Synthesis and characterization of poly(allyl methacrylate) obtained by free radical initiator


Vardareli T. K., Keskin S., Usanmaz A.

JOURNAL OF MACROMOLECULAR SCIENCE PART A-PURE AND APPLIED CHEMISTRY, vol.45, no.4, pp.302-311, 2008 (SCI-Expanded) identifier identifier

  • Publication Type: Article / Article
  • Volume: 45 Issue: 4
  • Publication Date: 2008
  • Doi Number: 10.1080/10601320701863783
  • Journal Name: JOURNAL OF MACROMOLECULAR SCIENCE PART A-PURE AND APPLIED CHEMISTRY
  • Journal Indexes: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Page Numbers: pp.302-311
  • Keywords: allyl methacrylate, solution polymerization, TGA-FT-IR, NMR, XPS, THERMAL-DEGRADATION, ALLYL METHACRYLATE, CROSS-LINKING, POLYMERIZATION, POLYMERS, GELATION
  • Middle East Technical University Affiliated: Yes

Abstract

Allyl methacrylate was polymerized in CCl4 solution by alpha,alpha'-azoisobutyronitrile at 50, 60, and 70 degrees C. The kinetic curves were auto-accelarated types at 60 and 70 degrees C, but almost linear at 50 degrees C. Arrhenius activation energy was 77.5 kJ/mol. The polymer was insoluble in common organic solvents. It was characterized by FT-IR, NMR, DSC, TGA and XPS methods. About 98-99% of allyl side groups were remained as pendant even after completion of the polymerization. The spectroscopic and thermal results showed that polymerization is not a cyclopolymerization type, but may have end group cyclization. The high molecular weight is the main cause of a polymer being insoluble even in the early stage of the polymerization. Molecular weight of 1.1106 for a soluble polymer fraction was measured by light scattering method. The Tg of polymer was 94 degrees C, and after curing at 150-200 degrees C, increased to 211 degrees C. The thermal pyrolysis of polymer at about 350 degrees C gave an anhydride by linkage type degradation, and side group cyclization. The XPS analysis showed the presence of radical fragments of AIBN (initiator) and CCl4 (solvent) associated with oligomers.