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Synthesis and morphology characteristics of new highly branched polycaprolactone PCL
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SYSNO ASEP 0584545 Document Type J - Journal Article R&D Document Type Journal Article Subsidiary J Článek ve WOS Title Synthesis and morphology characteristics of new highly branched polycaprolactone PCL Author(s) Ziolo, A. (PL)
Mossety-Leszczak, B. (PL)
Walczak, M. (PL)
Strachota, Beata (UMCH-V) RID
Strachota, Adam (UMCH-V) RID, ORCID
Awsiuk, K. (PL)
Janiszewska, N. (PL)
Raczkowska, J. (PL)Article number 991 Source Title Molecules. - : MDPI
Roč. 29, č. 5 (2024)Number of pages 23 s. Language eng - English Country CH - Switzerland Keywords highly branched polymers ; star polymers ; poly(caprolactone) Subject RIV CD - Macromolecular Chemistry OECD category Polymer science Method of publishing Open access Institutional support UMCH-V - RVO:61389013 UT WOS 001182919900001 EID SCOPUS 85187763264 DOI 10.3390/molecules29050991 Annotation A simple and efficient method for the synthesis of biodegradable, highly branched polycaprolactone (PCL) is presented. The solvent-free (bulk) reaction was carried out via ring opening polymerization (ROP), catalyzed by tin octanoate Sn(Oct)2, and it employed hyperbranched polyamide (HPPA) as a macro-initiator. The core–shell structure of the obtained products (PCL-HPPA), with the hyperbranched HPPA core and linear PCL chains as shell, was in the focus of the product characterization. 1H nuclear magnetic resonance (1H NMR) and elemental analysis confirmed the covalent incorporation of the HPPA in the products, as well as a high degree of grafting conversion of its amino functional groups. Confocal Raman Micro spectroscopy, and especially Time-of-Flight Secondary Ion Mass Spectrometry, further supported the existence of a core–shell structure in the products. Direct observation of macromolecules by means of cryogenic transmission electron microscopy, as well as gel permeation chromatography (GPC), suggested the existence of a minor ‘aggregated’ product fraction with multiple HPPA cores, which was attributed to transesterification reactions. Differential scanning calorimetry, as well as X-ray diffraction, demonstrated that the PCL-HPPA polymers displayed a similar degree of crystallinity to linear neat PCL, but that the branched products possessed smaller and less regular crystallites. Workplace Institute of Macromolecular Chemistry Contact Eva Čechová, cechova@imc.cas.cz ; Tel.: 296 809 358 Year of Publishing 2025 Electronic address https://www.mdpi.com/1420-3049/29/5/991
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