Polymer TestingPub Date : 2025-07-19DOI: 10.1016/j.polymertesting.2025.108934
Hechen Liu , Ying Zou , Jinyang Xu , Songsong Zhou , Xiong Wu , Yunpeng Liu
{"title":"Efficient recycling of anhydride-cured epoxy resins for electrical insulation: Green economy and tunable performance","authors":"Hechen Liu , Ying Zou , Jinyang Xu , Songsong Zhou , Xiong Wu , Yunpeng Liu","doi":"10.1016/j.polymertesting.2025.108934","DOIUrl":"10.1016/j.polymertesting.2025.108934","url":null,"abstract":"<div><div>The accumulation of resin-based electrical waste poses significant resource wastage and environmental challenges, with chemical recycling representing a key solution. This study innovatively developed a graded alcoholysis-hydrolysis reaction strategy, enabling both the efficient degradation of anhydride-cured epoxy resin within 1 h under mild conditions and the subsequent reuse of the degradation products in regeneration of new epoxy resins. Central to this work is a uniquely designed benzyl alcohol/K<sub>3</sub>PO<sub>4</sub> recycling system, which enables the closed-loop utilization of not only the epoxy resin but also the system itself, owing to the facile separation of its components. Specifically, the average recovery rates of benzyl alcohol and K<sub>3</sub>PO<sub>4</sub> can reach 80.38 % and 90.95 % over 10 cycles, while the recycling system constructed after 10 cycles using them retained over 80 % of degradation efficiency. Furthermore, the study systematically investigated the synthesis of new epoxy resins by adjusting the proportion of recycled resin. As the recycled resin content increased, the insulation performance of the regenerated resin improved, whereas its mechanical strength and thermal stability exhibited a decline. When the recycled resin content reached 30 wt%, the breakdown strength of the regenerated resin increased by 13.5 % compared to the pristine resin, while maintaining a flexural stress of 72.87 MPa and a glass transition temperature exceeding 100 °C. This research provides innovative insights and a theoretical foundation for advancing green decommissioning technologies for resin-based electrical equipment.</div></div>","PeriodicalId":20628,"journal":{"name":"Polymer Testing","volume":"150 ","pages":"Article 108934"},"PeriodicalIF":5.0,"publicationDate":"2025-07-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144665612","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Flexible sensor based on self-assembly of halloysite nanotubes in ionic liquids/thermoplastic polyurethane composites","authors":"Xiuqi Zhou , Jiajun Chen , Wenwu Zhang , Wenming Zhao , Qinghu Wang , Xiongqi Peng","doi":"10.1016/j.polymertesting.2025.108931","DOIUrl":"10.1016/j.polymertesting.2025.108931","url":null,"abstract":"<div><div>Ionogels are gradually entering the flexible sensor field due to their excellent ionic conductivity, thermal stability and wide electrochemical window. It is critical to balance the mechanical and conductivity properties of ionogels for further application. Herein, inspired by vapor-induced phase separation strategy and self-assembled strategy, a flexible strain-sensor was developed by adding ionic liquid (IL) decorated halloysite nanotube (HNT) into thermoplastic polyurethane (TPU) matrix. As a phase separation material, the rigid regions of TPU offered strength and toughness for ionogels, while the soft regions offered high stretchability. Due to electrostatic interaction, the cations and anions of IL self-assembled onto the inner and outer surface of HNT. The HNT obtained orderly arrangement structure after shear process, which provides effective ionic transport channels for IL. As a strain sensor, the as-prepared TPU@IL@HNT sensor exhibited highly gauge factor, fast response speed (400 ms), and excellent cycle stability (5625 cycles) at a strain of 40 %. A linear relation between strain and resistance change was found for TPU@IL@HNT sensor, which is an important criterion for their application on strain sensors. As a whole, the TPU@IL@HNT sensor prepared in this work could serve as an excellent sensing unit for wearable devices.