Tetracrystalline Tetrablock Quarterpolymers: Four Different Crystallites under the Same Roof

Multicrystalline block polymers having three or more crystalline segments are essential materials for the advancement of physics in the field of crystallinity. The challenging synthesis of multicrystalline polymers has resulted in only a limited number of tricrystalline terpolymers having been repor...

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Bibliographic Details
Published in:Angewandte Chemie International Edition 2019-11, Vol.58 (45), p.16267-16274
Main Authors: Ladelta, Viko, Zapsas, George, Abou‐hamad, Edy, Gnanou, Yves, Hadjichristidis, Nikos
Format: Article
Language:English
Subjects:
Calorimetry
catalyst switch
Catalysts
Chemical synthesis
Crystal structure
Crystallinity
Crystallites
Crystals
Differential scanning calorimetry
Domains
Ethylene oxide
Magnetic resonance spectroscopy
multicrystalline polymers
NMR
NMR spectroscopy
Nuclear magnetic resonance
Polyethylene
Polyethylene oxide
Polyethylenes
polyhomologation
Polylactic acid
Polymerization
Polymers
Ring opening polymerization
Spectroscopy
Spectrum analysis
Terpolymers
tetrablock quarterpolymers
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Summary:Multicrystalline block polymers having three or more crystalline segments are essential materials for the advancement of physics in the field of crystallinity. The challenging synthesis of multicrystalline polymers has resulted in only a limited number of tricrystalline terpolymers having been reported to date. We report, for the first time, the synthesis of polyethylene‐b‐poly(ethylene oxide)‐b‐poly(ϵ‐caprolactone)‐b‐poly(l‐lactide) (PE‐b‐PEO‐b‐PCL‐b‐PLLA), a tetracrystalline tetrablock quarterpolymer, by combining polyhomologation, ring‐opening polymerization, and an organic/metal “catalyst switch” strategy. 1H NMR spectroscopy and gel‐permeation chromatography confirmed the formation of the tetrablock quarterpolymer, while differential scanning calorimetry, X‐ray diffraction, and wide‐line separation solid‐state NMR spectroscopy revealed the existence of four different crystalline domains. Four in a row: The combination of polyhomologation, ring‐opening polymerization, and an organic/metal catalyst switch strategy led to the tetracrystalline tetrablock quarterpolymer polyethylene‐b‐poly(ethylene oxide)‐b‐poly(ϵ‐caprolactone)‐b‐poly(l‐lactide). The existence of four different crystalline domains in the polymer was confirmed by differential scanning calorimetry, X‐ray diffraction, and wide‐line separation solid‐state NMR spectroscopy.
ISSN:1433-7851
1521-3773
DOI:10.1002/anie.201908688