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Characterization and polymerization of a cyclic precursor to poly(p-phenylene sulfide)

Zimmerman, Dean Arthur

Abstract Details

1995, Doctor of Philosophy, Case Western Reserve University, Macromolecular Science.
Cyclic phenylene sulfide (CPS) oligomers are examined as a precursor to poly(p-phenylene sulfide) (PPS). The vibrational spectra of the polymer is examined and bands are assigned based on para-disubstituted benzene modes and symmetry of the polymer. Isothermal crystallization of quenched PPS is examined in-situ by infrared spectroscopy using a heated cell. In addition, the spectra of the quenched, annealed and cured PPS are examined, and the bands are interpreted based on the structure of the polymer. Commercial PPS is extracted and a soluble fraction is obtained. The cyclic hexamer of phenylene sulfide (CHPS) is isolated and characterized. The vibrational spectra are examined and compared to the polymer. Differences in the spectra are interpreted based on the symmetry of the molecules. The CHPS is polymerized in the melt, and the spectrum of the resulting polymer is compared to commercial PPS in order to examine the differences between the two materials. Also, a crystal structure change induced by heating or pressure is identified in the CHPS. This crystal structure change is investigated using infrared spectroscopy, Raman spectroscopy, X-ray powder diffractometry, and scanning electron microscopy (SEM). The onset of the transformation is identified by differential scanning calorimetry (DSC), optical microscopy, and an infrared technique using a heated cell. Molecular modeling is employed to examine the lowest energy state of the molecule. A mixture of CPS oligomers is obtained by employing high dilution in the PPS synthesis. The mixture is polymerized by heating with and without the presence of carbon fibers. DSC is used to examine the crystallization parameters, which are used to estimate the molecular weight. The effect of different reaction temperatures are employed to examine the effect on the molecular weight. The effect of annealing is also examined. Optical microscopy and SEM are used to examine the morphology of the resulting polymer. The morphology on the surface of carbon fibers is also examined. The effect of high temperatures (>340°C) on the two materials is also evaluated by infrared spectroscopy.
Hatsuo Ishida (Advisor)
166 p.

Recommended Citations

Citations

  • Zimmerman, D. A. (1995). Characterization and polymerization of a cyclic precursor to poly(p-phenylene sulfide) [Doctoral dissertation, Case Western Reserve University]. OhioLINK Electronic Theses and Dissertations Center. http://rave.ohiolink.edu/etdc/view?acc_num=case1058208724

    APA Style (7th edition)

  • Zimmerman, Dean. Characterization and polymerization of a cyclic precursor to poly(p-phenylene sulfide). 1995. Case Western Reserve University, Doctoral dissertation. OhioLINK Electronic Theses and Dissertations Center, http://rave.ohiolink.edu/etdc/view?acc_num=case1058208724.

    MLA Style (8th edition)

  • Zimmerman, Dean. "Characterization and polymerization of a cyclic precursor to poly(p-phenylene sulfide)." Doctoral dissertation, Case Western Reserve University, 1995. http://rave.ohiolink.edu/etdc/view?acc_num=case1058208724

    Chicago Manual of Style (17th edition)