, b, c) indicate statistically significant differences among treatments (Tukey’s test, <span class="html-italic">p</span> &lt; 0.05). Data are presented as mean ± SD (n = 5). Error bars indicate the standard deviation (±SD).</p>
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<p>Effects of shiitake fungi bed age on rice seedling growth and biomass accumulation. (<b>A</b>) Representative images of rice seedlings exposed to volatile compounds (VCs) from young (YSFB), mature (MSFB), and waste (WSFB) shiitake fungi beds compared to the control (scale bar = 5 cm is shown as white bar at the left). (<b>B</b>) Dry weight (mg) of rice seedlings. (<b>C</b>) Plant height (cm) of rice seedlings. (<b>D</b>) Root length (cm) of rice seedlings. Different letters indicate statistically significant differences among treatments (Tukey’s test, <span class="html-italic">p</span> &lt; 0.05). Data are presented as mean ± SD (n = 5). Error bars indicate the standard deviation (±SD).</p>
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<p>Representative GC-MS chromatogram of volatile compounds emitted from waste shiitake FBs (WSFB). The total ion chromatogram (TIC) shows six major peaks identified at different retention times, which correspond to distinct volatile organic compounds (VOCs). Peaks are labeled as follows: (1), (2), (3), (4), (5), and (6), indicating significant VOCs detected. Retention times and intensities of these peaks suggest the presence of dominant compounds contributing to the overall volatile emissions profile.</p>
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<p>Growth responses of rice seedlings to increasing dose rates of 3-octanone, 3-octanol, 1-octen-3-one, and 1-octen-3-ol. (<b>A</b>–<b>C</b>) Dry weight, plant height, and root length under 3-octanone treatments. (<b>D</b>–<b>F</b>) Dry weight, plant height, and root length under 3-octanol treatments. (<b>G</b>–<b>I</b>) Dry weight, plant height, and root length under 1-Octen-3-one treatments. (<b>J</b>–<b>L</b>) Dry weight, plant height, and root length under 1-octen-3-ol treatments. Error bars indicate the standard deviation (mean ± SD). Letters above indicate significant differences between treatments (<span class="html-italic">p</span> &lt; 0.05). The same letters indicate no statistical significance against the control while the different letters indicate statistical significance.</p>
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18 pages, 7811 KiB  
Article
Plastic Litter Detection in the Environment Using Hyperspectral Aerial Remote Sensing and Machine Learning
by Marco Balsi, Monica Moroni and Soufyane Bouchelaghem
Remote Sens. 2025, 17(5), 938; https://doi.org/10.3390/rs17050938 - 6 Mar 2025
Viewed by 134
Abstract
Plastic waste has become a critical environmental issue, necessitating effective methods for detection and monitoring. This article presents a machine-learning-based methodology and embedded solution to detect plastic waste in the environment using an airborne hyperspectral sensor operating in the short-wave infrared (SWIR) band. [...] Read more.
Plastic waste has become a critical environmental issue, necessitating effective methods for detection and monitoring. This article presents a machine-learning-based methodology and embedded solution to detect plastic waste in the environment using an airborne hyperspectral sensor operating in the short-wave infrared (SWIR) band. Experimental data were obtained from drone flights in several case studies in natural and controlled environments. Data were preprocessed to simply equalize the spectra across the whole band and across different environmental conditions, and machine learning techniques were applied to detect plastics even in real-time. Several algorithms for spectrum calibration, feature selection, and classification were optimized and compared to obtain an optimal solution that has high-quality results under cross-validation. This way, deploying the system in different environments without requiring complicated manual adjustments or re-learning is possible. The results of this work prove the feasibility of the proposed plastic litter detection approach using high-definition aerial remote sensing, with high specificity to plastic polymers that are not obtained using visible and NIR data. Full article
(This article belongs to the Section Environmental Remote Sensing)
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<p>Hyperspectral sensor assembly.</p>
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<p>Drone and sensor in flight.</p>
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<p>Situation on ground for the surveys used for plastic detection machine learning. (<b>a</b>) Jan20, (<b>b</b>) Mar20, (<b>c</b>) Apr22, (<b>d</b>) 7Feb24a and 7Feb24b, (<b>e</b>) 21Feb24a, (<b>f</b>) 21Feb24b. Material labels are self-explanatory. Unknown or unsorted plastic materials are indicated here as mixed (this class also includes type-7 plastics according to international codes), unknown, or beach, the latter indicating weathered litter collected on a beach. High- and low-density PE (HDPE and LDPE) have different standard codes but are chemically equal and not distinguishable by their reflected spectrum, so they were grouped in a single PE class in our work. These images were obtained by just stitching together a few visible images taken in the same or in separate flights, so they are not necessarily rectangular. They are not co-registered with the hyperspectral data because they are just meant to record the situation on the ground for documentation.</p>
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<p>Comparison of spectra acquired from the drone (21Feb24a) and spectra acquired from the spectroradiometer. Blue lines show the reflectance measured by the spectroradiometer, and black lines show the reflectance as estimated from the drone sensor, both normalized to arbitrary units for visualization purposes. The standard deviation of the drone spectra is indicated by gray shading. Please notice that the standard deviation blows up near the band that we cut because it is dark in sunlight (so that under calibration, the division by the small values of the white spectrum is unreliable) and that another relatively dark band exists around approximately 1120 nm. <span class="html-italic">x</span>-axis: wavelength in nm; <span class="html-italic">y</span>-axis: arbitrary units for the black line, reflectance for the blue line.</p>
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<p>Kappa score for classifiers for all plastics vs. number of features selected by mRMR. Dashed line: LDA, solid line: SVM.</p>
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<p>Results of classification by the SVM classifier trained on the 21Feb24a cube (raw data) and tested on the same cube. (<b>a</b>) Desired output, all plastics; (<b>b</b>) classifier output, all plastics; (<b>c</b>) desired output, PET; (<b>d</b>) classifier output, PET (“don’t care”); (<b>e</b>) classifier output, PET only. White: positive response; black: negative response; gray: external pixels (outside the surveyed area).</p>
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<p>Results of classification by the SVM classifier trained on seven datasets, with simple level adjustment, on the 21Feb24a dataset. (<b>a</b>) Desired output, all plastics; (<b>b</b>) classifier output, all plastics; (<b>c</b>) classifier output, PET (“don’t care”); (<b>d</b>) classifier output, PET only. Materials: (1) mixed plastics; (2) PS; (3) weathered plastic litter collected on a beach; (4) PP; (5) PVC; (6) PE; (7) PET. White: positive response; black: negative response; gray: external pixels (outside the surveyed area).</p>
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<p>Results of classification by the SVM classifier trained on seven datasets, with simple level adjustment, on the 21Feb24a dataset. (<b>a</b>) PE only; (<b>b</b>) PVC only; (<b>c</b>) PS only; (<b>d</b>) PP only; (<b>e</b>) logical OR combinations of the outcomes for all five plastic polymers, to be compared to <a href="#remotesensing-17-00938-f007" class="html-fig">Figure 7</a>b. White: positive response; black: negative response; gray: external pixels (outside the surveyed area).</p>
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<p>Wavelength features chosen by mRMR.</p>
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<p>Results of the application of the SVM classifiers for “all plastics”, trained on seven cubes (gound truth mask and classification for each cube, respectively): (<b>a</b>,<b>b</b>) Jan20; (<b>c</b>,<b>d</b>) Mar20; (<b>e</b>,<b>f</b>) Apr22; (<b>g</b>,<b>h</b>) 7Feb24a; (<b>i</b>,<b>j</b>) 7Feb24b; (<b>k</b>,<b>l</b>) 21Feb24a; and (<b>m</b>,<b>n</b>) 21Feb24b. White: positive response; black: negative response; gray: external pixels (outside the surveyed area).</p>
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<p>Results of the application of the SVM classifiers for “all plastics”, trained on seven cubes (gound truth mask and classification for each cube, respectively): (<b>a</b>,<b>b</b>) Jan20; (<b>c</b>,<b>d</b>) Mar20; (<b>e</b>,<b>f</b>) Apr22; (<b>g</b>,<b>h</b>) 7Feb24a; (<b>i</b>,<b>j</b>) 7Feb24b; (<b>k</b>,<b>l</b>) 21Feb24a; and (<b>m</b>,<b>n</b>) 21Feb24b. White: positive response; black: negative response; gray: external pixels (outside the surveyed area).</p>
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<p>Plastic recognition at sea. (<b>a</b>) Photograph from the drone; (<b>b</b>) visible images mosaic; (<b>c</b>) detection result. Objects: (1) and (2), plastic containers; (3), metal coated bag; (4), rubber pipe; (5), wooden stick.</p>
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21 pages, 5465 KiB  
Article
Effects of Untreated Waste Lignin as a Sustainable Asphalt Emulsion Substitute on Water Resistance and Environmental Impacts in Reclaimed Half-Warm Asphalt Mixtures
by Ana María Rodríguez Pasandín, Pablo Orosa, Ana María Rodríguez-Alloza, Edoardo Nardi and Natalia Pérez-Barge
Coatings 2025, 15(3), 304; https://doi.org/10.3390/coatings15030304 - 5 Mar 2025
Viewed by 343
Abstract
Polymers are known to produce beneficial effects on asphalt mixtures, and lignin biopolymers could further improve them while contributing to sustainability and circularity. In this research, conventional asphalt emulsion was replaced with liquid waste containing lignin from the wood industry in half-warm mix [...] Read more.