</div></div>","PeriodicalId":20628,"journal":{"name":"Polymer Testing","volume":"150 ","pages":"Article 108931"},"PeriodicalIF":5.0,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144670908","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Advanced epoxy composites for tribological Applications: Investigating the role of hybrid ceramic and lubricant fillers","authors":"Ratchagaraja Dhairiyasamy , Welson Bassi , Abdullah A. Algethami , Bahaa Saleh , Sivakumar Jaganathan , Deekshant Varshney , Subhav Singh","doi":"10.1016/j.polymertesting.2025.108932","DOIUrl":"10.1016/j.polymertesting.2025.108932","url":null,"abstract":"<div><div>Epoxy resins are widely employed in structural and industrial applications due to their high strength and chemical resistance, but their poor tribological performance under dynamic loading conditions limits their use in high-friction environments. Enhancing these properties through the use of functional fillers presents a promising approach; however, the combined effects of reinforcing and lubricating agents within epoxy remain underexplored. This study aims to evaluate the tribological and thermal performance of epoxy composites reinforced with silicon carbide (SiC), graphite (Gr), and molybdenum disulfide (MoS<sub>2</sub>), both individually and in hybrid combinations. Eight composite formulations were prepared via mechanical stirring, ultrasonication, and compression molding, and were subjected to pin-on-disc testing under varying normal loads and sliding speeds. The composites were characterized in terms of coefficient of friction (COF), specific wear rate, and interfacial temperature rise, alongside SEM and EDX analysis of the worn surfaces. Results revealed that SiC improved wear resistance, while Gr and MoS<sub>2</sub> reduced COF and surface heating. The ternary composite (EP + SiC + Gr + MoS<sub>2</sub>) demonstrated the best overall performance, with a 94 % wear reduction and 40 % lower COF compared to pure epoxy. These findings confirm the synergistic benefit of combining reinforcing and lubricating fillers in polymer composites. Future studies should explore long-term performance and applicability under real operating conditions.</div></div>","PeriodicalId":20628,"journal":{"name":"Polymer Testing","volume":"150 ","pages":"Article 108932"},"PeriodicalIF":5.0,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144670907","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Polymer TestingPub Date : 2025-07-17DOI: 10.1016/j.polymertesting.2025.108928
Junsu Kim , Seungjae Lee , Mingeun Park , Yehyun Kim , Nam-Joon Cho , Hyungju Ahn , Du Yeol Ryu
{"title":"Depth-dependent structural analysis of polyolefin multilayer films using microbeam X-ray diffraction","authors":"Junsu Kim , Seungjae Lee , Mingeun Park , Yehyun Kim , Nam-Joon Cho , Hyungju Ahn , Du Yeol Ryu","doi":"10.1016/j.polymertesting.2025.108928","DOIUrl":"10.1016/j.polymertesting.2025.108928","url":null,"abstract":"<div><div>Recent tightening of global regulations on plastic waste treatment has promoted the use of single type materials (over 95 %) with similar chemical identities. To meet such a mono-material regulation for upcycling and downcycling, polyolefin (PO) multilayer films comprising polyethylene (PE) and polypropylene (PP) have been most widely fabricated with the other functional layers because of their complementary physicochemical properties. To characterize depth-dependent compositional and structural properties of the PO multilayer films, we propose an analytical integration of a focused ion beam with scanning electron microscopy (FIB-SEM) technique and synchrotron microbeam wide-angle x-ray diffraction (M-WAXD). The two types of PE/(PE + PP)/PE and PP/PE/PP multilayer films were sequentially step-milled using the FIB-SEM, which enabled the high-resolution depth control of the films. The step-milled sculptures of multilayer films were exposed normal to microbeam x-rays in a transmission-mode, providing insights into the composition, nanoparticle dispersion, and crystal orientation as a function of film thickness. Our results highlight the analytical capability using an effective combination of FIB-SEM technique and M-WAXD, pointing out the importance of depth-dependent structural analysis for mono-material PO multilayer films.</div></div>","PeriodicalId":20628,"journal":{"name":"Polymer Testing","volume":"150 ","pages":"Article 108928"},"PeriodicalIF":5.0,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144653310","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Polymer TestingPub Date : 2025-07-17DOI: 10.1016/j.polymertesting.2025.108933
C. Valdés , V. Guzmán , M. Mamani , C. Vergara , R. Andler
