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Photo‐induced polymerization of styrene‐maleic acid copolymers for the extraction of membrane proteins 用于提取膜蛋白的苯乙烯-马来酸共聚物的光诱导聚合反应
IF 3.4 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2024-08-31 DOI: 10.1002/pol.20240295
Valentin Monjal, Pierre Guillet, Alexis Moreno, Marine Soulié, Grégory Durand
We report herein the photoinduced electron/energy transfer–reversible addition‐fragmentation chain transfer (PET‐RAFT) polymerization of styrene‐maleic anhydride (SMAnh) using the photocatalyst, zinc tetraphenylporphirine, under a white cool LED light. PET‐RAFT is an easy and convenient polymerization method that does not require deoxygenation unlike other radical polymerizations. Various parameters, for example, the amount of styrene in the feed or the solvent, and their influence on the polymerization were studied. After hydrolysis of the anhydride moieties, the resulting styrene‐maleic acid (SMA) copolymers obtained by PET‐RAFT copolymerization were evaluated for their solubilization efficiency of three different membrane proteins, BmrA and AcrB, overexpressed in Escherichia coli, and A2AR, expressed in insect cells (Sf9). The different copolymers provided similar solubilization rates to the commercially available SMA; however, a highly improved migration behavior on sodium dodecyl‐sulfate polyacrylamide gel electrophoresis was observed which could, facilitate downstream analyses. Overall, we demonstrated that PET‐RAFT is a versatile oxygen tolerant polymerization technique to yield SMA, a suitable polymer for biochemical applications.
我们在此报告使用光催化剂四苯基卟吩锌在白色冷光 LED 灯下对苯乙烯-马来酸酐(SMAnh)进行光诱导电子/能量转移-可逆加成-断裂链转移(PET-RAFT)聚合的情况。PET-RAFT 是一种简单方便的聚合方法,与其他自由基聚合不同,它不需要脱氧。研究了各种参数,例如进料或溶剂中苯乙烯的含量及其对聚合的影响。在水解酸酐分子后,评估了 PET-RAFT 共聚法得到的苯乙烯-马来酸(SMA)共聚物对三种不同膜蛋白(在大肠杆菌中过度表达的 BmrA 和 AcrB 以及在昆虫细胞(Sf9)中表达的 A2AR)的溶解效率。不同共聚物的增溶率与市售的 SMA 相似,但在十二烷基硫酸钠聚丙烯酰胺凝胶电泳上的迁移行为有很大改善,这有助于下游分析。总之,我们证明 PET-RAFT 是一种多功能的耐氧聚合技术,可生成 SMA,这是一种适用于生化应用的聚合物。
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引用次数: 0
Isotactic polypropylene produced by rac/meso mixtures of hafnocene complexes through selective rac activation rac/meso混合物通过选择性rac活化生产铪络合物的同素异形聚丙烯
IF 3.4 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2024-08-30 DOI: 10.1002/pol.20240610
Tim M. Lenz, Bernhard Rieger
Meso isomers of indenyl‐based group IV hafnocene complexes produce atactic polypropylene (aPP) and thus, have to be tediously separated from their racemic analogs for the production of isotactic polypropylene (iPP). Herein, we report a facile activation protocol to selectively convert only the racemic precatalysts into catalytically active species when isomeric precatalyst mixtures are employed. At the same time, the meso isomers are deactivated, thus yielding no polypropylene at all. The macromolecular characteristics of iPP, that is, melting transition, molecular weight, and tacticity, obtained by this protocol were analog to the characteristics of iPP produced by the corresponding pure racemic isomers, as proven for different complexes, isomeric ratios, and polymerization conditions. Nuclear magnetic resonance experiments revealed that the employed precatalyst activation protocol – that is, alkylation with triisobutylaluminum and subsequent generation of a free coordination site with [Ph3C][B(C6F5)4] – led to catalytically active, binuclear hydride‐bridged racemic species but inactive meso resting states. The separation of both precatalyst isomers, which was believed to be crucial to obtaining pure iPP since the 1980s, rendered hafnocene syntheses unnecessarily laborious and can be circumvented by the activation protocol established in this work.