Polymers are known to produce beneficial effects on asphalt mixtures, and lignin biopolymers could further improve them while contributing to sustainability and circularity. In this research, conventional asphalt emulsion was replaced with liquid waste containing lignin from the wood industry in half-warm mix asphalt (HWMA) at varying substitution levels of 0% (control), 5%, 10%, 15%, and 20%. Additionally, 100% reclaimed asphalt pavement (RAP) was used as aggregate. The impact of asphalt emulsion substitution on the mixtures’ adhesion, cohesion, and water resistance was analyzed. Indirect tensile strength tests evaluated the HWMA’s resistance to moisture damage and ductility. Rolling bottle and boiling water tests were conducted to assess the binder-aggregate affinity. Moreover, a Life Cycle Assessment (LCA) was performed to compare the environmental benefits of HWMA with those of Hot Mix Asphalt (HMA). The findings revealed that substituting asphalt emulsion with the waste lignin up to 15% enhances the mixture’s cohesion, while only substitutions up to 5% produce mixtures with enhanced water resistance. Environmental impacts were significantly reduced for all the HWMA studied, with the Global Warming Potential (GWP) showing up to 33.5% reduction compared to a conventional HMA. Full article
(This article belongs to the Special Issue Recent Research in Asphalt and Pavement Materials)
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<p>Flow chart of the research plan.</p>
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<p>System boundary for the HWMA production.</p>
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<p>System boundary for the HMA production.</p>
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<p>Diffractogram of the mixture of asphalt emulsion and waste lignin by XRD.</p>
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<p>The surface of the aggregates that remain coated (%) after the rolling bottle and boiling water tests.</p>
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<p>Detail of the surface that remained coated in the loose mixtures made with (<b>a</b>) 0% waste lignin instead of asphalt emulsion after 24 h in the rolling bottle test and (<b>b</b>) 20% waste lignin.</p>
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<p>Mass loss after the Cantabro test.</p>
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<p>HWMA specimen made with 5% waste lignin in place of asphalt emulsion before and after the Cantabro test.</p>
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<p>Compaction curves for the tested mixtures.</p>
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<p>Strain at breaking for the tested mixtures.</p>
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<p>Comparison of environmental impacts between the HWMA and the HMA.</p>
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<p>Contribution of key indexes for 1 ton of HWA_L0 mixture.</p>
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<p>Contribution of key indexes for 1 ton of HWA_L5 mixture.</p>
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<p>Contribution of key indexes for 1 ton of HWA_L10 mixture.</p>
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<p>Contribution of key indexes for 1 ton of HWA_L15 mixture.</p>
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<p>Contribution of key indexes for 1 ton of HWA_L20 mixture.</p>
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<p>Contribution of key indexes for 1 ton of the conventional mixture.</p>
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29 pages, 9288 KiB  
Article
Machine Learning-Driven Prediction of Composite Materials Properties Based on Experimental Testing Data
by Khrystyna Berladir, Katarzyna Antosz, Vitalii Ivanov and Zuzana Mitaľová
Polymers 2025, 17(5), 694; https://doi.org/10.3390/polym17050694 - 5 Mar 2025
Viewed by 313
Abstract
The growing demand for high-performance and cost-effective composite materials necessitates advanced computational approaches for optimizing their composition and properties. This study aimed at the application of machine learning for the prediction and optimization of the functional properties of composites based on a thermoplastic [...] Read more.
The growing demand for high-performance and cost-effective composite materials necessitates advanced computational approaches for optimizing their composition and properties. This study aimed at the application of machine learning for the prediction and optimization of the functional properties of composites based on a thermoplastic matrix with various fillers (two types of fibrous, four types of dispersed, and two types of nano-dispersed fillers). The experimental methods involved material production through powder metallurgy, further microstructural analysis, and mechanical and tribological testing. The microstructural analysis revealed distinct structural modifications and interfacial interactions influencing their functional properties. The key findings indicate that optimal filler selection can significantly enhance wear resistance while maintaining adequate mechanical strength. Carbon fibers at 20 wt. % significantly improved wear resistance (by 17–25 times) while reducing tensile strength and elongation. Basalt fibers at 10 wt. % provided an effective balance between reinforcement and wear resistance (by 11–16 times). Kaolin at 2 wt. % greatly enhanced wear resistance (by 45–57 times) with moderate strength reduction. Coke at 20 wt. % maximized wear resistance (by 9−15 times) while maintaining acceptable mechanical properties. Graphite at 10 wt. % ensured a balance between strength and wear, as higher concentrations drastically decreased mechanical properties. Sodium chloride at 5 wt. % offered moderate wear resistance improvement (by 3–4 times) with minimal impact on strength. Titanium dioxide at 3 wt. % enhanced wear resistance (by 11–12.5 times) while slightly reducing tensile strength. Ultra-dispersed PTFE at 1 wt. % optimized both strength and wear properties. The work analyzed in detail the effect of PTFE content and filler content on composite properties based on machine learning-driven prediction. Regression models demonstrated high R-squared values (0.74 for density, 0.67 for tensile strength, 0.80 for relative elongation, and 0.79 for wear intensity), explaining up to 80% of the variability in composite properties. Despite its efficiency, the limitations include potential multicollinearity, a lack of consideration of external factors, and the need for further validation under real-world conditions. Thus, the machine learning approach reduces the need for extensive experimental testing, minimizing material waste and production costs, contributing to SDG 9. This study highlights the potential use of machine learning in polymer composite design, offering a data-driven framework for the rational choice of fillers, thereby contributing to sustainable industrial practices. Full article
(This article belongs to the Section Polymer Physics and Theory)
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<p>Commonly used types of computational methods for solving materials science tasks.</p>
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<p>The microstructures of components used for designing PCMs: (<b>a</b>) sodium chloride; (<b>b</b>) ultra-PTFE; (<b>c</b>) graphite; (<b>d</b>) kaolin; (<b>e</b>) basalt fiber; (<b>f</b>) PTFE (matrix).</p>
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<p>The microstructures of components used for designing PCMs: (<b>a</b>) sodium chloride; (<b>b</b>) ultra-PTFE; (<b>c</b>) graphite; (<b>d</b>) kaolin; (<b>e</b>) basalt fiber; (<b>f</b>) PTFE (matrix).</p>
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<p>Flowchart of the production process for obtaining test samples.</p>