{"title":"Desulfurization of vulcanized rubber by a synergism of chemical and biological treatment, with the strains Gordonia desulfuricans and Rhodococcus erythropolis","authors":"C. Valdés , V. Guzmán , M. Mamani , C. Vergara , R. Andler","doi":"10.1016/j.polymertesting.2025.108933","DOIUrl":"10.1016/j.polymertesting.2025.108933","url":null,"abstract":"<div><div>Developing and improving methods for the management of rubber waste accumulation and its recycling are crucial in addressing environmental problems, and desulfurization is a critical preliminary step before the rubber degradation. This study evaluates the desulfurization of pre- and post-treated vulcanized rubber using a green chemistry method that combines microwave (MW) with hydrogen peroxide and sulfur-oxidizing bacterial strains, <em>Gordonia desulfuricans</em> and <em>Rhodococcus erythropolis</em>. The results indicate that the rubber particles subjected to a synergism of a both treatments were able to continue being desulfurized despite the preliminary treatment. This can be verified in a greater mass loss (14.1 ± 0.8 % using <em>G. desulfuricans</em>, and 11 ± 0.4 % using <em>R. erythropolis</em>, with MW pretreatment) and sulfate release when combining both treatments (14.4 ± 0.7 mg/g using <em>G. desulfuricans</em>, and 22.4 ± 1 mg/g using <em>R. erythropolis</em>, with MW pretreatment). Also, significant changes in C-S and S-O bands, and greater surface fragmentation. A decrease in cross-link density was also observed in cultures with unpretreated rubber and in particles biologically pretreated with subsequent chemical treatment (5.18 × 10<sup>−4</sup>±3.2 × 10<sup>−5</sup> using <em>G. desulfuricans</em> and 5.4 × 10<sup>−4</sup>±4.5 × 10<sup>−5</sup> using <em>R. erythropolis</em>, with MW post-treatment). In addition, the analyses of metals copper, lead, chromium, barium and antimony showed that they were detected in concentrations lower than the maximum limits allowed for effluent discharges to sewage networks, which allows to consider that it consists of an environmentally safe method, reaching values of 1341, 3.6, 3.2, 42, and <1 μg/L, respectively with MW method. Finally, when evaluating desulfurization with biological pretreatment, and subsequent chemical treatment, better results were obtained.</div></div>","PeriodicalId":20628,"journal":{"name":"Polymer Testing","volume":"150 ","pages":"Article 108933"},"PeriodicalIF":5.0,"publicationDate":"2025-07-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144665611","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Polymer TestingPub Date : 2025-07-12DOI: 10.1016/j.polymertesting.2025.108927
F.E. Fiorini , A. Canegrati , L.M. Martulli , P. Steck , A. Bernasconi
{"title":"Stress triaxiality and failure in SFRPs: a novel workflow for failure curve determination, considering fibre orientation and specimen geometry","authors":"F.E. Fiorini , A. Canegrati , L.M. Martulli , P. Steck , A. Bernasconi","doi":"10.1016/j.polymertesting.2025.108927","DOIUrl":"10.1016/j.polymertesting.2025.108927","url":null,"abstract":"<div><div>This research investigates the static failure behaviour of a PA6T/6I GF50, focusing on the distribution of the stress triaxiality at critical points where failure is expected. The study explores whether a relationship exists between this stress state indicator and the strain experienced by the material, providing insights into when critical failure conditions are reached. Experimental tests, including uniaxial, biaxial, bending and shear, were conducted on various specimen types and loading orientations relative to their injection moulding direction. Finite element simulations, accounting for material's anisotropic elasto-plastic response, were run to evaluate the critical local stresses at failure locations. Digital image correlation was employed throughout the test campaign to monitor strain evolution. The evolution of the stress triaxiality during loading was computed from simulation results at both the macro (composite level) and micro-scales (matrix level). At the macro scale, it was evaluated using both isotropic (von Mises) and anisotropic (Hill 48) yield models. However, neither approach successfully identified generalized failure curves, as those correlating stress triaxiality with equivalent plastic strain, applicable across all loading scenarios and specimen geometries. To overcome this limitation, a new approach based on the calculation of the stress triaxiality and equivalent plastic strain locally at critical failure points was proposed. This allowed the identification of a failure curve that is independent of loading conditions and specimen geometry, underscoring the importance of triaxiality-based material characterization over traditional uniaxial approaches for accurately predicting failure in anisotropic short fibre-reinforced polymers.</div></div>","PeriodicalId":20628,"journal":{"name":"Polymer Testing","volume":"150 ","pages":"Article 108927"},"PeriodicalIF":5.0,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144633541","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Polymer TestingPub Date : 2025-07-12DOI: 10.1016/j.polymertesting.2025.108921
Van Anh Thi Nguyen , Sun-Ho Jang , Yebom Kim , Yong-Seok Choi , Sung-Kon Kim , Seongseop Kim , Jun Woo Jeon
