Polyolefin Film Enhancement Using                Cyclic Olefin Copolymers                 For Retort Applications         ...
Project Objectives                 Desired Enhancements for Commercial Retort Films                 TOPAS COC Value Propos...
Desired Enhancements for Retort                      Extend Product Shelf Life From 3 To 5 Years                      Elim...
What Are Cyclic Olefin Copolymers (COC)?             The cyclic olefin copolymer (COC) molecule is a             linear ch...
TOPAS® COC - Basic Properties                 Glass transition temperatures, °C(°F)    Glass Clear, Transparent           ...
TOPAS® COC – Value Proposition in Retort                Moisture & Oxygen Barrier     - 1.5X to 5X barrier of polyolefins ...
Test Structures: TOPAS Blends I      ID           T1: 70/30 TOPAS 6013 / LLDPE                       T7: 5-Layer 6013 / LL...
Test Structures: TOPAS Blends IIID       T5: PP / LLDPE+LDPE / PP                             T12: 36% TOPAS 6015 PP Coex ...
Flat Film PropertiesSPE Polyolefins & FlexPackCon            www.topas.com
Tensile Strength At Yield (ASTM D882)                                                                                     ...
Impact Resistance                                                 Film          Slow Puncture Slow Puncture               ...
Tensile Modulus (ASTM D882)                                                                                             MD...
Tear Resistance (ASTM D1922)                                                                              MD    TD        ...
Retort Pouch PreparationSPE Polyolefins & FlexPackCon     www.topas.com
Pouch Preparation            Lamination            ▶ Faustel Pilot Size Laminator            ▶ 50 FPM Line Speed          ...
Pouch Preparation              Pouch Fabrication              ▶ Pouch Machine: Shanghi                       Gaoqin Packag...
Pouch Preparation                  Pouch Filling and Sealing                 ▶ Pouch Filling Machine: Toyo                ...
Pouch Seal Strength (ASTM F88-05)                                                      TOPAS®    Bottom Seal    Side Seal ...
Retort Program: Standard 250ºF Program             Temperature Sequence               (ºF)     Time (Minute) Pressure (psi...
Pouch Appearance After 250ºF Retort                                                            ®                          ...
Retort Program: Elevated 260ºF                                    Program     Temperature                                 ...
Pouch Appearance After 260ºF Retort                                                    TOPAS®                             ...
Retort ResultsSPE Polyolefins & FlexPackCon         www.topas.com
Tensile Modulus (ASTM D882)                                                                                     Preretort ...
Tensile Strength (ASTM D882)                                                                                       Prereto...
Yield Elongation (ASTM D882)                                                                                 Preretort   P...
T5: After & Before Retort / DMA                                                                                  Sample: A...
T1: After & Before Retort / DMA                                                                                    Sample:...
T7: After & Before Retort / DMA                                                                                       Samp...
T8: After & Before Retort / DMA                                                                                   Sample: ...
T12: Before & After Retort / DMA                                                                                  Sample: ...
T16: Pouches Before & After Retort                                                                                 Sample:...
T14: After & Before Retort / DMA                                                                                   Sample:...
T18: Pouches Before & After Retort                                                                                    Samp...
Pouch Burst Test: (ASTM D642-00)                                                            TOPAS® COC   250ºF Retort   26...
Gelbo Flex: (ASTM D392-93)                                                      Film                                      ...
MVTR @ 37.8ºC; 100% R.H. (ASTM F1249-01)                                                                            Post 2...
OTR @ 37.8ºC; 0% R.H. (ASTM D3985-02)                                                                               Post 2...
Summary & ConclusionsSPE Polyolefins & FlexPackCon    www.topas.com
Film & Retort Pouch Property Comparative                                         T5: PP / (LLDPE+LDPE) / PP       T12: PP ...
TOPAS® COC – Conclusions & Benefits                                TOPAS COC Enhances Stiffness, Dimensional Stability &  ...
Acknowledgments               TOPAS® Retort Team:                        Adam Barton, Wolfram Goerlitz, Randy Jester,     ...
NOTICE TO USERS: To the best of our knowledge, the information contained in this publication is accurate, however we do no...
