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UV-Induced Degradation and Active Restructuring of LSR Mold Surfaces: Restoring Release Functionality Through LMW PDMS Migration 紫外光诱导的LSR模具表面降解和主动重组:通过LMW PDMS迁移恢复释放功能
IF 3.1 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2026-10-21 Epub Date: 2026-09-28 DOI: 10.1002/app.71557
Wonsun Lee, Kiyoung Kim

This study investigates the loss and restoration of release functionality in service-aged liquid silicone rubber (LSR) molds used for UV-curable epoxy injection. Repeated molding cycles and UV exposure were associated with epoxy-residue accumulation and surface oxidation, which reduced surface hydrophobicity and promoted demolding failure. Conventional water-based cleaning removed loosely bound contaminants and gave only temporary wetting recovery, indicating that cleaning alone did not restore the degraded surface chemistry. We therefore developed a regeneration protocol combining ultrasonic cleaning with baking at 140°C. X-ray photoelectron spectroscopy (XPS) and attenuated-total-reflectance Fourier-transform infrared spectroscopy (ATR-FTIR) showed a decrease in silanol-related signals and recovery of the siloxane-rich surface after the combined treatment, consistent with outward migration of low-molecular-weight polydimethylsiloxane (LMW PDMS). The regenerated molds retained dimensional stability and achieved a > 44% increase in functional lifetime in a pilot-scale UV-epoxy injection process. These findings provide a practical regeneration route for extending the service life of LSR molds while clarifying the coupled roles of contaminant removal and thermally activated surface restructuring.

本研究研究了用于紫外光固化环氧树脂注射的液态硅橡胶(LSR)模具的释放功能的丧失和恢复。重复的成型循环和紫外线暴露与环氧残留物积累和表面氧化有关,这降低了表面疏水性并促进脱模失败。传统的水基清洗去除松散结合的污染物,只能暂时恢复润湿,这表明单纯的清洗并不能恢复已降解的表面化学成分。因此,我们开发了一种再生方案,将超声波清洗与140°C的烘烤相结合。x射线光电子能谱(XPS)和衰减全反射傅里叶变换红外光谱(ATR-FTIR)显示,复合处理后硅醇相关信号减少,富硅氧烷表面恢复,与低分子量聚二甲基硅氧烷(LMW PDMS)向外迁移一致。在中试规模的uv -环氧树脂注射工艺中,再生模具保持了尺寸稳定性,并使功能寿命增加了44%。这些发现为延长LSR模具的使用寿命提供了一条实用的再生途径,同时阐明了污染物去除和热激活表面重组的耦合作用。
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引用次数: 0
Solvent-Resistant Natural Rubber With Humidity-Responsive Functionality Enabled by Layer-by-Layer Self-Assembly for Sensor Applications 耐溶剂天然橡胶,具有湿度响应功能,可逐层自组装用于传感器应用
IF 3.1 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2026-10-21 Epub Date: 2026-09-30 DOI: 10.1002/app.71561
Yuting Huang, Rui Huang, Huimin Yuan, Chengrui Qiu, Shuangquan Liao

We develop a general strategy for preparing solvent-resistant coated natural rubber by constructing a chemically stable polymer layer on the surface of natural rubber via layer-by-layer self-assembly. The coating process entails the sequential layer-by-layer deposition of poly(diallyldimethylammonium) chloride (PDDA) and poly(styrenesulfonate) (PSS) onto the rubber surface, which is subsequently immersed in aqueous solutions of polyvinyl alcohol (PVA). The resulting coating effectively protects natural rubber from organic solvent erosion and dissolution, enabling the coated rubber to remain intact in toluene for over 15 h and in common oils for more than 7 days, without compromising its mechanical properties. By using this solvent-resistant coating, and integrating the humidity-sensitive property of PVA with the excellent mechanical performance of natural rubber, we uniformly deposit the PVA layer in the form of microdroplets onto one side of the curved surface of natural rubber. We fabricate a natural rubber material with humidity-responsive capability and extend its potential applications in the field of humidity sensors.

