Synthesis of Ultra-Small Branched Star Poly(epsilon-caprolactone)s and their High End Group Concentration Effects on Crystallization
- Authors
- Choi, Woohyuk; Chung, Jae Woo; Kwak, Seung-Yeop
- Issue Date
- 1-May-2015
- Publisher
- WILEY-BLACKWELL
- Keywords
- crystallization; end-capping; monomer-to-polymer conversion; ring-opening polymerization; star polymers; ultra-small branch; vacuum purification
- Citation
- JOURNAL OF POLYMER SCIENCE PART A-POLYMER CHEMISTRY, v.53, no.9, pp.1134 - 1142
- Journal Title
- JOURNAL OF POLYMER SCIENCE PART A-POLYMER CHEMISTRY
- Volume
- 53
- Number
- 9
- Start Page
- 1134
- End Page
- 1142
- URI
- http://scholarworks.bwise.kr/ssu/handle/2018.sw.ssu/8734
- DOI
- 10.1002/pola.27544
- ISSN
- 0887-624X
- Abstract
- We successfully synthesize the three- and six-branched star poly(epsilon-caprolactone)s with extremely small branched segments (USB-SPCLs) using a facile pseudo-one-pot process in a pilot scale and investigate the effect of ultra-small branches on their crystallization behaviors. The number of branched segments and the individual branched segment lengths for USB-SPCLs are precisely controlled via manipulating monomer-to-core ratio, adjusting monomer-to-polymer conversion, end-capping the terminal hydroxyl groups, and vacuum purification, which results in USB-SPCLs having the branched segments below five degree of polymerization with a high yield exceeding 93%. The molecular weights obtained from H-1 NMR spectroscopy are consistent with that obtained from MALDI-TOF-MS and the molecular weight distributions are narrow with M-w/M(n)1.2, indicating that USB-SPCLs have mono-dispersed branches. USB-SPCLs have low melting temperatures and broad double-melting peaks attributed to their extremely small branches, and the crystallization behaviors for USB-SPCLs depend on the end group concentration. On the other hand, the glass transitions for USB-SPCLs depend on the total molecular weights, regardless of the number and length of branched segments. (c) 2015 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2015, 53, 1134-1142
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