Zitieren Sie bitte immer diesen URN: urn:nbn:de:kobv:b43-652844
Poly(butylene terephthalate): About condensation, cyclization, degradation and elimination reactions in the solid state, and the role of smooth crystal surfaces
- Three commercial poly(butylene terephthalate) (PBT) samples - Pocan B1300 (B13), Pocan B1600 (B16), and Addigy P 1210 (AP121) - served as the starting materials for the annealing experiments, which were conducted with and without the addition of esterification and transesterification catalysts. The catalysts used were Sn(II) 2-ethylhexanoate (SnOct₂), Zr(IV) acetylacetonate, and 4-toluene sulfonic acid (TSA). Temperatures varied between 150 and 210 °C. The PBT samples were characterized using differential scanning calorimetry (DSC), gel permeation chromatography (GPC), small-angle X-ray scattering (SAXS), and matrix-assisted laser desorption/ionization time-of-flight (MALDI TOF) mass spectrometry. The MALDI mass spectra of all three samples differed greatly but displayed mass peaks of cycles. Similar results were produced by annealing with SnOct₂ or Zr(acac)₄, which favored the formation of even-numbered cycles within the mass range below m/z 5000, along with slow degradation. TSAThree commercial poly(butylene terephthalate) (PBT) samples - Pocan B1300 (B13), Pocan B1600 (B16), and Addigy P 1210 (AP121) - served as the starting materials for the annealing experiments, which were conducted with and without the addition of esterification and transesterification catalysts. The catalysts used were Sn(II) 2-ethylhexanoate (SnOct₂), Zr(IV) acetylacetonate, and 4-toluene sulfonic acid (TSA). Temperatures varied between 150 and 210 °C. The PBT samples were characterized using differential scanning calorimetry (DSC), gel permeation chromatography (GPC), small-angle X-ray scattering (SAXS), and matrix-assisted laser desorption/ionization time-of-flight (MALDI TOF) mass spectrometry. The MALDI mass spectra of all three samples differed greatly but displayed mass peaks of cycles. Similar results were produced by annealing with SnOct₂ or Zr(acac)₄, which favored the formation of even-numbered cycles within the mass range below m/z 5000, along with slow degradation. TSA favored a more intensive degradation without the formation of cycles or even with the destruction of cycles. PBT chains with two carboxylic (COOH) end groups were the most stable species under all circumstances. The origin of the extremely high melting point of AP121 (241–242 °C) can be explained by the smoothing of crystallite surfaces via transesterification. The results suggest that combining MALDI mass spectrometry and SAXS measurements provides a new way to better understand the solid-state chemistry of PBT and related polyesters.…


| Autor*innen: | Hans R. Kricheldorf, Steffen WeidnerORCiD, Andreas Meyer |
|---|---|
| Dokumenttyp: | Zeitschriftenartikel |
| Veröffentlichungsform: | Verlagsliteratur |
| Sprache: | Englisch |
| Titel des übergeordneten Werkes (Englisch): | Polymer Degradation and Stability |
| Jahr der Erstveröffentlichung: | 2026 |
| Organisationseinheit der BAM: | 6 Materialchemie |
| 6 Materialchemie / 6.3 Strukturanalytik | |
| Veröffentlichende Institution: | Bundesanstalt für Materialforschung und -prüfung (BAM) |
| Verlag: | Elsevier Ltd. |
| Jahrgang/Band: | 245 |
| Aufsatznummer: | 111862 |
| Erste Seite: | 1 |
| Letzte Seite: | 11 |
| DDC-Klassifikation: | Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Ingenieurwissenschaften und zugeordnete Tätigkeiten |
| Freie Schlagwörter: | Crystallization; MALDI-TOF MS; Polybutylene Terephthalate; cyclization; solid state |
| Themenfelder/Aktivitätsfelder der BAM: | Material |
| Material / Degradationsmechanismen | |
| DOI: | 10.1016/j.polymdegradstab.2025.111862 |
| URN: | urn:nbn:de:kobv:b43-652844 |
| ISSN: | 0141-3910 |
| Verfügbarkeit des Dokuments: | Datei für die Öffentlichkeit verfügbar ("Open Access") |
| Lizenz (Deutsch): | Creative Commons - CC BY-NC-ND - Namensnennung - Nicht kommerziell - Keine Bearbeitungen 4.0 International |
| Datum der Freischaltung: | 05.01.2026 |
| Referierte Publikation: | Ja |
| Datum der Eintragung als referierte Publikation: | 05.01.2026 |
| Schriftenreihen ohne Nummerierung: | Wissenschaftliche Artikel der BAM |