我们通过一层一层的自组装在天然橡胶表面构建化学稳定的聚合物层,开发了一种制备耐溶剂涂层天然橡胶的一般策略。涂层过程需要将聚二烯基二甲基氯化铵(PDDA)和聚苯乙烯磺酸盐(PSS)逐层逐层沉积在橡胶表面,随后将其浸入聚乙烯醇(PVA)的水溶液中。由此产生的涂层有效地保护天然橡胶免受有机溶剂的侵蚀和溶解,使涂层橡胶在甲苯中保持完整超过15小时,在普通油中保持完整超过7天,而不影响其机械性能。利用这种耐溶剂涂层,结合PVA的湿敏特性和天然橡胶优异的力学性能,我们将PVA层以微滴的形式均匀地沉积在天然橡胶曲面的一侧。我们制造了一种具有湿度响应能力的天然橡胶材料,并扩展了其在湿度传感器领域的潜在应用。
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引用次数: 0
Conductive Network Enhancement in Polybenzoxazine-Based Composite Bipolar Plates via Selective Localization of Carbon Black 通过炭黑的选择性定位增强聚苯并恶嗪基复合双极板的导电网络
IF 3.1 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2026-10-21 Epub Date: 2026-10-04 DOI: 10.1002/app.71558
Yi-Zhang Tong, Zi-Tai Zheng, Fu-Kun Huang, Yu-Kun Yang, Si-Min Huang, Xian-Wu Cao

Polymer-based proton exchange membrane fuel cell (PEMFC) composite bipolar plates (CBPs) typically contain over 80 wt% conductive filler to fulfill the conductivity requirement, limiting PEMFC lightweighting. Utilizing multi-scale conductive fillers to optimize the conduction path is an effective strategy for enhancing filler efficiency. Herein, graphite flakes (GF) are selected as the primary conductive filler, and carbon black (CB) is used as the secondary filler to fabricate polybenzoxazine (PBA)-based CBPs via dry dispersion method. The impact of GF size and content, and GF/CB filler ratio on the conductivity and various service properties of CBPs are investigated. Results demonstrate that smaller-sized GF contributes to superior electrical performance. Owing to the selective distribution of CB within the PBA phase, the conductivity of PBA/GF/CB CBPs is substantially enhanced. At identical total filler loading, the binary PBA/GF CBP fails to meet the DOE target (100 S/cm), whereas the addition of 4 wt% CB brings the conductivity up to the DOE requirement (116.36 S/cm). Notably, the CBP containing 52 wt% GF and 8 wt% CB achieves the highest in-plane conductivity (153.12 S/cm) as well as the maximum power density (673.13 mW/cm2). Moreover, PBA/GF/CB CBPs also exhibit satisfactory flexural strength, thermal conductivity, corrosion resistance, and hydrophobicity.

聚合物基质子交换膜燃料电池(PEMFC)复合双极板(CBPs)通常含有超过80wt %的导电填料,以满足电导率要求,限制了PEMFC的轻量化。利用多尺度导电填料优化导电路径是提高填料效率的有效策略。本文以石墨薄片(GF)为主要导电填料,以炭黑(CB)为次要填料,采用干分散法制备了聚苯并恶嗪(PBA)基CBPs。研究了GF粒径、含量和GF/CB填料比对CBPs电导率和各项使用性能的影响。结果表明,更小尺寸的GF具有更好的电性能。由于CB在PBA相内的选择性分布,PBA/GF/CB CBPs的电导率得到了显著提高。在相同的填料总量下,二元PBA/GF CBP不能满足DOE的目标(100 S/cm),而添加4 wt%的CB则使其电导率达到DOE的要求(116.36 S/cm)。值得注意的是,含有52 wt% GF和8 wt% CB的CBP实现了最高的面内电导率(153.12 S/cm)和最大功率密度(673.13 mW/cm2)。此外,PBA/GF/CB CBPs还表现出令人满意的抗弯强度、导热性、耐腐蚀性和疏水性。
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引用次数: 0
Study on Thermal Properties and Crystallization Behavior of Silica-Modified Polyetheretherketone Composites 二氧化硅改性聚醚醚酮复合材料的热性能及结晶行为研究
IF 3.1 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2026-10-21 Epub Date: 2026-10-08 DOI: 10.1002/app.71556
Shuaishuai Lv, Bo Wang, Yufei Chen, Xinyuan Chen, Ji Chen, Pengfei Wang, Hongjun Ni, Yu Zhu

This study employs KH560 to surface-modify nano-SiO2, which is then melt-blended with PEEK to prepare composites with loadings of 0–7 phr. At 3 phr, the melting temperature rose to 348.5°C, the melting enthalpy reached a maximum of 80.33 J g−1, and the corrected crystallinity remained comparable to that of pure PEEK, while the filler dispersion was the most uniform. Concurrently, the water contact angle decreased from 81.7° to 70.6°–72.8°, thermal conductivity increased substantially, and the dielectric breakdown strength nearly doubled, reaching ≈24.7 kV mm−1 at 5 phr. Compared with the higher loadings commonly reported in the literature, significant multi-property improvements were achieved at only 3–5 phr. These results demonstrate that KH560 surface modification effectively enhances the thermal, crystallization, dielectric, and surface performance of PEEK at low filler contents.

