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Synthesis of poly(sebacic anhydride): effect of various catalysts on structure and thermal properties

  • Alena Pavelkova
  • Pavel Kucharczyk
  • Jiri Zednik
  • Vladimir Sedlarik
Original Paper
  • 414 Downloads

Abstract

The authors investigate the efficiency of various catalysts (22 types, based on oxides, carbonates, chlorides, organometallic compounds, N-heterocyclic carbine based compounds, cadmium acetate and molecular sieves) in the process of poly(sebacic acid) anhydride (PSA) synthesis. Their efficiency was studied utilizing methods that characterize the molecular weight distribution (gel permeation chromatography, GPC), structure (Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR), mass spectroscopy (MS)) and thermal properties (differential scanning calorimetry, (DSC), thermogravimetry (TGA)) of the final products. Such structural characterization gave good insight into the resulting polymer structure. Findings reveal the crucial role of catalyst selection in the resulting properties of PSA. The maximum M w values reached were found at approximately 280 kg.mol−1, which in the case of the calcium oxide catalyst was achieved after 60 min of reaction. TGA analyses showed a two-step thermal degradation process for all samples. No significant effect of the catalyst used was observed on polyanhydride thermal stability. However, it was proven that such catalysts do significantly influence the crystallinity of the resulting polyanhydrides.

Keywords

Poly(sebacic anhydride) Melt polycondensation Catalysts Thermal properties NMR DSC GPC DSC Py-GC/MS 

Notes

Acknowledgments

This work was supported by Operational Programme Research and Development for Innovations, co-funded by the European Regional Development Fund and the national budget of the Czech Republic (project CZ.1.05/2.1.00/03.0111), within the framework of a project entitled Centre of Polymer Systems and Operational Programme Education for Competitiveness, co-funded by the European Social Fund (ESF) and the national budget of the Czech Republic, within the framework of the project Advanced Theoretical and Experimental Studies (project CZ.1.07/2.3.00/20.0104). The authors are also grateful to the Ministry of Education, Youth and Sports of the Czech Republic for co-supporting this work within the framework of the EUPRO project (no. LE12002) and Internal grant agency of Tomas Bata University in Zlin (project no. IGA/FT/2014/012).

Supplementary material

10965_2014_426_Fig7_ESM.gif (568 kb)
Figure S1

SEM pictures of selected catalysts (GIF 568 kb)

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High Resolution Image (TIFF 22379 kb)
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Figure S2

XRD spectra of selected catalysts (GIF 2 kb)

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Figure S2

XRD spectra of selected catalysts (GIF 2 kb)

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High Resolution Image (TIFF 8939 kb)
10965_2014_426_MOESM3_ESM.tif (9.3 mb)
High Resolution Image (TIFF 9479 kb)

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Copyright information

© Springer Science+Business Media Dordrecht 2014

Authors and Affiliations

  • Alena Pavelkova
    • 1
    • 2
  • Pavel Kucharczyk
    • 1
  • Jiri Zednik
    • 3
  • Vladimir Sedlarik
    • 1
  1. 1.Centre of Polymer Systems, University InstituteTomas Bata University in ZlinZlinCzech Republic
  2. 2.Polymer Centre, Faculty of TechnologyTomas Bata University in ZlinZlinCzech Republic
  3. 3.Faculty of Science, Department of Physical and Macromolecular ChemistryCharles University in PraguePrague 2Czech Republic

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