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Dr. Larry G. Bourland poly VISIONS, INC 25 Devco Drive Manchester, PA 17345

Solutions for PET: Nucleating Additives for Crystallization Rate & GraftedModifiers for Impact Strength. Dr. Larry G. Bourland poly VISIONS, INC 25 Devco Drive Manchester, PA 17345. Advantages High Melting (265 o C) Temperatures Heat Resistance Low Cost Excellent Barrier. Drawbacks

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Dr. Larry G. Bourland poly VISIONS, INC 25 Devco Drive Manchester, PA 17345

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  1. Solutions for PET: Nucleating Additives for Crystallization Rate & GraftedModifiers for Impact Strength Dr. Larry G. BourlandpolyVISIONS, INC25 Devco DriveManchester, PA 17345

  2. Advantages High Melting (265oC) Temperatures Heat Resistance Low Cost Excellent Barrier Drawbacks Degrades by Moisture Induced Chain Scission Reactions in Melt State Slow Crystallization Rate Brittle at Low Temperatures Attributes of PET

  3. Drawbacks Degrades by Moisture Induced Chain Scission Reactions in Melt State Slow Crystallization Rate Brittle at Low Temperatures Solutions Dry Material before Processing Reactions Promote grafting of end groups Avoid Chain Scission Crystallization Rate Acceleration by Heterogeneous Nucleant Retardation by Homogeneous Additives Impact modify with Rubber compatibilized using PET-g-Rubber Solutions to Drawbacks

  4. Presentation Topics • Melt Rheology of PET & PET Alloys • Vacuum Drying • Testing Procedures • Melt Flow Rate (MFR) vs PET IV • Capillary Melt Viscosity • ( h vs. g )  Evidence for reaction • ( h vs. time)  Evidence for completed reaction • Control of Crystallization Rate • Mineral Heterogeneous Nucleants • Reactive Degradation of PET • Efficiencies of Rate Acceleration • Miscible Polymers Homogeneous Nucleants • Reaction or Miscibility? • Efficiency of Rate Retardation • Impact Strength at low temperatures • Evidence for PET End Group Reaction with modified rubber to produce PET-g-Rubber additive • PET-graft-Rubber additives compatibilizes Rubber with PET --> enhanced impact strengths at low temperatures

  5. Melt RheologySample Drying • Measurements • Capillary Rheometry (Viscosity vs. Shear Rate) Data Comparison • Viscosity at Common Shear Rate (200 sec-1)

  6. Vacuum Drying Temps & Times

  7. PET Viscosity vs. Dry Time & Temperature

  8. Melt Flow Conditions for PET Modifications to ASTM Procedures  range of 1-10 (g/10 min) for PET products: • Test Temperature 285oC • Orifice Diameter 0.040 inch • Weight Load 3.7 Kg • Sample Load Time <1 minute • Drying Requirements < 20 ppm or (time at temperature to achieve constant viscosity)

  9. Correlation of MFR vs PET IV

  10. Melt RheologyGrafting Reactions Capillary Rheology Measurements • Extent of Reaction: • Viscosity vs. Time • Evidence for Reaction: • Viscosity vs. Shear Rate

  11. Melt Viscosity vs. TimeCompletion of Reaction: PET-graft-Rubber

  12. Extent of Reaction: PET-graft-Rubber

  13. Accelerating PET Crystallization Heterogeneous Nucleants for PET: Type Nucleating Reactive Talc Yes Yes CaCO3 Yes Yes BaSO4 Yes Yes Carbon Black Yes No Silicates No No Mica No No

  14. Talc Reactivity

  15. Reactivity of PET / Talc: Size and Origin

  16. Reactivity of PET / CaCO3 & BaSO4

  17. Crystallization Rate: %Nucleant & Type

  18. PET Nucleation by Talc Masterbatch

  19. Development of Crystallinity during Thermoforming

  20. Retarding PET Crystallization Miscible Additives Retard Crystallization • Homogeneous Effect • Some Waxes and Plasticizer • Selected Polycarbonates • Enhanced Potential Reaction with PET

  21. Retardation of PET Crystallization Rate

  22. Impact Modification of PET Rubbery Additives alone are ineffective: • Immiscible with PET • Poor Interfacial Contact • Limited Stress Transfer to Rubber PET/Rubber Interfacial compatibilization with Graft Copolymer is effective: • Primary Rubber  EMAC Copolymer • Graft Compatibilizer  PET-g-EMAC • Homopolymer Matrix 0.95 IV PET

  23. GFWI Improved with Graft Compatibilizer

  24. GFWI Improved with Graft Compatibilizer

  25. Conclusions PET Melt Rheology • Reliable Methodology • MFR Correlates with IV for pure PET Resins • Melt Flow of PET Alloys • Reactivity of PET with Minerals • Reactivity of PET with Functionalized Polymers: • Reaction Exists • Extent of Reaction • Stability of Reactants

  26. Conclusions PET Additives Crystallization Rate Control • Accelerate Rate of PET Crystallization • PET / Mineral Masterbatches • Heterogeneous Nucleation • Retard Rate of PET Crystallization • PET / PC Alloys • Homogeneous Effect Improve Impact Strength of PET: • PET-g-Rubber Modifier by Reactive Extrusion with Functionalized Rubber • Compatibilizer for PET / Rubber Interface • Improve Impact Strength of PET at Ambient and Low Temperatures

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