茚基第 IV 组二茂铪络合物的中位异构体可生成无规聚丙烯 (aPP),因此在生产异方性聚丙烯 (iPP) 时必须将其与外消旋类似物进行繁琐的分离。在此,我们报告了一种简便的活化方案,当使用异构前催化剂混合物时,只需将外消旋前催化剂选择性地转化为催化活性物质。与此同时,中间异构体也会失活,因此根本不会产生聚丙烯。在不同的配合物、异构体比例和聚合条件下,该方案得到的 iPP 的大分子特性,即熔融转变、分子量和触变性,与相应的纯外消旋异构体生成的 iPP 的特性类似。核磁共振实验显示,所采用的前催化剂活化方案--即用三异丁基铝进行烷基化,然后用 [Ph3C][B(C6F5)4] 生成一个自由配位位点--可产生具有催化活性的双核氢桥外消旋物,但无活性的中间静止态。自 20 世纪 80 年代以来,人们一直认为分离这两种前催化剂异构体是获得纯 iPP 的关键所在。
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引用次数: 0
Optimization of fiber content, length and its effect on overall properties of Licuala grandis leaf stalk fiber/polyester reinforced bio‐composites 优化叶柄纤维/聚酯增强生物复合材料的纤维含量、长度及其对总体性能的影响
IF 3.4 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2024-08-30 DOI: 10.1002/pol.20240526
Siga Selvin Deva Kumar, Rajesh Resselian, Dev Anand Manoharan, Yesudhasan Thooyavan, Joseph Selvi Binoj
Despite their better mechanical qualities, plant fibers are now appreciated enough to be employed as an additional component in composite manufacture rather than synthetic materials. Industries are making efforts to preserve nature's ecological equilibrium in order to avoid catastrophic natural disasters. This study investigated thermal, mechanical, morphological, and moisture‐capture capabilities of Licuala grandis leaf stalk fibers (LGLSFs) reinforced in an unsaturated polyester resin (UPR) matrix biocomposite. Biocomposites were fabricated by compression molding technology, with different weight ratios and sizes. The biocomposite containing 30 wt.% and 5 mm length LGLSF had best mechanical properties, with equal impact (5.4 J/cm2), hardness (70.4 HRRW), flexural (58 MPa), and tensile (64.9 MPa) values. Furthermore, prolonging LGLSF reinforcement to 15 mm increased the bio‐composite specimen's tensile, flexural, hardness, and impact characteristics by 9.09%, 9.65%, 14.8%, and 6.25%, respectively. The Fourier transform infrared (FTIR), scanning electron microscopy (SEM), and X‐ray diffraction (XRD) spectra were analyzed to determine the bio‐composite's feasibility for commercial use. The bio‐composite specimen is ideal for usage in vehicle and aviation upholstery due to its sufficient hydrophobicity, lowered density, and heat resistance up to 236 °C, which are accomplished through a sufficient weight ratio of LGLSF and UPR, as well as LGLSF dimensions.
尽管植物纤维具有更好的机械性能,但现在它们已受到足够的重视,在复合材料生产中被用作替代合成材料的另一种成分。各行各业都在努力保护大自然的生态平衡,以避免灾难性的自然灾害。本研究调查了在不饱和聚酯树脂(UPR)基质生物复合材料中增强的Licuala grandis叶柄纤维(LGLSFs)的热、机械、形态和吸湿能力。生物复合材料通过压缩成型技术制成,具有不同的重量比和尺寸。含有 30 重量比和 5 毫米长 LGLSF 的生物复合材料具有最佳的机械性能,其冲击(5.4 J/cm2)、硬度(70.4 HRRW)、弯曲(58 MPa)和拉伸(64.9 MPa)值相同。此外,将 LGLSF 增强层延长至 15 毫米后,生物复合材料试样的拉伸、弯曲、硬度和冲击特性分别提高了 9.09%、9.65%、14.8% 和 6.25%。通过分析傅立叶变换红外光谱(FTIR)、扫描电子显微镜(SEM)和 X 射线衍射光谱(XRD),确定了生物复合材料的商业用途可行性。生物复合材料试样具有足够的疏水性、较低的密度和高达 236 ℃ 的耐热性,因此非常适合用于汽车和航空内饰,而这些都是通过 LGLSF 和 UPR 足够的重量比以及 LGLSF 的尺寸实现的。
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引用次数: 0
A study of poly(pentaerythritol triallyl ether) embolic granules with medium swelling properties using for vascular embolizations against hepatocellar carcinoma 具有中等膨胀特性的聚季戊四醇三烯丙基醚栓塞颗粒用于肝细胞癌血管栓塞的研究
IF 3.4 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2024-08-30 DOI: 10.1002/pol.20240023
Lingyin Lin, Runxing Lin, Xufeng Li, Yanfang Zhou, Xiaotian Zhao, Wanqiu Huang, Qiuxia Li, Yugang Huang, He Wang, Guodong Ye