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<p>The microstructure of the composite with 20% carbon fibers.</p>
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<p>The microstructure of composite with 10% basalt fibers.</p>
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<p>The microstructure of the composite with 2% kaolin.</p>
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<p>The microstructure of the composite with 20% coke.</p>
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<p>The microstructure of composite with 10% coke.</p>
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<p>The microstructure of the composite with 2% sodium chloride.</p>
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<p>The microstructure of composite with 5% titanium dioxide.</p>
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<p>The microstructure of composite with 1% ultra-PTFE.</p>
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<p>The functional properties of the designed two-component PCMs based on the filler concentrations: (<b>a</b>) density, (<b>b</b>) tensile strength, (<b>c</b>) relative elongation, (<b>d</b>) wear intensity (for 100% PTFE, the wear intensity is 610 × 10<sup>−6</sup> mm<sup>3</sup>/N·m).</p>
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<p>The functional properties of the designed three-component PCMs based on the filler concentrations: (<b>a</b>) density, (<b>b</b>) tensile strength, (<b>c</b>) relative elongation, (<b>d</b>) wear intensity (for 100% PTFE, the wear intensity is 610 × 10<sup>−6</sup> mm<sup>3</sup>/N·m).</p>
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<p>Boxplot density versus PTFE.</p>
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<p>Box plot tensile strength versus PTFE.</p>
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<p>Box plot of relative elongation versus PTFE.</p>
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<p>Box plot wear intensity versus PTFE.</p>
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21 pages, 3101 KiB  
Article
Microplastic Deposits Prediction on Urban Sandy Beaches: Integrating Remote Sensing, GNSS Positioning, µ-Raman Spectroscopy, and Machine Learning Models
by Anderson Targino da Silva Ferreira, Regina Célia de Oliveira, Eduardo Siegle, Maria Carolina Hernandez Ribeiro, Luciana Slomp Esteves, Maria Kuznetsova, Jessica Dipold, Anderson Zanardi de Freitas and Niklaus Ursus Wetter
Microplastics 2025, 4(1), 12; https://doi.org/10.3390/microplastics4010012 - 5 Mar 2025
Viewed by 201
Abstract
This study focuses on the deposition of microplastics (MPs) on urban beaches along the central São Paulo coastline, utilizing advanced methodologies such as remote sensing, GNSS altimetric surveys, µ-Raman spectroscopy, and machine learning (ML) models. MP concentrations ranged from 6 to 35 MPs/m [...] Read more.
This study focuses on the deposition of microplastics (MPs) on urban beaches along the central São Paulo coastline, utilizing advanced methodologies such as remote sensing, GNSS altimetric surveys, µ-Raman spectroscopy, and machine learning (ML) models. MP concentrations ranged from 6 to 35 MPs/m2, with the highest densities observed near the Port of Santos, attributed to industrial and port activities. The predominant MP types identified were foams (48.7%), fragments (27.7%), and pellets (23.2%), while fibers were rare (0.4%). Beach slope and orientation were found to facilitate the concentration of MP deposition, particularly for foams and pellets. The study’s ML models showed high predictive accuracy, with Random Forest and Gradient Boosting performing exceptionally well for specific MP categories (pellet, fragment, fiber, foam, and film). Polymer characterization revealed the prevalence of polyethylene, polypropylene, and polystyrene, reflecting sources such as disposable packaging and industrial raw materials. The findings emphasize the need for improved waste management and targeted urban beach cleanups, which currently fail to address smaller MPs effectively. This research highlights the critical role of combining in situ data with predictive models to understand MP dynamics in coastal environments. It provides actionable insights for mitigation strategies and contributes to global efforts aligned with the Sustainable Development Goals, particularly SDG 14, aimed at conserving marine ecosystems and reducing pollution. Full article
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<p>Flowchart of the steps in the methodology used in this research. RS: orbital remote sensing images; MNDWI: modified normalized difference water index; HD<sub>sat</sub>: horizontal distance derived by satellite; VD<sub>tide</sub>: vertical distance derived by tide; tanβ<sub>sat</sub>: slope derived by satellite; GNSS: global navigation satellite system; Alt<sub>GNSS</sub>: altitude derived by GNSS; tanβ<sub>GNSS</sub>: slope derived by GNSS; μ-Raman: micro-Raman analysis; ML: machine learning models; and MP deposits: microplastic deposits.</p>
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<p>Sediment sampling sites and GNSS positioning locations. Urban areas are highlighted in red, with emphasis on the Port of Santos and the industrial region of Cubatão.</p>
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<p>Beach sampling point (P1), modified from [<a href="#B1-microplastics-04-00012" class="html-bibr">1</a>]. Examples of GNSS base, rover surveys, and area (1 m<sup>2</sup>) of superficial sediment collection.</p>
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<p>SHAP analysis of variable contributions for predicting microplastic deposition using multiple machine learning models: (<b>a</b>) SVR—Support Vector Regression for pellets; (<b>b</b>) GB—Gradient Boosting for fragments; (<b>c</b>) RF—Random Forest for fibers; (<b>d</b>) RF—Random Forest for foams; and (<b>e</b>) GB—Gradient Boosting for total MP. The intensity of each variable is represented by the color scale, ranging from blue (low values) to red (high values), indicating the magnitude of the feature’s influence.</p>
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<p>GNSS sediment samples and transect models: (<b>a</b>) beach slope (tanβ); (<b>b</b>) beach face direction (Aspect).</p>
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<p>Modeled points and GNSS sediment sample points: (<b>a</b>) pellet, (<b>b</b>) foam, (<b>c</b>) fragment, (<b>d</b>) fiber, and (<b>e</b>) total MP (m<sup>2</sup>).</p>
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<p>Perceptual maps showing the standardized adjusted residual (ASR) values between the microplastic deposition models: (<b>a</b>) pellet, (<b>b</b>) foam, (<b>c</b>) fragment, and (<b>d</b>) total MP (m<sup>2</sup>) in relation to beaches’ modeled points (PG, SVS, GUA, and BER). The colored cells indicate significant relationships between variables (+1.96 ≤ good SAR). VL (very low), L (low), M (medium), H (high), and VH (very high) represent the different levels of MP/m<sup>2</sup> deposition by CA.</p>
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<p>Raman spectra of polymers: (<b>a</b>,<b>b</b>) polyethylene; (<b>c</b>) polypropylene; and (<b>d</b>) polystyrene.</p>
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23 pages, 1716 KiB  
Article
Food-Grade Microwave-Assisted Depolymerization of Grape Seed Condensed Tannins: Optimizing the Reaction Using Gallic Acid as a Nucleophile
by Carolina F. Morales and Fernando A. Osorio
Polymers 2025, 17(5), 682; https://doi.org/10.3390/polym17050682 - 4 Mar 2025
Viewed by 155
Abstract
Food waste has a significant social impact but can be revalued as a source of bioactive compounds, such as condensed tannins. This abundant biomass, corresponding to a polymeric antioxidant, must be depolymerized to become bioavailable. Previous studies have investigated polymer degradation into oligomers [...] Read more.
