Synthesis and characterization of anhydride-functional polycaprolactone

Jacob John, Jian Tang, Zhihong Yang, Mrinal Bhattacharya

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70 Scopus citations

Abstract

Polycaprolactone-graft-maleic anhydride (PCL-g-MA) copolymer was prepared by grafting maleic anhydride onto PCL in a batch mixer and in an extruder using dicumyl peroxide as the initiator. The graft content was determined with the volumetric method by converting the anhydride functions to acid groups and then titrating with ethanolic potassium hydroxide. The grafted polymer was extracted with xylene to remove any unreacted monomer before the estimation step. The effect of temperature and the various concentrations of the initiator and monomer used for the grafting reaction were investigated. The presence of residual initiator in the reaction product was checked using thin-layer chromatography. Molecular weight determination was carried out for the pure and grafted polymer using gel permeation chromatography to determine if chain scission was present. Results indicate that maleic anhydride is grafted onto PCL using free radical initiators. The grafting reaction was confirmed by FTIR and NMR techniques. FTIR spectra showed absorption bands around 1785 and 1858 cm-1. NMR spectra gave signals for methine proton at 3.47 ppm. For a given peroxide level, a higher temperature or residence (reaction) time gave higher percentage of grafted MA. There was an optimum temperature and initiator concentration after which the percentage of MA grafted on PCL decreased. The number-average molecular weight, tensile strength, and the percent elongation of PCL-g-MA were comparable to those of PCL before grafting.

Original languageEnglish (US)
Pages (from-to)1139-1148
Number of pages10
JournalJournal of Polymer Science, Part A: Polymer Chemistry
Volume35
Issue number6
DOIs
StatePublished - Apr 30 1997

Keywords

  • Anhydride-functional polymer
  • Chemical grafting
  • FTIR
  • H-NMR
  • Polycaprolactone

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