Interventional embolotherapy is widely used in clinical treatment of conservative liver cancer. This method has many advantages, such as good targeting, mild trauma, and low complications. The operation of transcatheter arterial embolization is to inject embolic microspheres into the arterial blood vessels of diseased organs, so as to occlude them and interrupt the blood supply, thus achieving the therapeutic purpose. However, there are still some deficiencies in clinical materials, for example catheter obstruction or vascular regeneration. In this study, pentaerythritol triallyl ether (APE) and its esterified product APEAA were used to prepare new polymeric amorphous embolic granules (PAPE and PAPEAA). The purpose is to overcome the excessive swelling problems of traditional polyvinyl alcohol granules (PVA). We verified that PAPE and PAPEAA were quickly and efficiently polymerized by photo‐driven radical‐mediated [3 + 2] cyclopolymerization mechanism (PRMC). RT‐FTIR was used to explore the best route of photopolymerization initiated by four photoinitiators. Four physical properties experiments all prove that the particle has good physical properties. In vivo animal experiments, it is confirmed that the particles can achieve the expected effect and have good biological safety. The results show that the amorphous granules can meet the requirements of clinical injection and can be used as a new embolic material.
介入栓塞疗法广泛应用于保守性肝癌的临床治疗。该方法具有靶向性好、创伤小、并发症少等诸多优点。经导管动脉栓塞术的操作方法是将栓塞微球注入病变器官的动脉血管中,使其闭塞,中断血液供应,从而达到治疗目的。但在临床材料上仍存在一些不足,如导管阻塞或血管再生等。本研究利用季戊四醇三烯丙基醚(APE)及其酯化产物 APEAA 制备了新型高分子无定形栓塞颗粒(PAPE 和 PAPEAA)。目的是克服传统聚乙烯醇颗粒(PVA)的过度膨胀问题。我们验证了 PAPE 和 PAPEAA 通过光驱动自由基介导的 [3 + 2] 环聚合机制(PRMC)快速高效地聚合。利用 RT-FTIR 技术探索了四种光引发剂引发光聚合的最佳途径。四项物理性质实验均证明颗粒具有良好的物理性质。在体内动物实验中,证实颗粒能达到预期效果,并具有良好的生物安全性。结果表明,无定形颗粒能满足临床注射的要求,可用作新型栓塞材料。
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引用次数: 0
Physical aging of a glassy polymer in cultural heritage conservation 文化遗产保护中玻璃聚合物的物理老化
IF 3.4 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2024-08-27 DOI: 10.1002/pol.20240449
Yahya Rharbi, Frederic Hugenell
Artworks, particularly easel paintings, are multi‐component materials intended to last indefinitely. The protective coatings applied to these artworks often consist of amorphous glass‐like polymers, which undergo slow physical aging and structural recovery below their glass transition temperature. This process alters key physical properties such as mechanical strength, optical clarity, and thermal stability over extended periods. This study investigates the time‐dependent evolution of these properties in Laropal A81, a widely used synthetic resin for cultural heritage conservation, particularly as a replacement for ancient varnishes. The investigation involves characterization of enthalpy recovery via differential scanning calorimetry, refractive index evolution via refractometry, and creep compliance evolution via rheological measurements. The aging behavior of Laropal A81 is further analyzed using the Kohlrausch–Williams–Watts function and the Tool–Narayanaswamy–Moynihan model, enabling the quantification of critical dynamic parameters such as activation energy, nonlinearity, partition coefficients, and non‐exponentiality. The gained insights into the long‐term behavior of this coating's properties can be valuable for improving preservation and restoration strategies for cultural heritage.
