Synthesis and Characterization of Triblock Terpolymers with three Potentially Crystallisable Blocks: Polyethylene‐<i>b</i>‐poly(ethylene oxide)‐<i>b</i>‐poly(ε‐caprolactone)

Vivas, M.; Contreras, Jesús M; López‐Carrasquero, Francisco; Lorenzo, Arnaldo T.; Arnal, María L.; Balsamo, Vittoria; Müller, Alejandro J.; Laredo, E.; Schmalz, Holger; Abetz, Volker

doi:10.1002/masy.200690110

Cited by 19 publications

(23 citation statements)

References 29 publications

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“…Ohno and coworkers investigated dicationic PEG‐based molten salts bearing imidazolium cations as ion conducting materials 40. Basically, modified PEO‐polymers can be prepared via anionic polymerization, based on methods developed earlier (for relevant citaitons see refs 41–44…”

Section: Introductionmentioning

confidence: 99%

Ethylene glycol‐based ionic liquids via azide/alkyne click chemistry

Zare

Mahrova

Tojo

et al. 2012

J. Polym. Sci. A Polym. Chem.

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A facile synthetic route for the preparation of dicationic ethylene glycol based-ionic liquids (ILs) via the azide/ alkyne ''click'' reaction is presented. The copper(I) catalyzed, microwave-assisted azide/alkyne ''click'' reaction between diazido-ethylene glycols and the corresponding alkyne containing IL-head group enables a simple preparation of different sets of poly(ethylene glycol)-based ILs. Beside tetra-and hexa(ethylene glycol)-based ILs, also oligomeric (M n ¼ 400 g/mol) and polymeric ILs (M n up to 1550 g/mol) could be prepared in good yield and with full conversion of the ionic head group.The prepared ILs were extensively characterized via NMR spectroscopy and ESI-time-of-flight (TOF) mass spectroscopy, revealing the formation of multiply charged ions in the negative mode. Thermal stability proved to be exceptionally high (up to 300 C) together with low glass-transition temperatures.

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Section: Introductionmentioning

confidence: 99%

Ethylene glycol‐based ionic liquids via azide/alkyne click chemistry

Zare

Mahrova

Tojo

et al. 2012

J. Polym. Sci. A Polym. Chem.

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“…Some of us, synthesized a PE-b-PEO-b-PCL triblock terpolymer in which the central block was not able to crystallize, mainly due to topological restrictions imposed by the previously crystallized PE and PCL blocks. 11 Later, Sun et al reported the synthesis of triblock and pentablock terpolymers composed of PCL, PLLA and PEG. 12 The authors reported that the terpolymers were crystalline from DSC analysis and WAXS experiments performed at room temperature.…”

Section: Please Do Not Adjust Marginsmentioning

confidence: 99%

Sequential crystallization and morphology of triple crystalline biodegradable PEO-b-PCL-b-PLLA triblock terpolymers

et al. 2016

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The sequential crystallization of poly(ethylene oxide)-b-poly(e-caprolactone)-b-poly(L-lactide) (PEO-b-PCL-b-PLLA) triblock terpolymers, in which the three blocks are able to crystallize separately and sequentially from the melt, is presented. Two terpolymers with identical PEO and PCL block lengths and two different PLLA block lengths were prepared, thus the effect of increasing PLLA content on the crystallization behavior and morphology was evaluated. Wide angle X-Ray scattering (WAXS) experiments performed on cooling from the melt confirmed the triple crystalline nature of these terpolymers and revealed that they crystallize in sequence: the PLLA block crystallizes first, then the PCL block, and finally the PEO block. Differential scanning calorimetry (DSC) analysis further demonstrated that the three blocks can crystallize from the melt when a low cooling rate is employed. The crystallization process takes place from a homogenous melt as indicated by small angle X-Ray scattering (SAXS) experiments. The crystallization and melting enthalpies and temperatures of both PEO and PCL blocks decrease as PLLA content in the terpolymer increases. Polarized light optical microscopy (PLOM) demonstrated that the PLLA block templates the morphology of the terpolymer, as it forms spherulites upon cooling from the melt. The subsequent crystallization of PCL and PEO blocks occurs inside the interlamellar regions of the previously formed PLLA block spherulites. In this way, unique triple crystalline mixed spherulitic superstructures have been observed for the first time. As the PLLA content in the terpolymer is reduced the superstructural morphology changes from spherulites to a more axialitic-like structure.

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“…The second type is polyethylene‐ block ‐poly(ethylene oxide)‐ block ‐poly( ε ‐caprolactone) (PE‐ b ‐PEO‐ b ‐PCL), which was reported by Abetz and his coworker in 2006 . To the best of our knowledge, this is the only example of tricrystalline triblock terpolymer containing PE block in the chain due to the challenging polymerization steps.…”

Section: Introductionmentioning

confidence: 85%

A new tricrystalline triblock terpolymer by combining polyhomologation and ring‐opening polymerization. synthesis and thermal properties

Ladelta

Ζάψας

Gnanou

et al. 2019

J. Polym. Sci. Part A: Polym. Chem.

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New tricrystalline triblock terpolymers, polyethylene‐block‐poly(ε‐caprolactone)‐block‐poly(L‐lactide) (PE‐b‐PCL‐b‐PLLA), were synthesized by ROP of ε‐caprolactone (CL) and L‐lactide (LLA) from linear ω‐hydroxyl polyethylene (PE‐OH) macroinitiators. The linear PE‐OH macroinitiators were prepared by C1 polymerization of methylsulfoxonium methylide (polyhomologation). Tin(II) 2‐ethylhexanoate was used as the catalyst for the sequential ROP of CL and LLA in one‐pot polymerization at 85 °C in toluene (PE‐OH macroinitiators are soluble in toluene at 80 °C). 1H NMR spectra confirmed the formation of PE‐b‐PCL‐b‐PLLA triblock terpolymers through the appearance of the characteristic proton peaks of each block. GPC traces showed the increase in the number average molecular weight from PE‐OH macroinitiator to PE‐b‐PCL, and PE‐b‐PCL‐b‐PLLA corroborating the successful synthesis. The existence of three crystalline blocks was proved by DSC and XRD spectroscopy. © 2019 The Authors. Journal of Polymer Science Part A: Polymer Chemistry published by Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019, 57, 2450–2456

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Synthesis and Characterization of Triblock Terpolymers with three Potentially Crystallisable Blocks: Polyethylene‐b‐poly(ethylene oxide)‐b‐poly(ε‐caprolactone)

Cited by 19 publications

References 29 publications

Ethylene glycol‐based ionic liquids via azide/alkyne click chemistry

Ethylene glycol‐based ionic liquids via azide/alkyne click chemistry

Sequential crystallization and morphology of triple crystalline biodegradable PEO-b-PCL-b-PLLA triblock terpolymers

A new tricrystalline triblock terpolymer by combining polyhomologation and ring‐opening polymerization. synthesis and thermal properties

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