Structural characterizations, thermal behavior, and electrical measurements of the amidosulfonic acid catalyzed thermal ring-opening polymerization of substituted cyclotriphosphazene in 1,2,4-trichlorobenzene solution


Koran K., GÖRGÜLÜ A. O.

Advances in Polymer Technology, cilt.37, sa.8, ss.3229-3239, 2018 (SCI-Expanded) identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 37 Sayı: 8
  • Basım Tarihi: 2018
  • Doi Numarası: 10.1002/adv.22092
  • Dergi Adı: Advances in Polymer Technology
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Sayfa Sayıları: ss.3229-3239
  • Anahtar Kelimeler: activation energy, dielectric constant, dielectric property, polyphosphazene, ring-opening polymerization
  • Marmara Üniversitesi Adresli: Evet

Özet

In this study, we aimed to design and synthesize poly[3,3,5,5-tetrachloro-1,1-bis{spiro(2′,2″-dioxy-1′-1″-biphenylyl)}phosphazene] (3) in order to obtain a polymer which is resistant to moisture and hydrolysis and also contains chlorine atoms within its structure. For this reason, the polymerization experiments of polymer 3 were performed using ring-opening polymerization (ROP) of 3,3,5,5-tetrachloro-1,1-bis[spiro(2′,2″-dioxy-1′,1″-biphenylyl)]cyclotriphosphazene (2) at different time and temperature. In particular, ROP of 2 was successful in 1,2,4-trichlorobenzene solution in the presence amidosulfonic acid and promoter (CaSO 4 .2H 2 O) in sealed glass tubes under vacuum for 60, 72, and 96 hr at 220°C. The changes in molecular weight and molecular weight distribution of the polymer 3 were noted as a function of polymerization reaction time. The structure of polymer 3 was approved by gel permeation chromatography (GPC), FT-IR, NMR spectroscopy ( 31 P, 1 H, 13 C), and elemental analysis. The glass transition temperature (T g ) and thermal stability of polymer 3 were determined using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), respectively. Dielectric properties of 3 were determined as a function of frequency at five different temperatures by an impedance analyzer. The activation energy of polymer 3 was calculated using Flynn–Wall–Ozawa (F–W–O) integral method.