艺术品,尤其是架上绘画,是一种旨在无限期保存的多组分材料。这些艺术品的保护涂层通常由无定形的玻璃状聚合物组成,在低于玻璃转化温度时会发生缓慢的物理老化和结构恢复。这一过程会长期改变关键的物理特性,如机械强度、光学清晰度和热稳定性。Laropal A81 是一种广泛用于文化遗产保护的合成树脂,尤其是作为古代清漆的替代品。调查包括通过差示扫描量热法对焓恢复进行表征,通过折射仪对折射率的演变进行表征,以及通过流变学测量对蠕变顺应性的演变进行表征。利用 Kohlrausch-Williams-Watts 函数和 Tool-Narayanaswamy-Moynihan 模型对 Laropal A81 的老化行为进行了进一步分析,从而对活化能、非线性、分配系数和非幂性等关键动态参数进行了量化。对这种涂层特性长期行为的深入了解对于改进文化遗产的保护和修复策略非常有价值。
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引用次数: 0
Recyclable, healable, and stretchable thermoset shape memory polythiourethane/carbon nanotube composite with segregated conductive structure for strain sensing 可回收、可愈合、可拉伸的热固性形状记忆聚硫乙烷/碳纳米管复合材料,具有用于应变传感的分离式导电结构
IF 3.9 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2024-08-27 DOI: 10.1002/pol.20240412
Fangfang Hu, Chenxin Yao, Miaoming Huang, Suqin He, Hao Liu, Wentao Liu, Chengshen Zhu, Wanlin Xu

Segregated conductive polymer composites (CPCs) show high conductivity at low loading of filler. However, the weak interactions between fillers and polymer matrix may destroy the mechanical property of the segregated CPCs. Moreover, even with the introduction of dynamic bonds in thermoset polymers, the preparation of thermosetting CPCs remains a big challenge, as most crosslinked polymers should be ground into granules or crushed into powder with liquid nitrogen before mixing with fillers. Herein, the dynamic crosslinked polythiourethane microspheres (PTUM) are designed and synthesized. Then, a special mixing method (the mixing temperature is higher than melting temperature of soft segments of PTUM) is used to make the carbon nanotubes (CNTs) adhering closely to the surface of the crosslinked PTUM, promoting the formation of compacted conductive network. The CNT-3%/PTUM shows the electrical conductivity of 21.9 S/m and an elongation at break of 472%. Additionally, the CNT/PTUM composites exhibit good self-healing property, reprocessability, and close-loop recycling property. The construction of dynamic crosslinked microspheres and compacted segregated conductive network in this work supplies a new approach to prepare thermoset CPCs with simultaneous high electrical conductivity and mechanical property, which is expected to be applied to wearable strain sensors.

离析导电聚合物复合材料(CPCs)在填料含量较低的情况下具有较高的导电性。然而,填料与聚合物基体之间的微弱相互作用可能会破坏离析导电聚合物复合材料的机械性能。此外,即使在热固性聚合物中引入了动态键,热固性 CPC 的制备仍然是一个巨大的挑战,因为大多数交联聚合物在与填料混合之前都要先用液氮研磨成颗粒或粉碎成粉末。本文设计并合成了动态交联聚氨酯微球(PTUM)。然后,采用特殊的混合方法(混合温度高于 PTUM 软段的熔化温度)使碳纳米管(CNTs)紧密附着在交联 PTUM 的表面,促进形成致密的导电网络。CNT-3%/PTUM 的导电率为 21.9 S/m,断裂伸长率为 472%。此外,CNT/PTUM 复合材料还具有良好的自愈性、可再加工性和闭环回收性。本研究中的动态交联微球和致密分离导电网络的构建为制备同时具有高导电性和机械性能的热固性 CPC 提供了一种新方法,有望应用于可穿戴应变传感器。
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引用次数: 0
A review on thermally induced phase separation technology in the fabrication of microporous polymer membrane devices for sustained-repellent delivery: Crystallization and morphological studies 综述热诱导相分离技术在制造微孔聚合物膜器件中的应用,以实现持续驱虫:结晶和形态研究
IF 3.4 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2024-08-27 DOI: 10.1002/pol.20240232
António Benjamim Mapossa, Robert Kimutai Tewo, Suprakas Sinha Ray, Washington Mhike, Uttandaraman Sundararaj
This article reports recent advances in thermally induced phase separation technology in fabricating microporous scaffold polymeric membranes as devices suitable for the controlled release of insect repellent. The key aspects, such as the crystallization behavior and morphological study of the polymeric membrane-based repellent, were reported and discussed. Studies demonstrated that trapping of such repellents into microporous polymeric materials can be achieved by spinodal decomposition of the polymer/liquid repellent system. Usually, solubility is enhanced at elevated temperatures. Rapid cooling of such solution below the UCST leads to the formation of cocontinuous phase structures by decomposition. The polymer then forms an open-cell structure with the repellent trapped inside. Approaches to forming such an open-cell polymer structure containing mosquito repellent were successfully performed and confirmed with the SEM and POM techniques. It showed the structure of a polymer and liquid repellent prepared by spinodal decomposition, providing proof that thermally induced spinodal decomposition is a route to trap liquid mosquito repellent into a microporous polymer matrix. Additionally, the effects of polymer type, repellent nature, cooling conditions, and fillers on the morphology and performance of TIPS membranes are also discussed. Finally, challenges in developing microporous polymeric membrane-based repellent using TIPS technology are addressed.
