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Polymer Synthesis, Characterization and Processing

Polymer Synthesis, Characterization and Processing. R. A. Weiss, M. Cakmak , S. Gupta, E. McClanahan University of Akron. Annual Review, October 28, 2011. Topics Under Investigation. Characterization of PP-OH from Mike Chung Synthesis of High Temperature Polymers

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Polymer Synthesis, Characterization and Processing

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  1. Polymer Synthesis, Characterization and Processing R. A. Weiss, M. Cakmak, S. Gupta, E. McClanahan University of Akron Annual Review, October 28, 2011

  2. Topics Under Investigation • Characterization of PP-OH from Mike Chung • Synthesis of High Temperature Polymers • Characterization and Processing of PP from Borealis

  3. Characterization of PP-OH from M. Chung Need access to high temperature GPC (Brian Coughlin, UMass (Amherst))

  4. Intensity (a.u.) 10 15 20 25 30 35 40 45 50 2θ (deg) Effect of OH-substitution on Crystal Structure Wide-Angle X-Ray Diffraction PP and PP-OH have monoclinic crystal structures – no effect of OH substitution

  5. Lamellar Thickness of Crystals Small Angle X-Ray Scattering) Polypropylene d = 15.0 nm PP-OH (3.93% OH) d = 12.3 nm Iq2 (a.u.) PP-1 PP-2 PP-OH (1.3) PP-OH (1.4) PP-OH (1.7) PP-OH (3.9) 0 0.25 0.5 0.75 1.0 1.25 1.5 1.75 2.0 q (nm-1) Spherulite (space-filling) Growth Direction d Chain Direction lamella thickness (long spacing) Scattering Invariant

  6. Melt Rheology (Dynamic Experiments) aTw (1/s) aTw (1/s) • TTS works well • With increasing [OH], the melt viscosity increases and the melt becomes more elastic

  7. Melt Rheology of PP-OH Samples 105 104 103 102 101 100 τ ~ 0.01 s τ ~ 0.3 s PP (Mv = 511 kg/mol) G” η’0.1 ~ 103 Pa.s G’ 106 105 104 103 102 bTG’ or bTG” (Pa) PP-OH (1.7 mol% OH) (Mv = 388 kg/mol) ?? 2 2 G” 1 1 G’ η’0.1 ~ 2 x 104 Pa.s 10-2 10-1 100 101 102 103 aTω (s-1) ViscoelasticMastercurves @ 200C

  8. Cole-Cole Plot

  9. Anomalous Behavior for PP-OH (3.9 mol% OH) Weak Elastic Network No viscous flow bTG’ or bTG” (Pa) 2 G0.1 ~ 2 x 103 Pa 1 η’0.1 ~ 2 x 104 Pas aTω (s-1)

  10. Steady Shear Viscosity h (Pa.s)

  11. Sulfonated Poly(ether ether ketone) Red: acid Blue Zn-salt Tm %xyl % Crystallinity Tg

  12. Borealis Polypropylene Material Commercial Grades

  13. PP Rheology

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