本研究采用KH560对纳米sio2进行表面改性,然后与PEEK熔融共混制备负载量为0-7 phr的复合材料。在3 phr时,熔融温度上升到348.5℃,熔融焓达到最大值80.33 J g−1,修正结晶度与纯PEEK相当,填料分散性最均匀。同时,水接触角从81.7°减小到70.6°~ 72.8°,导热系数大幅提高,介质击穿强度几乎翻倍,在5 phr时达到≈24.7 kV mm−1。与文献中通常报道的更高负载相比,仅在3-5小时内就实现了显著的多属性改善。结果表明,在填料含量较低的情况下,KH560表面改性能有效提高PEEK的热性能、结晶性能、介电性能和表面性能。
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引用次数: 0
Frequency-Dependent Viscoelasticity in Bidisperse Carbon Black-Filled Natural Rubber Nanocomposites: The Critical Role of Heterosized Filler Pairs 双分散炭黑填充天然橡胶纳米复合材料的频率相关粘弹性:异质填料对的关键作用
IF 3.1 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2026-10-21 Epub Date: 2026-09-29 DOI: 10.1002/app.71564
Tianzi Zhang, Fanlin Zeng, Qing Li, Hongyu Guo

The frequency-dependent viscoelasticity of bidisperse carbon black (CB)-filled natural rubber (NR) nanocomposites is investigated using coarse-grained molecular dynamics. The Payne effect becomes more pronounced with increasing frequency and strain amplitude. High frequencies cause extensive nanoparticle (NP) network disruption, reducing loss modulus. Low frequencies enable network reformation and chain friction, increasing loss modulus under large strains. The change in non-bonded interaction energy is dominated by CBCB interactions, with negligible NRNR and CBNR contributions on the normalized per-pair scale. A frequency-driven transition in the dominant CB pair is identified: same-sized pairs dominate at low frequencies, while heterosized pairs prevail at high frequencies. The frequency 2.5 × 10−5 fs−1 marks a characteristic point where the NP network maximally constrains chain mobility. These findings establish that the Payne effect is primarily governed by NP network dynamics, with heterosized CB pairs playing a key role in modulating the frequency-dependent energy dissipation.

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引用次数: 0
Emerging Strategies in Nanomaterial-Engineered Biopolymeric Superabsorbents for Climate-Resilient Water and Nutrient Management 用于气候适应性水和养分管理的纳米材料工程生物聚合物高吸水性新策略
IF 3.1 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2026-10-21 Epub Date: 2026-10-05 DOI: 10.1002/app.71376
Anurag Ajgalle, Chinmaya Mahapatra

This review assesses the benefits of nanoparticle modified superabsorbents such as cellulose nanocrystal-based SAPs, lignin-based and cellulose-based superabsorbent polymers that can absorb up to 825 g/g water due to advanced physicochemical interactions including hydrogen bonds and osmotic pressure-driven swelling. This technology allows optimizing water retention in the soil, reducing the water consumption by 25%, nitrogen losses by 40%–70%, and phosphorus losses by 80%–90%. The improvement of soil water status is achieved due to the formation of a highly cross-linked 3D network of polymers. However, the efficiency of such polymers depends on the effect of the environment on the superabsorbent polymers (SAP) properties, including their salinity and temperature, as their water absorption capacity can decrease under pressure. Natural and semi-synthetic SAPs made from cellulose, starch, chitosan, and other natural polymers are promising materials that can be used as biodegradable alternatives to polyacrylic superabsorbent. However, a critical analysis reveals limitations in synthetic SAPs, such as environmental persistence and microplastic formation, necessitating a shift toward biodegradable alternatives. Nanotechnology integrations, like nanoclay modified SAPs retaining 80% capacity in saline soils (EC = 10 dS/m), promise enhanced performance, but challenges, such as elevated production costs and inconsistent performance across various soil types.

