Macrocycles 25. Cyclic poly(ether sulfone)s derived from 4-tert-butylcatechol

  • Poly(ether sulfone)s were prepared by polycondensation of silylated 4-tert-butylcatechol and 4,4?-difluorodiphenylsulfone in N-methylpyrrolidone. The feed ratio and the reaction time were varied to study the influence of stoichiometry and conversion on molecular weight and extent of cyclization. Molecular weights and molecular weight distributions (MWD)s were characterized by SEC measurements calibrated with polystyrene. Light scattering confirmed that calibration with polystyrene gives reasonable results and revealed a tendency towards a bimodal MWD for the samples rich in cycles. The MALDI-TOF mass spectrometry indicated that the extent of cyclization increased with higher conversion and with optimization of the stoichiometry. This interpretation was confirmed by 1H NMR endgroup analyses. For the samples with the highest molar masses only mass peaks of cycles were found, which were detectable up to 20 000 Da before and up to 27 000 Da after fractionation. Via the pseudo-high dilutionPoly(ether sulfone)s were prepared by polycondensation of silylated 4-tert-butylcatechol and 4,4?-difluorodiphenylsulfone in N-methylpyrrolidone. The feed ratio and the reaction time were varied to study the influence of stoichiometry and conversion on molecular weight and extent of cyclization. Molecular weights and molecular weight distributions (MWD)s were characterized by SEC measurements calibrated with polystyrene. Light scattering confirmed that calibration with polystyrene gives reasonable results and revealed a tendency towards a bimodal MWD for the samples rich in cycles. The MALDI-TOF mass spectrometry indicated that the extent of cyclization increased with higher conversion and with optimization of the stoichiometry. This interpretation was confirmed by 1H NMR endgroup analyses. For the samples with the highest molar masses only mass peaks of cycles were found, which were detectable up to 20 000 Da before and up to 27 000 Da after fractionation. Via the pseudo-high dilution method low molar mass poly(ether sulfone) containing more than 95 mol% of cycles were prepared, and even these low molar mass samples had broad MWDs. DSC measurements indicated that the glass transition temperatures depend on the structure of the endgroups and increase with higher fractions of cycles.zeige mehrzeige weniger

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Metadaten
Autor*innen:H.R. Kricheldorf, L. Vakhtangishvili, G. Schwarz, Günter Schulz, Ralph-Peter Krüger
Dokumenttyp:Zeitschriftenartikel
Veröffentlichungsform:Verlagsliteratur
Sprache:Englisch
Titel des übergeordneten Werkes (Englisch):Polymer
Jahr der Erstveröffentlichung:2003
Verlag:Springer
Verlagsort:Berlin
Jahrgang/Band:44
Erste Seite:4471
Letzte Seite:4480
Freie Schlagwörter:MALDI-TOF mass spectrometry; Poly(ether sulfone)s; Polycondensation
DOI:10.1016/S0032-3861(03)00410-5
ISSN:0032-3861
ISSN:1873-2291
Verfügbarkeit des Dokuments:Physisches Exemplar in der Bibliothek der BAM vorhanden ("Hardcopy Access")
Bibliotheksstandort:Sonderstandort: Publica-Schrank
Bibliotheksstandort:ZP 23
Datum der Freischaltung:19.02.2016
Referierte Publikation:Ja
Datum der Eintragung als referierte Publikation:25.08.2003
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