Food waste has a significant social impact but can be revalued as a source of bioactive compounds, such as condensed tannins. This abundant biomass, corresponding to a polymeric antioxidant, must be depolymerized to become bioavailable. Previous studies have investigated polymer degradation into oligomers using high temperatures and expensive nucleophiles, often under conditions unsuitable for food applications. In the present investigation, it is proposed that the depolymerization of condensed tannins can occur under food-grade conditions using a Generally Recognized as Safe (GRAS) solvent by optimizing the reaction’s heating method with microwave assistance and using gallic acid as a nucleophile. Thermal studies indicate that the degradation of total polyphenols content follows first-order kinetics and occurs above 80 °C in microwave. Depolymerization follows second-order kinetics, yielding epicatechin as the primary product with zero-order formation kinetics. The optimized factors were 80% v/v ethanol, 10 mg/mL polymeric tannins, and 5.88 mg/mL gallic acid. Under these conditions, the reaction efficiency was 99.9%, the mean particle diameter was 5.7 nm, the total polyphenols content was 297.3 ± 15.9 EAG mg/g, and the inhibition of ABTS●+ and DPPH● radicals was 93.5 ± 0.9% and 88.2 ± 1.5%, respectively. These results are promising for future scaling processes. Full article
(This article belongs to the Section Polymer Chemistry)
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<p>UHPLC/UV chromatograms at a wavelength of 280 nm of P (<b>a</b>) initial (P) and (<b>b</b>) after thiolysis depolymerization (P-Tiol).</p>
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<p>Linearized graphs for TPC on P as a function of time for (<b>a</b>) TB 40 °C, M40 °C, TB 60 °C, and M60 °C and (<b>b</b>) TB60 °C and M60 °C.</p>
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<p>Molar concentration graphs as a function of depolymerization time for (<b>a</b>) GA, Ep, and P; fitted graphs with linearized models for (<b>b</b>) GA, (<b>c</b>) Ep, and (<b>d</b>) remaining polymers (P<sub>R</sub>). All the molecules studied are in a mixed depolymerization products suspension (P-Dep).</p>
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<p>Color parameters change graphs as a function of depolymerization time for (<b>a</b>) visual color (photography of P-Dep the samples), (<b>b</b>) L*, (<b>c</b>) a*, (<b>d</b>) ∆E*, and (<b>e</b>) ∆C*.</p>
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18 pages, 6652 KiB  
Article
Tensile Strength Predictive Modeling of Natural-Fiber-Reinforced Recycled Aggregate Concrete Using Explainable Gradient Boosting Models
by Celal Cakiroglu, Farnaz Ahadian, Gebrail Bekdaş and Zong Woo Geem
J. Compos. Sci. 2025, 9(3), 119; https://doi.org/10.3390/jcs9030119 - 4 Mar 2025
Viewed by 110
Abstract
Natural fiber composites have gained significant attention in recent years due to their environmental benefits and unique mechanical properties. These materials combine natural fibers with polymer matrices to create sustainable alternatives to traditional synthetic composites. In addition to natural fiber reinforcement, the usage [...] Read more.
Natural fiber composites have gained significant attention in recent years due to their environmental benefits and unique mechanical properties. These materials combine natural fibers with polymer matrices to create sustainable alternatives to traditional synthetic composites. In addition to natural fiber reinforcement, the usage of recycled aggregates in concrete has been proposed as a remedy to combat the rapidly increasing amount of construction and demolition waste in recent years. However, the accurate prediction of the structural performance metrics, such as tensile strength, remains a challenge for concrete composites reinforced with natural fibers and containing recycled aggregates. This study aims to develop predictive models of natural-fiber-reinforced recycled aggregate concrete based on experimental results collected from the literature. The models have been trained on a dataset consisting of 482 data points. Each data point consists of the amounts of cement, fine and coarse aggregate, water-to-binder ratio, percentages of recycled coarse aggregate and natural fiber, and the fiber length. The output feature of the dataset is the splitting tensile strength of the concrete. Extreme gradient boosting (XGBoost), light gradient boosting machine (LightGBM) and extra trees regressor models were trained to predict the tensile strength of the specimens. For optimum performance, the hyperparameters of these models were optimized using the blended search strategy (BlendSearch) and cost-related frugal optimization (CFO). The tensile strength could be predicted with a coefficient of determination greater than 0.95 by the XGBoost model. To make the predictive models accessible, an online graphical user interface was also made available on the Streamlit platform. A feature importance analysis was carried out using the Shapley additive explanations (SHAP) approach. Full article
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<p>(<b>a</b>) Coir [<a href="#B30-jcs-09-00119" class="html-bibr">30</a>], (<b>b</b>) ramie [<a href="#B16-jcs-09-00119" class="html-bibr">16</a>], (<b>c</b>) jute [<a href="#B31-jcs-09-00119" class="html-bibr">31</a>] fibers.</p>
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<p>Distribution of the input and output features.</p>
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<p>Parallel coordinates’ plot of the dataset.</p>
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<p>Isolation of data points.</p>
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<p>Predictive model development and interpretation.</p>
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<p>Explained variance ratios.</p>
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<p>Outliers for (<b>a</b>) contamination = 0.1, (<b>b</b>) contamination = 0.06, (<b>c</b>) contamination = 0.02, (<b>d</b>) contamination = 0.01.</p>
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<p>Model performances with respect to contamination.</p>
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<p>Extra trees model performance fluctuations on the test set.</p>
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<p>Hyperparameter optimization steps.</p>
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<p>Predicted and true values for (<b>a</b>) extra trees, (<b>b</b>) LightGBM, (<b>c</b>) XGBoost.</p>
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<p>Online graphical user interface.</p>
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<p>SHAP feature importances.</p>
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<p>SHAP summary plot.</p>
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<p>SHAP heatmap plot.</p>
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28 pages, 8366 KiB  
Article
Artificial Neural Network Modeling of Mechanical Properties of 3D-Printed Polyamide 12 and Its Fiber-Reinforced Composites
by Catalin Fetecau, Felicia Stan and Doina Boazu
Polymers 2025, 17(5), 677; https://doi.org/10.3390/polym17050677 - 3 Mar 2025
Viewed by 284
Abstract
Fused filament fabrication (FFF) has recently emerged as a sustainable digital manufacturing technology to fabricate polymer composite parts with complex structures and minimal waste. However, FFF-printed composite parts frequently exhibit heterogeneous structures with low mechanical properties. To manufacture high-end parts with good mechanical [...] Read more.