这篇综述评估了纳米颗粒改性的高吸水性聚合物的好处,如纤维素纳米晶体基的sap,木质素基和纤维素基的高吸水性聚合物,由于先进的物理化学相互作用,包括氢键和渗透压驱动的膨胀,可以吸收高达825 g/g的水。该技术可以优化土壤保水,减少25%的耗水量,减少40%-70%的氮损失,减少80%-90%的磷损失。土壤水分状况的改善是由于形成了一个高度交联的聚合物三维网络。然而,这种聚合物的效率取决于环境对高吸水性聚合物(SAP)性能的影响,包括它们的盐度和温度,因为它们的吸水能力在压力下会下降。由纤维素、淀粉、壳聚糖和其他天然聚合物制成的天然和半合成sap是很有前途的材料,可以作为聚丙烯酸高吸水性材料的可生物降解替代品。然而,一项关键的分析揭示了合成sap的局限性,例如环境持久性和微塑料的形成,需要转向可生物降解的替代品。纳米技术集成,如纳米粘土改性的sap在盐渍土壤(EC = 10 dS/m)中保持80%的容量,有望提高性能,但也存在一些挑战,如生产成本增加和不同土壤类型的性能不一致。
{"title":"Emerging Strategies in Nanomaterial-Engineered Biopolymeric Superabsorbents for Climate-Resilient Water and Nutrient Management","authors":"Anurag Ajgalle,&nbsp;Chinmaya Mahapatra","doi":"10.1002/app.71376","DOIUrl":"https://doi.org/10.1002/app.71376","url":null,"abstract":"<p>This review assesses the benefits of nanoparticle modified superabsorbents such as cellulose nanocrystal-based SAPs, lignin-based and cellulose-based superabsorbent polymers that can absorb up to 825 g/g water due to advanced physicochemical interactions including hydrogen bonds and osmotic pressure-driven swelling. This technology allows optimizing water retention in the soil, reducing the water consumption by 25%, nitrogen losses by 40%–70%, and phosphorus losses by 80%–90%. The improvement of soil water status is achieved due to the formation of a highly cross-linked 3D network of polymers. However, the efficiency of such polymers depends on the effect of the environment on the superabsorbent polymers (SAP) properties, including their salinity and temperature, as their water absorption capacity can decrease under pressure. Natural and semi-synthetic SAPs made from cellulose, starch, chitosan, and other natural polymers are promising materials that can be used as biodegradable alternatives to polyacrylic superabsorbent. However, a critical analysis reveals limitations in synthetic SAPs, such as environmental persistence and microplastic formation, necessitating a shift toward biodegradable alternatives. Nanotechnology integrations, like nanoclay modified SAPs retaining 80% capacity in saline soils (EC = 10 dS/m), promise enhanced performance, but challenges, such as elevated production costs and inconsistent performance across various soil types.</p>","PeriodicalId":183,"journal":{"name":"Journal of Applied Polymer Science","volume":"143 45","pages":""},"PeriodicalIF":3.1,"publicationDate":"2026-10-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/app.71376","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149235360","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Single- and Double-Layer Bioadsorptive Membranes for Phenol and Methylene Blue Removal From Synthetic Water 单层和双层生物吸附膜去除合成水中苯酚和亚甲基蓝
IF 3.1 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2026-10-21 Epub Date: 2026-09-29 DOI: 10.1002/app.71562
Sarah Achiche, Dalila Hank, Nadjiba Boulahia, Abdelmalek Chergui

The removal of phenolic pollutants and synthetic dyes from wastewater remains an important environmental challenge due to their potential adverse effects. In this study, single- and double-layer adsorptive composite membranes based on cellulose acetate (CA) and polyvinylpyrrolidone (PVP) are developed by solvent evaporation-induced phase separation (EIPS). Commercial powdered activated carbon (PAC) and two untreated agro-waste bioadsorbents, almond shells (Ash) and date pits (Dp), are incorporated either within the polymer matrix or deposited on the membrane surface. The influence of adsorbent nature and location on phenol and methylene blue removal is investigated. The double-layer membrane D.L(INS(PAC), SRF(Ash)) exhibits the highest methylene blue removal (60%) in both single- and mixed-pollutant systems, while its Ash-containing surface layer reaches 70% removal when tested separately. In comparison, D.L(INS(PAC), SRF(Dp)) achieves approximately 50%, whereas membranes with Ash or Dp incorporated internally and PAC deposited on the surface show less than 30% removal. Phenol removal remains limited (20%–30%) for all membranes. FTIR analysis confirms interactions between CA and the adsorbents, while contact angles of 47.7°–55° indicate hydrophilic surfaces. The results highlight the importance of adsorbent positioning for methylene blue removal.

