Synthesis and Characterization of Functionalized Crosslinkable Poly(ε‐caprolactone)

Abstract

Summary: A new and rather simple method to obtain randomly crosslinked PCL is reported. PCL was previously functionalized through radical grafting of MA and GMA in the melt, using a Brabender‐like apparatus. GMA was added in order to obtain higher grafting efficiency. The structure of PCL‐g‐MAGMA was elucidated by 1H NMR spectroscopy, and the content of grafted MA was determined by FT‐IR spectroscopy. PCL‐g‐MAGMA was successively crosslinked through reaction with HMDI. The degree of crosslinking was determined by solvent extractions with chloroform. Thermal and dynamic mechanical analysis and tensile tests were performed on plain PCL, on PCL‐g‐MAGMA and on crosslinked PCL samples.Schematic representation of PCL‐g‐MAGMA structure.magnified imageSchematic representation of PCL‐g‐MAGMA structure.

Amorphized cellulose as filler in biocomposites based on poly(ɛ-caprolactone)

“…In fact, as already reported (Laurienzo et al, 2006), the chemical modification of PCL with MA and GMA occurs without leaving a significant amount of unreacted epoxy groups, so that the possible chemical reaction between cellulose and residual epoxy groups should be considered negligible.…”

“…PCL-g-MAGMA was prepared in the melt by using a Brabender Plasticorder internal mixer (Haque et al, 2012;Laurienzo, Malinconico, Mattia, & Romano, 2006). A mixture constituted by 36 g of PCL, 2 g of MA and 0.5 g of dibenzoyl peroxide (DBPO) was first fed into the mixer at 100 • C and then 2 g of GMA were added dropwise.…”

Enhancement of interfacial adhesion between starch and grafted poly(ε-caprolactone)

“…On the other hand, it is well known that MA is prone to co-polymerize (Laurienzo et al, 2006). To enhance the functionalization degree of MA, the more reactive GMA co-monomer was added to the bulk.…”

“…The bands at 1777 and 1850 cm -1 , which correspond to symmetric and 8 asymmetric stretching vibration of the anhydride group, were taken as the analytical reference bands for quantitative determination. Before determination, a calibration curve was built up with different amounts of succinic anhydride in chloroform Laurienzo et al (2006). PCL and grafted PCL materials were characterized as to their structural properties through FTIR analysis, crystallization pattern by means of X-Ray diffraction spectra, and thermal behaviour by DSC, as described below.…”

“…Laurienzo et al (2006) adopted a rather innovative method to functionalize PCL, with simultaneous melt grafting of maleic anhydride (MA) and glycidyl methacrylate (GMA) in a batch mixer and in presence of peroxide as initiator. They found that the addition of GMA improved the grafting efficiency (Laurienzo et al, 2006 andMangiacapra et al, 2007). Nevertheless, the use of such grafted PCL as compatibilizer for starch-PCL systems has not yet been investigated.…”