Fused filament fabrication (FFF) has recently emerged as a sustainable digital manufacturing technology to fabricate polymer composite parts with complex structures and minimal waste. However, FFF-printed composite parts frequently exhibit heterogeneous structures with low mechanical properties. To manufacture high-end parts with good mechanical properties, advanced predictive tools are required. In this paper, Artificial Neural Network (ANN) models were developed to evaluate the mechanical properties of 3D-printed polyamide 12 (PA) and carbon fiber (CF) and glass fiber (GF) reinforced PA composites. Tensile samples were fabricated by FFF, considering two input parameters, such as printing orientation and infill density, and tested to determine the mechanical properties. Then, single- and multi-target ANN models were trained using the forward propagation Levenberg–Marquardt algorithm. Post-training performance analysis indicated that the ANN models work efficiently and accurately in predicting Young’s modulus and tensile strength of the 3D-printed PA and fiber-reinforced PA composites, with most relative errors being far less than 5%. In terms of mechanical properties, such as Young’s modulus and tensile strength, the 3D-printed composites outperform the unreinforced PA. Printing PA composites with 0° orientation and 100% infill density results in a maximum increase in Young’s modulus (up to 98% for CF/PA and 32% for GF/PA) and tensile strength (up to 36% for CF/PA and 18% for GF/PA) compared to the unreinforced PA. This study underscores the potential of the ANN models to predict the mechanical properties of 3D-printed parts, enhancing the use of 3D-printed PA composite components in structural applications. Full article
(This article belongs to the Special Issue 3D Printing of Polymer Composite Materials)
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<p>Geometry of the 3D-printed samples and printing direction (all dimensions in mm).</p>
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<p>Configuration of the feed-forward neural network: (<b>a</b>) one output (Young’s modulus or tensile strength); (<b>b</b>) two outputs (Young’s modulus and tensile strength).</p>
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<p>SEM images of the fractured surface of the FFF-printed PA sample with (<b>a</b>) 0°, (<b>b</b>) 90°, and (<b>c</b>) ±45° printing orientation.</p>
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<p>SEM images of the fractured surface of the FFF-printed CF/PA sample with (<b>a</b>) 0°, (<b>b</b>) 90°, and (<b>c</b>) ±45° printing orientation.</p>
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<p>SEM images of the fractured surface of the FFF-printed GF/PA sample with (<b>a</b>) 0°, (<b>b</b>) 90°, and (<b>c</b>) ±45° printing orientation.</p>
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<p>Representative stress–strain curves for 3D-printed samples with 0° printing orientation: (<b>a</b>) PA; (<b>b</b>) CF/PA; (<b>c</b>) GF/PA.</p>
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<p>Effect of printing orientation on the stress–strain curves of 3D-printed (<b>a</b>) PA, (<b>b</b>) CF/PA and (<b>c</b>) GF/PA (100% infill density).</p>
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<p>Effect of fillers on the stress–strain curves of samples 3D-printed with 0° printing orientation and 100% infill density.</p>
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<p>Mechanical properties of 3D-printed PA and PA-based composites (<b>a</b>) Young’s modulus, (<b>b</b>) tensile strength, (<b>c</b>) stress at break, and (<b>d</b>) strain at break.</p>
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<p>Main effects plot for 3D-printed PA-based samples: (<b>a</b>) Young’s modulus, (<b>b</b>) tensile strength, (<b>c</b>) stress at break, and (<b>d</b>) strain at break.</p>
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<p>Comparison of experimental Young’s modulus and tensile strength with the predicted values for the optimized ANN model with one output: (<b>a</b>,<b>b</b>) Training results; (<b>c</b>,<b>d</b>) Testing results.</p>
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<p>Comparison of experimental Young’s modulus and tensile strength with the predicted values for the optimized ANN model with two outputs: (<b>a</b>,<b>b</b>) Training results; (<b>c</b>,<b>d</b>) Testing results.</p>
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<p>Comparison between the predicted outcomes using the regression and ANN models for 3D-printed: (<b>a</b>,<b>b</b>) PA, (<b>c</b>,<b>d</b>) GF/PA; and (<b>e</b>,<b>f</b>) CF/PA samples.</p>
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<p>Comparison between the predicted outcomes using the regression and ANN models for 3D-printed: (<b>a</b>,<b>b</b>) PA, (<b>c</b>,<b>d</b>) GF/PA; and (<b>e</b>,<b>f</b>) CF/PA samples.</p>
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21 pages, 5221 KiB  
Article
Biocomposites of Starch Industry Residues from Cassava and Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) for Food Packaging
by Flávia Rocha Drummond, Paulo Henrique Machado Cardoso, Javier Mauricio Anaya-Mancipe and Rossana Mara da Silva Moreira Thiré
Processes 2025, 13(3), 719; https://doi.org/10.3390/pr13030719 - 2 Mar 2025
Viewed by 233
Abstract
Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) is thermoplastic, biodegradable, and derived from renewable-source polymers; thus, it can be used as an alternative to traditional synthetic polymers to reduce damage to the environment. The production of cassava starch generates a high amount of cassava bagasse (about 93% of [...] Read more.
Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) is thermoplastic, biodegradable, and derived from renewable-source polymers; thus, it can be used as an alternative to traditional synthetic polymers to reduce damage to the environment. The production of cassava starch generates a high amount of cassava bagasse (about 93% of processed roots) in the separation step of starch. The utilization of this waste is essential due to the difficulty of transportation and storage, besides the detriment caused to the environment by its incorrect disposal. This work aimed to evaluate the possibility of using cassava bagasse as a reinforcement in the production of biocomposites with PHBV matrices by compression molding. The physical–chemical and thermal properties of these biocomposites were characterized. The residue can be used as a filler in compression-molded PHBV biocomposites. The most suitable formulation was 10 wt. %, despite the presence of some cassava bagasse (CB) agglomerations. This film could be used as rigid packaging for chilled or shelf-aqueous food. Full article
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<p>Illustration of biocomposite processes cassava bagasse and poly(3-hydroxybutyrate-3-co-hydroxyvalerate) (PHBV) by compression molding.</p>
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<p>Cassava bagasse characterization. (<b>A</b>) SEM images in two magnifications. Left: 70× and right: 500×; (<b>B</b>) FTIR-ATR spectrogram of CB as receded; and (<b>C</b>) thermal evaluation by DSC (1st cycle heat).</p>
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<p>Chemical and compositional evaluation of CB/PHBV biocomposites by infrared spectroscopy. (<b>A</b>) Range between 4000 and 2000 cm<sup>−1</sup>; and (<b>B</b>) range evaluation in 2000 to 550 cm<sup>−1</sup>.</p>
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<p>NMR of PHBV0, PHBV5, and PHBV10.</p>
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<p>DSC thermograms of 2nd heating cycle of PHBV0, PHBV5, and PHBV10.</p>
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<p>TGA thermogram of biocomposites varying the amount of CB, (<b>A</b>) PHBV0, (<b>B</b>) PHBV5, (<b>C</b>) PHBV10, and (<b>D</b>) neat CB specimen.</p>
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<p>X-ray diffractograms (<b>A</b>) of CB, PHBV0, PHBV5, and PHBV10; (<b>B</b>) illustrates the principles of X-ray diffraction calculations, including Bragg’s Law and the Scherrer equation.</p>
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<p>Photographs of CB/PHBV composites with three different CB concentrations, evaluating the wettability contact angle and surface for one of the samples.</p>
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<p>SEM images of the cross-section of both sides fractured, highlighting the CB agglomerates for the two studied concentrations: (<b>A</b>) PHBV5 – yellow circles; and (<b>B</b>) PHBV10 – orange arrows.</p>
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10 pages, 3294 KiB  
Communication
First Appraisal of Effective Microplastics Removal from the Textile Manufacturing Processes
by Estefanía Bonnail, Sebastián Vera, Julián Blasco and T. Ángel DelValls
Appl. Sci. 2025, 15(5), 2630; https://doi.org/10.3390/app15052630 - 28 Feb 2025
Viewed by 250
Abstract
The textile industry consumes large volumes of freshwater, producing enormous wastewater containing chemicals from dyeing and bathing, but also microplastics concentrations that have not been deeply studied. Liquid wastes from the synthetic and natural textile manufacturers were treated with a new disruptive technology [...] Read more.
The textile industry consumes large volumes of freshwater, producing enormous wastewater containing chemicals from dyeing and bathing, but also microplastics concentrations that have not been deeply studied. Liquid wastes from the synthetic and natural textile manufacturers were treated with a new disruptive technology (Adiabatic Sonic Evaporation and Crystallization, ASEC), which completely removed contaminants from water, providing distilled water and crystallized solids. The current study presents the characterization of the industrial residues and the obtained by-products: microplastics and organic matter contained in the solid residue were analyzed and characterized through chromatography. The results of the analyses displayed that compounds such as benzene, benzoic acid and 2,4-dymethyl-1-heptene were found in the synthetic industry water samples as degraded compounds of polyester and polypropylene. Meanwhile, the natural industry water also contained polyester, nylon and PMM polymer. After the depuration of samples, microplastics were completely retained in the solid phase, together with the organic matter (sulfate and surfactants) resulting on clean water. This is the first study focused on the study of microplastics generated by the textile industry and their prevention by removing them as solid waste. Full article
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<p>Scheme of the manufacture textile processes for synthetic (<b>left</b>) and natural (<b>right</b>) fibers and the sampling locations (S1, S2, S3, N).</p>
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15 pages, 3572 KiB  
Article
PLA Reinforced with Limestone Waste: A Way to Sustainable Polymer Composites
by Dora Sousa, Catarina Baleia and Pedro Amaral
Polymers 2025, 17(5), 662; https://doi.org/10.3390/polym17050662 - 28 Feb 2025
Viewed by 267
Abstract
Waste stone sludge generated by the extractive industry has traditionally posed significant disposal challenges. This study redefines stone sludge as a valuable raw material by incorporating it into polylactic acid (PLA) to create sustainable composite materials. Pellets and filaments composed of up to [...] Read more.