{"title":"Single- and Double-Layer Bioadsorptive Membranes for Phenol and Methylene Blue Removal From Synthetic Water","authors":"Sarah Achiche,&nbsp;Dalila Hank,&nbsp;Nadjiba Boulahia,&nbsp;Abdelmalek Chergui","doi":"10.1002/app.71562","DOIUrl":"https://doi.org/10.1002/app.71562","url":null,"abstract":"<div>\u0000 \u0000 <p>The removal of phenolic pollutants and synthetic dyes from wastewater remains an important environmental challenge due to their potential adverse effects. In this study, single- and double-layer adsorptive composite membranes based on cellulose acetate (CA) and polyvinylpyrrolidone (PVP) are developed by solvent evaporation-induced phase separation (EIPS). Commercial powdered activated carbon (PAC) and two untreated agro-waste bioadsorbents, almond shells (Ash) and date pits (Dp), are incorporated either within the polymer matrix or deposited on the membrane surface. The influence of adsorbent nature and location on phenol and methylene blue removal is investigated. The double-layer membrane D.L(INS(PAC), SRF(Ash)) exhibits the highest methylene blue removal (60%) in both single- and mixed-pollutant systems, while its Ash-containing surface layer reaches 70% removal when tested separately. In comparison, D.L(INS(PAC), SRF(Dp)) achieves approximately 50%, whereas membranes with Ash or Dp incorporated internally and PAC deposited on the surface show less than 30% removal. Phenol removal remains limited (20%–30%) for all membranes. FTIR analysis confirms interactions between CA and the adsorbents, while contact angles of 47.7°–55° indicate hydrophilic surfaces. The results highlight the importance of adsorbent positioning for methylene blue removal.</p>\u0000 </div>","PeriodicalId":183,"journal":{"name":"Journal of Applied Polymer Science","volume":"143 45","pages":""},"PeriodicalIF":3.1,"publicationDate":"2026-10-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"149235243","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Green Extraction of Lignin From Date Palm (Phoenix dactylifera L.) Seed Waste and Its Integration Into Alginate-Based Films With Improved Moisture Resistance, Antioxidant Capacity, and Surface Hydrophobicity for Food Packaging Applications 枣椰树中木质素的绿色提取种子废料及其在海藻酸盐基薄膜中的整合,具有改善的抗湿性、抗氧化能力和表面疏水性,用于食品包装
IF 3.1 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2026-10-21 Epub Date: 2026-10-09 DOI: 10.1002/app.71568
Yasir Abbas Shah, Talha Shireen Khan, Ahmed Al-Harrasi, Saurabh Bhatia

The aim of the current study was to extract lignin-rich fraction from date palm ( Phoenix dactylifera L.) seeds and evaluate its application as a filler in sodium alginate-based films for food packaging applications. Lignin was isolated through a sonication-assisted mild alkaline hydrolytic process followed by acid precipitation. The isolated lignin was then characterized by using FTIR, XRD, SEM, and DSC analysis. FTIR analysis confirmed the presence of characteristic hydroxyl and aromatic functional groups associated with lignin. XRD analysis showed a low-crystallinity with a broad diffraction region linked with amorphous lignin. SEM analysis showed an irregular and porous morphology. DSC demonstrated favorable thermal behavior. Sodium alginate and lignin films were developed by adding lignin into the sodium alginate matrix at various concentrations by using the solution casting method. The light transmittance and water vapor transmission rate decreased with the addition of lignin. The haze value and antioxidant activity of the films increased with the increase in lignin concentration and improved the light-blocking ability. However, incorporating lignin did not significantly modify the mechanical properties of the films. The sample with the highest lignin concentration showed improved surface hydrophobic properties. These findings suggest that the date seed-derived lignin could be a suitable candidate for food packaging applications.