{"title":"Enhanced mechanical properties of biodegradable poly(butylene adipate-co-terephthalate) through naphthalate incorporation","authors":"Van Anh Thi Nguyen , Sun-Ho Jang , Yebom Kim , Yong-Seok Choi , Sung-Kon Kim , Seongseop Kim , Jun Woo Jeon","doi":"10.1016/j.polymertesting.2025.108921","DOIUrl":"10.1016/j.polymertesting.2025.108921","url":null,"abstract":"<div><div>Poly(butylene adipate-co-terephthalate) (PBAT) serves as a viable substitute for low-density polyethylene (LDPE), particularly in agricultural films and packaging. However, for broader application of PBAT, extensive research has been conducted to fundamentally enhance its mechanical properties. This study introduces a novel PBAT copolymer that incorporates naphthalate content to enhance mechanical performance by partially replacing terephthalate content with rigid aromatic naphthalate content. Synthesized via a two-step melt polymerization method with varying dimethyl 2,6-naphthalenedicarboxylate (DMN) content (0–100 mol% relative to the total phthalate content), the copolymer demonstrated a significant increase in tensile strength, reaching 56.01 MPa for PBATN80, compared to 14.43 MPa for pure PBAT, while maintaining elongation at break between 530 % and 743 %. X-ray diffraction analysis revealed that the crystalline structure of the copolymers changed in response to increasing naphthalate content; specifically, samples with naphthalate content exceeding 50 mol% exhibited distinct peaks associated with poly(butylene-2,6-naphthalate). This enhancement in their mechanical properties is believed to be attributed to the similarities in characteristics with <em>poly(butylene naphthalate) (</em>PBN). Importantly, biodegradability was preserved, albeit at slightly reduced rates. This research highlights a promising strategy to enhance mechanical properties of PBAT without compromising its biodegradable nature, suggesting its potential for sustainable applications.</div></div>","PeriodicalId":20628,"journal":{"name":"Polymer Testing","volume":"150 ","pages":"Article 108921"},"PeriodicalIF":5.0,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144670909","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Polymer TestingPub Date : 2025-07-12DOI: 10.1016/j.polymertesting.2025.108924
Fakhri-Eddin N. Lahfaidh, Nathanael Guigo, Luc Vincent, Nicolas Sbirrazzuoli
{"title":"Shedding light on the impact of a dissolution-precipitation recycling process on crystallization and thermal stability of PBS","authors":"Fakhri-Eddin N. Lahfaidh, Nathanael Guigo, Luc Vincent, Nicolas Sbirrazzuoli","doi":"10.1016/j.polymertesting.2025.108924","DOIUrl":"10.1016/j.polymertesting.2025.108924","url":null,"abstract":"<div><div>Poly(butylene succinate) (PBS) was recycled via dissolution/precipitation using Cyrene as a green solvent. The PBS recyclates were characterized by SEC, NMR, FTIR and TGA. The recycling process selectively removed the most polar chains and increased the proportion of shorter chains (lower M<sub>n</sub>), as determined by size exclusion chromatography (SEC). Nuclear magnetic resonance (NMR) and infrared (IR) spectroscopy confirmed a reduction in -OH end groups alongside an increase in -CH<sub>3</sub> end groups, indicating a slight decrease in polarity. This selective chain alteration significantly improved crystallization, as demonstrated by advanced kinetic analyses and Hoffman-Lauritzen (HL) theory. A lower energy barrier to nucleation (<em>K</em><sub>g</sub>) for recycled PBS (rPBS) highlighted an enhanced nucleation process, facilitating earlier crystallization during both heating and cooling, despite reduced diffusion. The recycled chains achieved favorable positioning more readily, influenced by entropic effects rather than the energetic barriers typically encountered during heating. This observation was further supported by higher pre-exponential term values in HL's equation for rPBS. Moreover, the pronounced crystallization differences during cooling were attributed to the low <em>K</em><sub>g</sub> values, emphasizing nucleation as the primary driving force. Ultimately, the formation of shorter chains and reduced polarity in rPBS were identified as key contributors to enhanced nucleation. Temperature-Modulated DSC (TOPEM) confirmed a structural heterogeneity inside the recycled sample. The thermal stability of both polymers was investigated, showing increased degradation at lower heating rates for rPBS, while being comparable to the fresh product at higher rates. Degradation mechanisms were studied using isoconversional kinetics, and showed major differences from 310 to 370 °C.</div></div>","PeriodicalId":20628,"journal":{"name":"Polymer Testing","volume":"150 ","pages":"Article 108924"},"PeriodicalIF":5.0,"publicationDate":"2025-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144633540","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Polymer TestingPub Date : 2025-07-10DOI: 10.1016/j.polymertesting.2025.108923