Waste stone sludge generated by the extractive industry has traditionally posed significant disposal challenges. This study redefines stone sludge as a valuable raw material by incorporating it into polylactic acid (PLA) to create sustainable composite materials. Pellets and filaments composed of up to 50% by weight of limestone powder and PLA were successfully produced using melt blending in a twin-screw extruder. Scanning electron microscopy (SEM), X-ray fluorescence (XRF), and X-ray diffraction (XRD) analyses revealed a uniform distribution of stone particles within the PLA matrix and confirmed the chemical and structural compatibility of the components. Thermogravimetric analysis (TGA) showed that the composites retained thermal stability, while mechanical testing demonstrated significant enhancements in stiffness, with an increase in elastic modulus for composites containing 50% limestone powder. The melt flow rate (MFR) decreases with increasing filler content. The brittleness also increased, reducing impact resistance. Mechanical tests were performed on injected and 3D-printed specimens. The filament produced was successfully used in 3D printing, with a small XYZ calibration cube. Full article
(This article belongs to the Section Circular and Green Polymer Science)
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<p>3devo filament maker schematics from the manual.</p>
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<p>SEM images of the utilized limestone powder (<b>a</b>). Size distribution in micrometers for the limestone powder (<b>b</b>).</p>
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<p>Pellets of the compound of PLA and limestone powder, (<b>a</b>) from virgin PLA, (<b>b</b>) from PLA recycled parts.</p>
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<p>(<b>a</b>) TGA thermograms, (<b>b</b>) DTG thermograms for PLA and composites.</p>
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<p>(<b>a</b>) TGA thermograms, (<b>b</b>) DTG thermograms for PLA and composites.</p>
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<p>(<b>a</b>) PLA filament of virgin PLA-LP, (<b>b</b>) recycled PLA-LP, (<b>c</b>) SEM image of the cross-section of the PLA-LP compound and (<b>d</b>) cube printed with a filament of 50 wt. % PLA/LP.</p>
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<p>Stress–strain curve for PLA and composites, injected (<b>a</b>) and printed (<b>b</b>). Attention to scale for comparison.</p>
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21 pages, 5488 KiB  
Article
Cellulose/TiO2 Humidity Sensor
by Susana Devesa, Zohra Benzarti, Madalena Costa, Diogo Cavaleiro, Pedro Faia and Sandra Carvalho
Sensors 2025, 25(5), 1506; https://doi.org/10.3390/s25051506 - 28 Feb 2025
Viewed by 160
Abstract
Resistivity-type humidity sensors, which detect changes in electrical resistance in response to variations in environmental humidity, have garnered significant interest due to their widespread application in industry, agriculture, and daily life. These sensors rely on diverse materials for fabrication, but their increasing variety [...] Read more.
Resistivity-type humidity sensors, which detect changes in electrical resistance in response to variations in environmental humidity, have garnered significant interest due to their widespread application in industry, agriculture, and daily life. These sensors rely on diverse materials for fabrication, but their increasing variety has contributed to the accumulation of electronic waste. As a biodegradable polymer, cellulose offers unique advantages, including a naturally hydrophilic structure and a large specific surface area. These properties enable cellulose to reduce e-waste generation while facilitating the efficient adsorption of water molecules. However, despite these benefits, humidity sensors based solely on cellulose often suffer from poor sensitivity due to its limited hydrophilicity and non-adjustable structure. To overcome these limitations, the development of composite materials emerges as a promising solution for enhancing the performance of cellulose-based humidity sensors. Combining the complementary properties of cellulose and TiO2, this work presents the development of a cellulose/TiO2 composite humidity sensor through a sustainable approach. The resulting composite material exhibits significantly improved sensitivity compared with a sensor fabricated purely from cellulose. To achieve this, TiO2 nanoparticles were incorporated into cellulose extracted from potato peels, and the composite film was fabricated using the casting method. The sensor’s performance was evaluated by analyzing the dependence of its complex impedance, measured over a frequency range between 2 kHz and 10 MHz, while varying relative humidity (RH). Full article
(This article belongs to the Section Physical Sensors)
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<p>Measuring chamber schematics (1—electrodes, 2—counterweights, 3—heating elements, 4—thermocouple, 5—g inlet and outlet, 6—samples holder).</p>
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<p>Photograph of the fabricated sensor sample.</p>
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<p>Diffractogram of (<b>a</b>) cellulose film and (<b>b</b>) TiO<sub>2</sub> nanoparticles.</p>
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<p>Raman spectra of (<b>a</b>) cellulose film and (<b>b</b>) TiO<sub>2</sub> nanoparticles.</p>
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<p>SEM micrographs of (<b>a</b>) cellulose and (<b>b</b>) cellulose/TiO<sub>2</sub> films.</p>
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<p>(<b>a</b>) SEM micrograph and (<b>b</b>) corresponding EDS elemental mapping of the cellulose/TiO<sub>2</sub> film.</p>
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<p>Electrical response of the cellulose film to moisture (0%, 50%, and 100%), at room temperature: (<b>a</b>) real part of the impedance as a function of frequency; (<b>b</b>) imaginary part of the impedance as a function of frequency; (<b>c</b>) Nyquist plots.</p>
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<p>Electrical response of the cellulose/TiO<sub>2</sub> film to moisture (0%, 50%, and 100%), at room temperature: (<b>a</b>) real part of the impedance as a function of frequency; (<b>b</b>) imaginary part of the impedance as a function of frequency; (<b>c</b>) Nyquist plots.</p>
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<p>Electrical response of the cellulose/TiO<sub>2</sub> film to moisture (0%, 50%, and 100%), at room temperature: (<b>a</b>) real part of the impedance as a function of frequency; (<b>b</b>) imaginary part of the impedance as a function of frequency; (<b>c</b>) Nyquist plots.</p>
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<p>Electrical response of cellulose and cellulose/TiO<sub>2</sub> films to moisture (0%, 50%, and 100%); impedance modulus, measured at room temperature and 2000 Hz.</p>
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<p>Electrical response of the cellulose/TiO<sub>2</sub> film to moisture (0%, 20%, 50%, 70%, and 100%), at room temperature: (<b>a</b>) real part of the impedance as a function of frequency; (<b>b</b>) imaginary part of the impedance as a function of frequency; (<b>c</b>) Nyquist plots.</p>
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<p>Electrical response of the cellulose/TiO<sub>2</sub> film to moisture (0%, 20%, 50%, 70%, and 100%), at room temperature: (<b>a</b>) real part of the impedance as a function of frequency; (<b>b</b>) imaginary part of the impedance as a function of frequency; (<b>c</b>) Nyquist plots.</p>
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<p>Dependence of the grain resistance on relative humidity and corresponding equivalent circuits adopted.</p>
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15 pages, 945 KiB  
Article
Incorporating Non-Linear Epoxy Resin Development in Infusion Simulations: A Dual-Exponent Viscosity Model Approach
by Mohammad W. Tahir, Umar Khan and Jan-Peter Schümann
Polymers 2025, 17(5), 657; https://doi.org/10.3390/polym17050657 - 28 Feb 2025
Viewed by 228
Abstract
In the field of liquid composite moulding (LCM) simulations, a long-standing assumption has dominated–the belief in constant resin viscosity. While effective in many cases, this assumption may not hold for the infusion process, which lasts for an extended period. This impacts the mechanical [...] Read more.
