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Journal of Thermal Analysis and Calorimetry

, Volume 67, Issue 1, pp 177–188 | Cite as

Thermal Analysis of Acrylonitrile Polymerization and Cyclization in the Presence of N,N-Dimethylformamide

  • M. A. Avilés
  • J. M. Ginés
  • J. C. del Rio
  • J. Pascual
  • J. L. Pérez-Rodríguez
  • P. J. Sánchez-SotoEmail author
Article

Abstract

This paper examines the polymerization of acrylonitrile to poly(acrylonitrile)(PAN), and its cyclization, in bulk form and using N,N-dimethylformamide (DMF) as solvent in which both monomer and polymer are soluble. Thermal analysis of the resultant products after polymerization has been performed by DSC and pyrolysis gas chromatography/mass spectrometry (Py-GC/MS). Scanning electron microscopy has been used to study the morphology of the resultant products and after thermal treatments. The DSC thermal curve of PAN-DMF sample is quite different from the PAN bulk sample, showing a single sharp exothermic peak associated with nitrile group polymerization (cyclization) of PAN at lower temperature (240°C) than that of bulk PAN sample (314°C). Cyclization of PAN was confirmed by IR spectroscopy. It was found that the amide molecules are difficult to eliminate completely in the product obtained after the polymerization reaction, even after prolonged heating at 110°C, and remain occluded. The formation of a complex by dipolar bonding is also possible and it is discussed. It is concluded that the amount of heat evolved as well as the temperature interval over which it is released are influenced by the chemical processing of PAN when using DMF as solvent of both monomer and polymer. Pyrolysis of these PAN samples revealed the release of occluded molecules of DMF, and several compounds containing nitrogen produced from the thermal degradation processes. All these results are interesting to know the chemical processing of carbon fibres and activated carbon fibres from PAN modified precursors.

acrylonitrile cyclization DMF DSC hexanedinitrile morphology poly(acrylonitrile) pyridine derivatives pyrolysis SEM 

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Copyright information

© Kluwer Academic Publishers 2002

Authors and Affiliations

  • M. A. Avilés
    • 1
  • J. M. Ginés
    • 2
  • J. C. del Rio
    • 3
  • J. Pascual
    • 4
  • J. L. Pérez-Rodríguez
    • 1
  • P. J. Sánchez-Soto
    • 1
    Email author
  1. 1.Instituto de Ciencia de Materiales de Sevilla (ICMSE), Centro Mixto Consejo Superior de Investigaciones Científicas (C.S.I.C.)Universidad de SevillaSevillaSpain
  2. 2.Departamento de Farmacia y Tecnología Farmaceútica, Facultad de FarmaciaUniversidad de SevillaSevillaSpain
  3. 3.Instituto de Recursos Naturales y Agrobiología de SevillaC.S.I.C.SevillaSpain
  4. 4.Departamento de Ingeniería Civil, de Materiales y Fabricación, Escuela Técnica Superior de Ingenieros IndustrialesUniversidad de MálagaMálagaSpain

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