本研究的目的是从枣椰树种子中提取富含木质素的组分,并评价其作为食品包装用海藻酸钠基薄膜填料的应用。采用超声辅助弱碱性水解-酸沉法制备木质素。然后用FTIR、XRD、SEM和DSC对分离得到的木质素进行了表征。FTIR分析证实木质素存在特征羟基和芳香官能团。XRD分析表明其结晶度低,衍射区宽,与无定形木质素相连。扫描电镜分析显示其形貌不规则且多孔。DSC显示了良好的热行为。采用溶液浇铸法,在海藻酸钠基质中加入不同浓度的木质素,制备了海藻酸钠和木质素薄膜。木材的透光率和水蒸气透过率随木质素的加入而降低。随着木质素浓度的增加,膜的霾值和抗氧化活性增加,阻光能力增强。然而,加入木质素并没有显著改变薄膜的机械性能。木质素浓度最高的样品表面疏水性得到改善。这些发现表明,枣子衍生木质素可能是食品包装应用的合适候选人。
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引用次数: 0
A Naphthalenediimide-Bridged Donor–Acceptor Polymer for Electrochemical Glucose Biosensing 用于葡萄糖电化学生物传感的萘二酰亚胺桥接给受体聚合物
IF 3.1 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2026-10-21 Epub Date: 2026-09-29 DOI: 10.1002/app.71563
Dogan Gurel, Omer Faruk Ozturk, Fatma Baycan

The previously reported naphthalenediimide (NDI)-bridged donor–acceptor type electroactive monomer (NDI-H-T) was synthesized according to the reported procedure and electropolymerized onto a graphite pencil electrode (GPE) surface to obtain a conductive p(NDI-H-T) film. Subsequently, gold nanoparticles (AuNPs) were electrodeposited onto the polymer-coated electrode surface, and glucose oxidase (GOx) was immobilized to fabricate the GPE/p(NDI-H-T)/AuNPs/GOx enzymatic glucose biosensor. The developed biosensor was characterized by cyclic voltammetry (CV) using a three-electrode system with Ag/AgCl, Pt, and modified GPE electrodes. Experimental parameters including electrode type, electropolymerization cycle number, electrolyte pH, and enzyme immobilization time were systematically optimized. Under optimized conditions, the proposed biosensor exhibited a linear response toward glucose within the concentration range of 0.0189–3.21 mM, with limit of detection (LOD) and limit of quantification (LOQ) values of 8.1 × 10−3 mM and 0.0269 mM, respectively. Furthermore, the biosensor demonstrated satisfactory selectivity against common interfering species and was effectively used for glucose detection in pomegranate juice samples. The obtained results demonstrated that the p(NDI-H-T)/AuNPs/GOx biosensor provides an effective platform for electrochemical glucose sensing applications.

将前人报道的萘二酰亚胺(NDI)桥接给受体型电活性单体(NDI- h - t)按照报道的方法合成,并在石墨铅笔电极(GPE)表面电聚合得到导电的p(NDI- h - t)薄膜。随后,将金纳米粒子(AuNPs)电沉积在聚合物包覆的电极表面,固定化葡萄糖氧化酶(GOx)制备GPE/p(NDI-H-T)/AuNPs/GOx酶促葡萄糖生物传感器。利用Ag/AgCl、Pt和改性GPE电极组成的三电极体系对所研制的生物传感器进行了循环伏安法(CV)表征。实验参数包括电极类型、电聚合循环次数、电解质pH、酶固定时间等。在优化条件下,该传感器对葡萄糖的检测浓度在0.0189 ~ 3.21 mM范围内呈线性响应,检测限(LOD)为8.1 × 10−3 mM,定量限(LOQ)为0.0269 mM。此外,该生物传感器对常见干扰物质具有良好的选择性,可有效地用于石榴汁样品中的葡萄糖检测。结果表明,p(NDI-H-T)/AuNPs/GOx生物传感器为电化学葡萄糖传感应用提供了一个有效的平台。
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引用次数: 0
One-Step Synthesis of a Phosphaphenanthrene–Imidazole Phosphorus–Nitrogen Flame Retardant for Epoxy Thermosets: Degradation Pathway and Fire-Safety Mechanism 环氧热固性磷菲-咪唑磷氮阻燃剂的一步合成:降解途径及防火机理
IF 3.1 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2026-10-21 Epub Date: 2026-10-08 DOI: 10.1002/app.71567
Hanzi Gao, Songfeng Xu, Jianglong Hu, Liming Lin, Qiang Ren, Zhengwu Jiang