本文报告了热诱导相分离技术在制造微孔支架聚合物膜作为驱虫剂控释装置方面的最新进展。文章对基于聚合物膜的驱虫剂的结晶行为和形态研究等关键方面进行了报告和讨论。研究表明,通过聚合物/液体驱虫剂体系的旋光分解,可将此类驱虫剂捕集到微孔聚合物材料中。通常,溶解度在温度升高时会增强。将这种溶液快速冷却到 UCST 以下,可通过分解形成共连续相结构。然后,聚合物会形成一个开孔结构,并将斥水剂困在其中。成功形成这种含有驱蚊剂的开孔聚合物结构的方法,已通过 SEM 和 POM 技术得到证实。它显示了通过旋光分解制备的聚合物和液态驱蚊剂的结构,证明了热诱导旋光分解是将液态驱蚊剂捕获到微孔聚合物基质中的一种途径。此外,还讨论了聚合物类型、驱蚊剂性质、冷却条件和填料对 TIPS 膜的形态和性能的影响。最后,还讨论了利用 TIPS 技术开发基于微孔聚合物膜的驱蚊剂所面临的挑战。
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引用次数: 0
Anionic polyaddition of 1,1-diphenylethylene derivatives for novel hydrocarbon polymers 1,1-二苯基乙烯衍生物的阴离子多加成,用于制造新型碳氢化合物聚合物
IF 3.9 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2024-08-24 DOI: 10.1002/pol.20240482
Honoka Matsumoto, Daisuke Tanioka, Kaoru Adachi

The anionic polyaddition of methyl-substituted 1,1-diphenylethylene derivatives, catalyzed by lithium diisopropylamide, was examined. Polymerization of the monomer was conducted at 50°C in THF with the addition of diisopropylamine. NMR and MALDI-TOF-MS analyses of the obtained polymer indicate that polymerization proceeded via a polyaddition reaction, in other words, repetition of the lithium amide-induced metalation reaction of the monomer at the methyl group and the subsequent nucleophilic addition reaction of the corresponding benzyllithium with the vinyl group in the monomer. On the other hand, the unsubstituted diphenylethylene monomer could not be polymerized by the same reaction condition. Consequently, the resulting polymer was indeed obtained by an anionic polyaddition mechanism. In conclusion, a novel hydrocarbon polymer containing a phenyl group in the main chain of the repeating unit was successfully obtained from a methyl-substituted 1,1-diphenylethylene monomer.

在二异丙基酰胺锂的催化下,研究了甲基取代的 1,1-二苯基乙烷衍生物的阴离子加成反应。单体的聚合在 50°C 的 THF 中进行,同时加入二异丙基胺。对得到的聚合物进行的核磁共振和 MALDI-TOF-MS 分析表明,聚合反应是通过加成反应进行的,换句话说,就是重复进行锂酰胺诱导的单体甲基金属化反应,以及随后相应的苄基锂与单体中乙烯基的亲核加成反应。另一方面,未取代的二苯基乙烯单体无法在相同的反应条件下聚合。因此,所得到的聚合物确实是通过阴离子加成机理获得的。总之,我们成功地从甲基取代的 1,1-二苯基乙烯单体中获得了一种新型烃聚合物,这种聚合物的重复单元主链中含有一个苯基。
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引用次数: 0
Effect of polymeric spherulite coatings on optical properties of chiral nematic cellulose nanocrystal films 聚合物球粒涂层对手性向列纤维素纳米晶薄膜光学特性的影响
IF 3.9 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2024-08-24 DOI: 10.1002/pol.20240307
Chhavi Verma, Monika Chhajed, E. Priya, Pradip K. Maji

Cellulose nanocrystals (CNCs) have received an abundance of attention because of their distinctive chiral nematic structure and exceptional optical characteristics. However, the use of free-standing films is constrained by the inherent stiffness and brittleness. In this work, CNC films with robust mechanical properties are prepared by simply coating them with polymeric spherulites. Maleic anhydride-grafted polypropylene (PP-g-MA) is used to coat CNC films. The optical properties of coated films were also analyzed using polarized optical microscope. It is observed that the circular extinction patterns for the coated CNC film were created by the radial symmetry of banded spherulites, which were responsible for the perception of the optical transmission bands of the CNC film. Interfacial anchoring plays a crucial role in enhancing the overall performance and properties of the composite system. The future development of numerous portable functional components needing improved optical, mechanical, and thermal qualities of CNC films is made possible by this protective coating approach.