In the field of liquid composite moulding (LCM) simulations, a long-standing assumption has dominated–the belief in constant resin viscosity. While effective in many cases, this assumption may not hold for the infusion process, which lasts for an extended period. This impacts the mechanical properties of the cured epoxy, which are crucial for load transfer in polymer structures. The majority of epoxy resins operate on a bipartite foundation, wherein their viscosity undergoes dynamic alterations during the process of cross-linking. Temperature and cross-linking intricately interact, with elevated temperatures initially reducing viscosity due to kinetic energy but later increasing it as cross-linking accelerates. This interplay significantly influences the efficiency of the infusion process, especially in large and intricate moulds. This article explores the significant temperature dependence of epoxy resin viscosity, proposing an accurate model rooted in its non-linear evolution. This model aligns with empirical evidence, offering insights into determining the optimal starting temperature for efficient mould filling. This study presents an advanced infusion model that extends existing non-linear dual-split viscosity approaches by incorporating the experimental validation of viscosity variations. Unlike previous models that primarily focus on theoretical or numerical frameworks, this work integrates experimental insights to optimize infusion temperature for efficient resin infusion in large and complex parts. Building on these findings, a novel mould-filling technique is proposed to enhance efficiency and reduce material waste. Full article
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<p>Schematic of the LCM. Different component of the resin to be mixed in specific proportion are shown with different colours.</p>
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<p>Plot of temperature development of RIMR 035c epoxy resin with four different hardeners redrawn from manufacturer datasheet.</p>
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<p>Plot of viscosity development with curing for the epoxy resin with fitted data for single exponent model presented in Equation (<a href="#FD1-polymers-17-00657" class="html-disp-formula">1</a>).</p>
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<p>Plot of viscosity development with curing for the epoxy resin with fitted data for dual exponent model shown in Equation (<a href="#FD3-polymers-17-00657" class="html-disp-formula">3</a>).</p>
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<p>Schematic diagram of a typical infusion process. Already resin filled region is highlighted with different colour.</p>
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<p>Plot of temperature development of RIMR 035c epoxy resin with four different hardeners under insulated setup [<a href="#B29-polymers-17-00657" class="html-bibr">29</a>].</p>
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<p>Comparison of the flow front position for real infusion of epoxy and the model presented in Equation (<a href="#FD6-polymers-17-00657" class="html-disp-formula">6</a>).</p>
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<p>Plot of the flow front with time for UD flow case. The dotted red line exemplifies a three-hour mould filling time-frame. Infusion at 40 or 45 °C results in an early gelation point causing an incomplete mould filling, while 25 °C causes inefficient filling and extended duration. An optimal starting temperature of 35 °C ensures efficient mould filling.</p>
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16 pages, 2647 KiB  
Article
Mechanical Properties of PVC/TPU Blends Enhanced with a Sustainable Bio-Plasticizer
by Yitbarek Firew Minale, Ivan Gajdoš, Pavol Štefčák, Tamás Szabó, Annamaria Polyákné Kovács, Andrea Ádámné Major and Kálmán Marossy
Sustainability 2025, 17(5), 2033; https://doi.org/10.3390/su17052033 - 26 Feb 2025
Viewed by 446
Abstract
The development of sustainable and mechanically versatile polymeric materials is essential to meet the growing demand for eco-friendly, high-performance products. This study investigates the mechanical properties of blends comprising polyvinyl chloride (PVC), thermoplastic polyurethane (TPU), and glycerol diacetate monolaurate, a bio-based plasticizer derived [...] Read more.
The development of sustainable and mechanically versatile polymeric materials is essential to meet the growing demand for eco-friendly, high-performance products. This study investigates the mechanical properties of blends comprising polyvinyl chloride (PVC), thermoplastic polyurethane (TPU), and glycerol diacetate monolaurate, a bio-based plasticizer derived from waste cooking oil, addressing the underexplored combined effects of these components. By varying the proportions, the blends’ tensile strength, elasticity, elongation at break, and hardness were tailored for diverse applications. Incorporating the bio-plasticizer significantly enhanced the PVC’s flexibility and elongation at break, while reducing its tensile strength and rigidity. The addition of TPU further enhanced the elasticity, toughness, and resilience, with the final properties governed by synergistic interactions between PVC’s rigidity, TPU’s elasticity, and the plasticizer’s softening effects. Dynamic mechanical analysis (DMA) confirmed that the bio-plasticizer enhanced the compatibility between the PVC and TPU, leading to ternary PVC/TPU/bio-plasticizer blends with an improved elasticity and elongation at break, without a significant loss in tensile strength. These blends exhibited a broad range of tunable properties, enabling applications from flexible films to impact-resistant components. Overall, these findings highlight the potential of PVC/TPU/bio-plasticizer systems to deliver high-performance materials with enhanced sustainability. This work offers valuable insights for developing greener polymer systems and advancing the creation of tailored materials for diverse industrial applications in alignment with global sustainability goals. Full article
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<p>The molecular structure of glycerol diacetate monolaurate.</p>
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<p>Representative tensile test specimens of the polymer blends.</p>
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<p>DMA curve of polymer blend samples.</p>
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<p>Stress–strain curves of the tested polymer blends.</p>
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<p>Tensile strength and Young’s modulus of polymer blends with varying compositions.</p>
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<p>Elongation at break of polymer blends with varying compositions.</p>
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<p>(<b>a</b>) Stress localization and neck formation in Rigid PVC; (<b>b</b>) uniform deformation in plasticized PVC under tensile load.</p>
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<p>Shore A and Shore D hardness of polymer blends with varying compositions.</p>
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104 pages, 13734 KiB  
Review
Advancing Textile Waste Recycling: Challenges and Opportunities Across Polymer and Non-Polymer Fiber Types
by Mehrdad Seifali Abbas-Abadi, Brecht Tomme, Bahman Goshayeshi, Oleksii Mynko, Yihan Wang, Sangram Roy, Rohit Kumar, Bhargav Baruah, Karen De Clerck, Steven De Meester, Dagmar R. D’hooge and Kevin M. Van Geem
Polymers 2025, 17(5), 628; https://doi.org/10.3390/polym17050628 - 26 Feb 2025
Viewed by 516
Abstract
The growing environmental impact of textile waste, fueled by the rapid rise in global fiber production, underscores the urgent need for sustainable end-of-life solutions. This review explores cutting-edge pathways for textile waste management, spotlighting innovations that reduce reliance on incineration and landfilling while [...] Read more.