Epoxy resins (EPs) possess excellent mechanical strength, chemical resistance, and adhesion, yet their inherent flammability limits their use in fire-sensitive applications. Under increasingly stringent safety requirements, developing simple and scalable halogen-free flame retardants remains a significant challenge. In this work, a phosphorus–nitrogen flame retardant, 6-(2-(1H-imidazol-1-yl)ethyl)dibenzo[c,e][1,2]oxaphosphinine 6-oxide (DIM), was synthesized via a one-step nucleophilic addition reaction between 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 1-vinylimidazole (VIM), and subsequently incorporated into epoxy thermosets, either alone or in combination with melamine (MEL). Fourier-transform infrared spectroscopy (FTIR) was used to evaluate the formation of DIM. The thermal degradation, fire performance, char structure, phosphorus retention, and evolved products of the resulting thermosets were investigated using thermogravimetric analysis (TGA), cone calorimetry, scanning electron microscopy (SEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), inductively coupled plasma optical emission spectroscopy (ICP-OES), TGA coupled with Fourier-transform infrared spectroscopy (TG-FTIR), and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). Changes in the characteristic FTIR bands of the PH and vinyl groups, together with the retention of the DOPO and imidazole frameworks, supported the formation of the proposed addition product. Among the investigated formulations, EP/DIM-MEL4 exhibited the greatest improvement in fire performance, with reductions of 31.9% and 36.0% in peak heat release rate and total heat release, respectively, relative to neat EP. Microscopic and spectroscopic analyses indicated the formation of a more expanded, continuous, and structurally ordered protective char. ICP-OES analysis showed that approximately 31.1% of the initial phosphorus was recovered in the solid residue. TG-FTIR and Py-GC/MS further suggested that volatile phosphorus-containing species contributed to gas-phase radical inhibition, whereas nitrogen-containing volatiles derived from the imidazole moiety and MEL contributed to flame-zone dilution. Overall, the improved fire safety of the DIM-containing epoxy thermosets is attributed to the combined effects of gas-phase inhibition and condensed-phase barrier formation. This work provides a simple strategy for developing DOPO-based phosphorus–nitrogen flame-retardant systems for epoxy thermosets.

环氧树脂(EPs)具有优异的机械强度、耐化学性和附着力,但其固有的可燃性限制了其在火灾敏感应用中的应用。在日益严格的安全要求下,开发简单且可扩展的无卤阻燃剂仍然是一个重大挑战。在这项工作中,通过9,10-二氢-9-氧-10-磷菲-10-氧化物(DOPO)和1-乙烯咪唑(VIM)之间的一步亲核加成反应,合成了一种磷氮阻燃剂6-(2-(1h -咪唑-1-酰基)乙基)二苯并[c,e][1,2]氧磷膦6-氧化物(DIM),随后将其单独或与三聚氰胺(MEL)联合掺入环氧热固性树脂中。采用傅里叶变换红外光谱(FTIR)评价了DIM的形成过程,并利用热重分析(TGA)、锥量热法、扫描电镜(SEM)、拉曼光谱(Raman)、x射线光电子能谱(XPS)、电感耦合等离子体发射光谱(ICP-OES)、TGA结合傅里叶变换红外光谱(TG-FTIR)和热解-气相色谱/质谱(Py-GC/MS)。P - H和乙烯基的特征FTIR波段的变化,以及DOPO和咪唑框架的保留,支持了所提出的加成产物的形成。在所研究的配方中,EP/DIM-MEL4的防火性能改善最大,峰值放热率和总放热率分别比纯EP降低31.9%和36.0%。显微和光谱分析表明,形成了一个更大的、连续的、结构有序的保护炭。ICP-OES分析表明,固体残渣中回收了约31.1%的初始磷。TG-FTIR和Py-GC/MS进一步表明,挥发性含磷物质有助于气相自由基抑制,而来自咪唑部分和MEL的含氮挥发性物质有助于火焰区稀释。总的来说,含dim的环氧热固性树脂的防火安全性的提高是由于气相抑制和凝聚相屏障形成的共同作用。这项工作为开发基于dopo的环氧热固性磷氮阻燃体系提供了一种简单的策略。
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引用次数: 0
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Journal of Applied Polymer Science
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