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Polyolefin Film Enhancement Using COC for Retort Applications

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Polyolefin Film Enhancement Using COC for Retort Applications

  1. 1. Polyolefin Film Enhancement Using Cyclic Olefin Copolymers For Retort Applications Paul D. Tatarka SPE Polyolefins & FlexPack Conference February 25-27, 2008SPE Polyolefins & FlexPackCon www.topas.com
  2. 2. Project Objectives Desired Enhancements for Commercial Retort Films TOPAS COC Value Proposition COC Test Film Structures: ▶ Monolayer Cast Films (4) ▶ Multilayer Blown FIlms (2) ▶ Multilayer Cast Films with PP Skin Layers (5) Retort Pouch Preparation Understand How COC Responds Under Retort Conditions ▶ Appearance, Burst Strength, Gelbo Flex and Barrier ▶ Identify Most Promising COC Film Structures Conclusions and Recommendations for Future StudySPE Polyolefins & FlexPackCon www.topas.com
  3. 3. Desired Enhancements for Retort Extend Product Shelf Life From 3 To 5 Years Eliminate Foil To Offer Package Clarity Increase Barrier: ▶OTR ▶MVTR Increase Retort Temperature & Reduce Cycle Time Enhance Package Durability To Prevent Loss of Barrier Increase Package Stiffness For Pouches & Rigid Containers Commercial Retort (4.58 mil) PET / adh / Foil / adh / Nylon / adh / cast PP 0.48 mil 0.50 mil 0.60 mil 3.00 milSPE Polyolefins & FlexPackCon www.topas.com
  4. 4. What Are Cyclic Olefin Copolymers (COC)? The cyclic olefin copolymer (COC) molecule is a linear chain of small CH2-CH2 links randomly interspersed with large bridged ring elements It cannot fold up to make a regular structure, i.e., a crystallite NB NB NB NB COC has no crystalline melting point, but only a glass transition temperature, Tg , at which the polymer goes from “glassy” to “rubbery” behaviorSPE Polyolefins & FlexPackCon www.topas.com
  5. 5. TOPAS® COC - Basic Properties Glass transition temperatures, °C(°F) Glass Clear, Transparent 70 - 180 (154 – 356) Sterilizable via Steam, EtO, Modulus of elasticity, N/mm2 (kpsi) gamma, beta (E-beam) 2300 – 3200 (330 – 460) Resistant to Alcohols, Tensile strength, N/mm2 (kpsi) Acids, Bases, Polar 63 (9.1) Solvents Density, g/cm3 High Purity, Low 1.02 Extractables Water uptake, % Low Water Transmission < 0.01 Rate (WVTR) WVTR, g-mil/100 in2 × day (38°C/90%RH) 0.24 – 0.40 Biocompatible Halogen-freeSPE Polyolefins & FlexPackCon www.topas.com
  6. 6. TOPAS® COC – Value Proposition in Retort Moisture & Oxygen Barrier - 1.5X to 5X barrier of polyolefins Add Heat Resistance - High Tg grades available (138 - 180ºC) Enhance Stiffness - >2X modulus other polyolefins; enhances dimensional stability Polyolefin Compatible - Improve performance of PE & PP components in retort Transparency - Could offer good package claritySPE Polyolefins & FlexPackCon www.topas.com