Zhenyan Xie , Guangkai Liao , Yuejun Liu , Yuankang Li , Bowen Li , Lingna Cui , Shuhong Fan , Diansong Gan
{"title":"Investigating the nano-scale creep behavior of BOPA6 films via nanoindentation","authors":"Zhenyan Xie , Guangkai Liao , Yuejun Liu , Yuankang Li , Bowen Li , Lingna Cui , Shuhong Fan , Diansong Gan","doi":"10.1016/j.polymertesting.2025.108923","DOIUrl":"10.1016/j.polymertesting.2025.108923","url":null,"abstract":"<div><div>In this study, the nano-scale creep behavior of biaxially oriented polyamide 6 (BOPA6) films was investigated via instrumented nanoindentation. A modified empirical equation was proposed to characterize the evolution of strain rate during the loading stage, showing excellent agreement with the experimental data (R<sup>2</sup> > 0.99). It was observed that an elevated loading rate resulted in higher strain rates and smoother strain-displacement curves, indicating a transition from thermally activated localized deformation to stress-driven cooperative mechanisms, as described by the Eyring activation model. In the holding stage, a power-law equation was used to analyze the creep behavior and determine the creep stress exponent <em>n.</em> It can be found that the value of <em>n</em> increased significantly with the elevated maximum holding load, suggesting enhanced stress sensitivity and the activation of viscoplastic mechanisms. These time-dependent deformation mechanisms were further interpreted within the framework of the Eyring activation model, which clarified the transition from local thermally activated molecular rearrangement to stress-driven cooperative deformation. Overall, these results deepen the understanding of nano-scale creep behavior in semi-crystalline polymers and offer theoretical guidance for enhancing the mechanical properties of BOPA6 films in advanced packaging and flexible electronics.</div></div>","PeriodicalId":20628,"journal":{"name":"Polymer Testing","volume":"150 ","pages":"Article 108923"},"PeriodicalIF":5.0,"publicationDate":"2025-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144605001","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Polymer TestingPub Date : 2025-07-10DOI: 10.1016/j.polymertesting.2025.108925
Aleksandra M. Fage , Christian A. Backhaus , Wolfgang Becker , Günter Lorenz , Anita Lorenz , Karsten Rebner , Frank Henning
{"title":"Mid- and near-infrared spectroscopies for quantitative tracking of isocyanate content: Streamlined development of monitoring tools for reactive extrusion synthesis of specialty polyurethanes","authors":"Aleksandra M. Fage , Christian A. Backhaus , Wolfgang Becker , Günter Lorenz , Anita Lorenz , Karsten Rebner , Frank Henning","doi":"10.1016/j.polymertesting.2025.108925","DOIUrl":"10.1016/j.polymertesting.2025.108925","url":null,"abstract":"<div><div>Robust in-situ monitoring can expedite the development and tuning of reactive extrusion (REX) processes, especially for the synthesis of polymers requiring insight into the reaction course, such as specialty polyurethanes (PUs). In order to advance the feasibility of such analysis, our research concentrated on a spectroscopic protocol that combines at-line mid-infrared (MIR) and on-line near-infrared (NIR) measurements in a laboratory extruder, assessing both their qualitative and quantitative capabilities. To mimic the depletion of the reactive species during polymerisation, a series of premixes were formulated and characterised under non-reactive conditions using a benchmark pair of a polyol and a diisocyanate. By this means, we identified suitable spectral features for quantifying isocyanate content via multivariate regression models. This approach achieved good calibration metrics for both MIR and NIR models and enabled a robust assessment of their predictive performance through cross-validation, using only a moderate number of spectral datasets. Our work is therefore the first step towards establishing a method for in-process NIR analysis with streamlined at-line MIR verification. It provides a shortcut for designing monitored REX syntheses of PUs and other material systems amenable to quantitative calibration based on spectroscopic data from raw reagents.</div></div>","PeriodicalId":20628,"journal":{"name":"Polymer Testing","volume":"150 ","pages":"Article 108925"},"PeriodicalIF":5.0,"publicationDate":"2025-07-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144631325","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}