纤维素纳米晶体(CNC)因其独特的手性向列结构和优异的光学特性而受到广泛关注。然而,独立薄膜的使用受到其固有硬度和脆性的限制。在这项工作中,通过简单地在数控薄膜上涂覆聚合物球形颗粒,制备出了具有坚固机械性能的数控薄膜。马来酸酐接枝聚丙烯(PP-g-MA)用于涂覆 CNC 薄膜。此外,还使用偏光光学显微镜分析了涂层薄膜的光学特性。结果表明,涂覆的 CNC 薄膜的圆形消光图案是由带状球形微粒的径向对称性产生的,它们是 CNC 薄膜光学透射带的感知原因。界面锚定对提高复合材料系统的整体性能和特性起着至关重要的作用。通过这种保护性涂层方法,未来可以开发出许多便携式功能部件,这些部件需要改进 CNC 薄膜的光学、机械和热学质量。
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引用次数: 0
Preparative temperature rising elution fractionation of polyolefin elastomer and its chain microstructure 聚烯烃弹性体的制备升温洗脱分馏及其链微结构
IF 3.9 3区 化学 Q2 POLYMER SCIENCE Pub Date : 2024-08-24 DOI: 10.1002/pol.20240345
Peng Liu, Shuang He, Tao Yang, Zhenkang Zhang, Yanhu Xue

Polyolefin elastomer (POE) has very weak crystalline ability, consequently, applying the conventional preparative temperature-rising elution fractionation (P-TREF) to separate is challenging. Here, a unique, home-built P-TREF apparatus with an extensive range of temperatures from −80°C to 150°C is applied to first fractionate POE depending on its crystallizability. The main fractions are eluted at 0°C, 8°C, 15°C, 20°C, 25°C, 30°C, and 35°C. The corresponding weight percentages of fractions are 8.31, 13.38, 15.59, 12.05, 13.39, 17.30, and 10.53 wt%, respectively. The chain structures of fractions are further analyzed by high-temperature gel permeation chromatography (HT-GPC), 13C-nuclear magnetic resonance spectroscopy (13C-NMR), differential scanning calorimetry (DSC), and successive self-nucleation and annealing (SSA). The crystallinity of the fraction grows continually as the elution temperature rises. The 1-octene comonomer concentrations within the fractions decreases from 13.8 to 7.9 mol% when the elution temperature rises from −10°C to 40°C. These findings enable for the detailed recognition of the chain microstructure of POE resin and the extension of the TREF approach to POE resins. This lays the groundwork for fundamental studies and practical uses in industry.

聚烯烃弹性体(POE)的结晶能力非常弱,因此采用传统的制备升温洗脱分馏(P-TREF)方法进行分离具有挑战性。在这里,我们采用了一种独特的自制 P-TREF 设备,该设备的温度范围从 -80°C 到 150°C,可根据 POE 的结晶性首先对其进行分馏。主要馏分在 0°C、8°C、15°C、20°C、25°C、30°C 和 35°C 下洗脱。馏分的相应重量百分比分别为 8.31、13.38、15.59、12.05、13.39、17.30 和 10.53 wt%。通过高温凝胶渗透色谱法(HT-GPC)、13C-核磁共振谱(13C-NMR)、差示扫描量热法(DSC)和连续自核退火法(SSA)进一步分析了馏分的链结构。随着洗脱温度的升高,馏分的结晶度不断增加。当洗脱温度从 -10°C 升至 40°C 时,馏分中的 1-辛烯单体浓度从 13.8 摩尔%降至 7.9 摩尔%。这些发现有助于详细了解 POE 树脂的链微观结构,并将 TREF 方法推广到 POE 树脂中。这为基础研究和工业实际应用奠定了基础。
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引用次数: 0
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