The growing environmental impact of textile waste, fueled by the rapid rise in global fiber production, underscores the urgent need for sustainable end-of-life solutions. This review explores cutting-edge pathways for textile waste management, spotlighting innovations that reduce reliance on incineration and landfilling while driving material circularity. It highlights advancements in collection, sorting, and pretreatment technologies, as well as both established and emerging recycling methods. Smart collection systems utilizing tags and sensors show great promise in streamlining logistics by automating pick-up routes and transactions. For sorting, automated technologies like near-infrared and hyperspectral imaging lead the way in accurate and scalable fiber separation. Automated disassembly techniques are effective at removing problematic elements, though other pretreatments, such as color and finish removal, still need to be customized for specific waste streams. Mechanical fiber recycling is ideal for textiles with strong mechanical properties but has limitations, particularly with blended fabrics, and cannot be repeated endlessly. Polymer recycling—through melting or dissolving waste polymers—produces higher-quality recycled materials but comes with high energy and solvent demands. Chemical recycling, especially solvolysis and pyrolysis, excels at breaking down synthetic polymers like polyester, with the potential to yield virgin-quality monomers. Meanwhile, biological methods, though still in their infancy, show promise for recycling natural fibers like cotton and wool. When other methods are not viable, gasification can be used to convert waste into synthesis gas. The review concludes that the future of sustainable textile recycling hinges on integrating automated sorting systems and advancing solvent-based and chemical recycling technologies. These innovations, supported by eco-design principles, progressive policies, and industry collaboration, are essential to building a resilient, circular textile economy. Full article
(This article belongs to the Section Circular and Green Polymer Science)
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Graphical abstract

Graphical abstract
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<p>The textile manufacturing chain, from building block to end product.</p>
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<p>Fiber categories based on polymer and fiber types.</p>
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<p>Worldwide distribution of fiber extraction and production. Natural fibers represent 30% of the total, while man-made fibers represent 70% [<a href="#B17-polymers-17-00628" class="html-bibr">17</a>].</p>
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<p>The viscose production process [<a href="#B101-polymers-17-00628" class="html-bibr">101</a>,<a href="#B102-polymers-17-00628" class="html-bibr">102</a>].</p>
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<p>The lyocell production process [<a href="#B109-polymers-17-00628" class="html-bibr">109</a>].</p>
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<p>Overall reaction for important polymerizations. The targeted polymer is listed above the arrow for clarity [<a href="#B111-polymers-17-00628" class="html-bibr">111</a>,<a href="#B112-polymers-17-00628" class="html-bibr">112</a>,<a href="#B114-polymers-17-00628" class="html-bibr">114</a>].</p>
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<p>The industrial polymerization and structure of PET [<a href="#B130-polymers-17-00628" class="html-bibr">130</a>,<a href="#B131-polymers-17-00628" class="html-bibr">131</a>].</p>
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<p>PA6,6 vs. PA6.</p>
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<p>Waste hierarchy staircase for textile end-of-life options. Ideally, processes at the top are used until they no longer yield a product or secondary raw material of sufficient quality, in which case a process lower down should be used, except for incineration or landfill.</p>
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<p>Textile waste management in the U.S. (1960–2018) [<a href="#B197-polymers-17-00628" class="html-bibr">197</a>].</p>
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<p>Example of the attenuated total reflection–Fourier transform infrared (ATR-FTIR) spectra of common fibers [<a href="#B231-polymers-17-00628" class="html-bibr">231</a>,<a href="#B232-polymers-17-00628" class="html-bibr">232</a>,<a href="#B233-polymers-17-00628" class="html-bibr">233</a>,<a href="#B234-polymers-17-00628" class="html-bibr">234</a>].</p>
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<p>Tire textile recovery [<a href="#B247-polymers-17-00628" class="html-bibr">247</a>].</p>
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<p>Re-extrusion of fibers from PET bottle or textile waste.</p>
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<p>The chain extension of recycled PET using PMDA [<a href="#B338-polymers-17-00628" class="html-bibr">338</a>].</p>
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<p>Dissolution of cellulose in an ionic liquid using the anti-H<sub>2</sub> bonding mechanism [<a href="#B357-polymers-17-00628" class="html-bibr">357</a>].</p>
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<p>Thermogravimetric analysis curves for original, hydrolyzed, and man-made cotton fibers [<a href="#B348-polymers-17-00628" class="html-bibr">348</a>].</p>
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<p>Functional groups of six polymer types, with examples theoretically lumped into one chain for the compactness of the figure [<a href="#B392-polymers-17-00628" class="html-bibr">392</a>,<a href="#B393-polymers-17-00628" class="html-bibr">393</a>,<a href="#B394-polymers-17-00628" class="html-bibr">394</a>,<a href="#B395-polymers-17-00628" class="html-bibr">395</a>,<a href="#B396-polymers-17-00628" class="html-bibr">396</a>,<a href="#B397-polymers-17-00628" class="html-bibr">397</a>,<a href="#B398-polymers-17-00628" class="html-bibr">398</a>,<a href="#B399-polymers-17-00628" class="html-bibr">399</a>,<a href="#B400-polymers-17-00628" class="html-bibr">400</a>,<a href="#B401-polymers-17-00628" class="html-bibr">401</a>,<a href="#B402-polymers-17-00628" class="html-bibr">402</a>,<a href="#B403-polymers-17-00628" class="html-bibr">403</a>,<a href="#B404-polymers-17-00628" class="html-bibr">404</a>,<a href="#B405-polymers-17-00628" class="html-bibr">405</a>,<a href="#B406-polymers-17-00628" class="html-bibr">406</a>,<a href="#B407-polymers-17-00628" class="html-bibr">407</a>].</p>
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<p>The thermal degradation process of PVC [<a href="#B408-polymers-17-00628" class="html-bibr">408</a>].</p>
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<p>Thermogravimetric analysis graphs of different polymers according to <a href="#polymers-17-00628-f017" class="html-fig">Figure 17</a> [<a href="#B392-polymers-17-00628" class="html-bibr">392</a>,<a href="#B393-polymers-17-00628" class="html-bibr">393</a>,<a href="#B394-polymers-17-00628" class="html-bibr">394</a>,<a href="#B395-polymers-17-00628" class="html-bibr">395</a>,<a href="#B396-polymers-17-00628" class="html-bibr">396</a>,<a href="#B397-polymers-17-00628" class="html-bibr">397</a>,<a href="#B398-polymers-17-00628" class="html-bibr">398</a>,<a href="#B399-polymers-17-00628" class="html-bibr">399</a>,<a href="#B400-polymers-17-00628" class="html-bibr">400</a>,<a href="#B401-polymers-17-00628" class="html-bibr">401</a>,<a href="#B402-polymers-17-00628" class="html-bibr">402</a>,<a href="#B403-polymers-17-00628" class="html-bibr">403</a>,<a href="#B404-polymers-17-00628" class="html-bibr">404</a>,<a href="#B405-polymers-17-00628" class="html-bibr">405</a>,<a href="#B406-polymers-17-00628" class="html-bibr">406</a>,<a href="#B417-polymers-17-00628" class="html-bibr">417</a>].</p>
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<p>The yields of PE pyrolysis products vs. temperature (adapted from [<a href="#B442-polymers-17-00628" class="html-bibr">442</a>]). PNA stands for polynuclear aromatics [<a href="#B442-polymers-17-00628" class="html-bibr">442</a>].</p>
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<p>Diagram illustrating PVC degradation and the subsequent reactions with light olefins during the pyrolysis of waste polyolefins [<a href="#B441-polymers-17-00628" class="html-bibr">441</a>].</p>
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<p>The proposed mechanism of PET degradation at elevated temperatures [<a href="#B411-polymers-17-00628" class="html-bibr">411</a>,<a href="#B452-polymers-17-00628" class="html-bibr">452</a>,<a href="#B453-polymers-17-00628" class="html-bibr">453</a>].</p>
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<p>Examples of PET depolymerization via solvolysis.</p>
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<p>Catalytic hydrogenation of PET via Ru(II) PNN pincer complexes [<a href="#B528-polymers-17-00628" class="html-bibr">528</a>].</p>
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<p>Reductive dechlorination of PVC to PE with the iridium catalyst/Et<sub>3</sub>SiH [<a href="#B565-polymers-17-00628" class="html-bibr">565</a>].</p>
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<p>Carbon footprint ranges of state-of-the-art virgin and recycled fiber production. v-PET = virgin PET; r-PET = recycled PET via methanolysis pathway [<a href="#B571-polymers-17-00628" class="html-bibr">571</a>]; r-PET, hydrolysis = PET recycled via the alkaline hydrolysis pathway [<a href="#B542-polymers-17-00628" class="html-bibr">542</a>]; v-Cotton and v-Viscose = virgin fibers; r-Viscose, CCA = cellulose carbamate fiber derived from waste cotton [<a href="#B573-polymers-17-00628" class="html-bibr">573</a>].</p>
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