Characterization of poly(ethylene glycol)-b-poly(ε-caprolactone) by liquid chromatography under critical conditions: Influence of catalysts and reaction conditions on product composition

被引:16
作者
Ahmed, Hasnat [1 ,3 ]
Trathnigg, Bernd [1 ,3 ]
Kappe, C. Oliver [2 ,3 ]
Saf, Robert [4 ,5 ]
机构
[1] CePOL MC, A-8010 Graz, Austria
[2] CDLMC, A-8010 Graz, Austria
[3] Karl Franzens Univ Graz, Inst Chem, A-8010 Graz, Austria
[4] CePOL SA, A-8010 Graz, Austria
[5] Graz Univ Technol, ICTM, A-8010 Graz, Austria
关键词
Block copolymers; Liquid chromatography; Critical conditions; Caprolactone; Microwave assisted polymerization; RING-OPENING POLYMERIZATION; TOF MASS-SPECTROMETRY; EPSILON-CAPROLACTONE; DIBLOCK COPOLYMERS; BLOCK-COPOLYMERS; CHEMICAL-COMPOSITION; COUPLED DENSITY; POLYMERS; FUNCTIONALITY; OXIDE)-BLOCK-POLY(L-LACTIDE);
D O I
10.1016/j.eurpolymj.2009.05.001
中图分类号
O63 [高分子化学(高聚物)];
学科分类号
070305 ; 080501 ; 081704 ;
摘要
Amphiphilic block copolymers were synthesised by ring opening polymerization of E-caprolactone with polyethylene glycol monomethyl ether (PEG-MME) using different catalysts (boron trifluoride, sodium hydride, and tin octoate) in a one pot procedure. The products obtained were characterized with respect to their molar mass distribution and content of homopolymers using size exclusion chromatography (SEC), Liquid chromatography under critical conditions (LCCC) and MALDI-TOF-MS. The homopolymers of caprolactone could be separated from the block copolymer by LCCC on a reversed phase column in tetrahydrofurane-water mobile phases with evaporative light scattering detection (ELSD). Residual monomer could be determined under the same conditions using density detection, a separation of the copolymer from residual initiator could be achieved on a normal phase column in acetone-water mobile phases. (C) 2009 Elsevier Ltd. All rights reserved.
引用
收藏
页码:2338 / 2347
页数:10
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