  7. 7. Test Structures: TOPAS Blends I ID T1: 70/30 TOPAS 6013 / LLDPE T7: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends T8: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends Purpose Forming Film, Steam Sterilizable Stiff, Heat Resistant Blown Film Process Cast Monolayer Blown Multilayer Gauge 4-mil 4.5-mil 3.0-mil Layer Material Layer Material Layer Thickness Percentage Resin Density M.I. Thickness Percentage Resin Density M.I. (%) In Layer Type (g/cc) (dg/min) (%) In Layer Type (g/cc) (dg/min) A 100 30 m-h-LLDPE 0.918 1.00 10 60 o-LLDPE 0.920 1.00 COC: COC: 70 6013F-04 1.020 0.90 40 6013F-04 1.020 0.90 B 20 85 o-LLDPE 0.920 1.00 COC: 15 6013F-04 1.020 0.90 C 40 65 HDPE 0.962 1.00 20 o-LLDPE 0.920 1.00 COC: 15 6013F-04 1.020 0.90 B 20 85 o-LLDPE 0.920 1.00 COC: 15 6013F-04 1.020 0.90 A 10 60 o-LLDPE 0.920 1.00 COC: 40 6013F-04 1.020 0.90SPE Polyolefins & FlexPackCon www.topas.com
  8. 8. Test Structures: TOPAS Blends IIID T5: PP / LLDPE+LDPE / PP T12: 36% TOPAS 6015 PP Coex T14: 21% TOPAS 6015 PP Coex T16: 36% TOPAS 5013 PP Coex T18: 21% TOPAS 5013 PP CoexPurpose PP Homopolymer LLDPE/LDPE Coex Without COC High COC Content Coex with PP Low COC Content Coex with PPProcess Cast 3-Layer Cast 5-Layer Cast 5-LayerGauge 6.0-mil 6-mil 6-mil Layer Material Layer Material Layer Material Layer Thickness Percentage Resin Density M.I. Thickness Percentage Resin Density M.I. Thickness Percentage Resin Density M.I. (%) In Layer Type (g/cc) (dg/min) (%) In Layer Type (g/cc) (dg/min) (%) In Layer Type (g/cc) (dg/min) PP PP PP D 20 100 Homopolymer 0.900 8.50 10 100 Homopolymer 0.900 8.50 10 100 Homopolymer 0.900 8.50 B 10 100 o-LLDPE 0.920 1.00 10 100 o-LLDPE 0.920 1.00 A 60 80 o-LLDPE 0.920 1.00 60 35 o-LLDPE 0.923 0.75 60 55 o-LLDPE 0.923 0.75 20 LDPE 0.918 12.00 60 COC 1.02 3.6 / 43 35 COC 1.02 3.6 / 43 5 LDPE 0.918 12.00 10 LDPE 0.918 12.00 B 10 100 o-LLDPE 0.920 1.00 10 100 o-LLDPE 0.920 1.00 PP PP Random PP Random C 20 100 Homopolymer 0.900 8.50 10 100 Copolymer 0.902 6.50 10 100 Copolymer 0.902 6.50SPE Polyolefins & FlexPackCon www.topas.com
  9. 9. Flat Film PropertiesSPE Polyolefins & FlexPackCon www.topas.com
  10. 10. Tensile Strength At Yield (ASTM D882) MD TD 6000 5000 Tensile Yield Strength (psi) 4000 3000 2000 1000 0 T5: PP / T1: TOPAS 6013 T7: T8: T12: 36% T16: 36% T14: 21% T18: 21% LLDPE+LDPE / / LLDPE 4.0 mil 6013+LLDPE & 6013+LLDPE & TOPAS 6015 PP TOPAS 5013 PP TOPAS 6015 PP TOPAS 5013 PP PP 6.0 mil 6013+HDPE 4.5 6013+HDPE 3.0 Coex Coex Coex Coex mil mil COC Improves Film Yield Strength By 50 – 200% Good Balance Between Machine and Transverse Directions (20 IPM)SPE Polyolefins & FlexPackCon www.topas.com
  11. 11. Impact Resistance Film Slow Puncture Slow Puncture Fast Puncture Gauge TOPAS® Break Force Energy to Fast Puncture Total Energy (ft- Film Description (mil) COC (%) (lb) Break (lbf-in) Peak Force (lb) lb) Test Method ASTM F1306-90 ASTM F1306-90 ISO 7765-2 ISO 7765-2 T5: PP / LLDPE+LDPE / PP 6.0 0 9.7 6.9 32.4 1.6 T1: TOPAS 6013 / LLDPE 4.0 70 10.2 1.8 11.8 0.1T7: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 4.5 20 5.4 3.1 17.8 0.6T8: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 3.0 20 3.8 1.5 9.4 0.4 T12: 36% TOPAS 6015 PP Coex 6.0 36 16.9 6.3 25.2 0.8 T16:36% TOPAS 5013 PP Coex 6.0 36 5.1 2.2 26.5 0.3 T14: 21% TOPAS 6015 PP Coex 6.0 21 13.0 6.4 40.5 1.7 T18: 21% TOPAS 5013 PP Coex 6.0 21 11.4 5.4 28.3 0.7 Puncture Resistance Can Be Enhanced By TOPAS COC; Depends On Content & Molecular Weight Lower Percentage Of Higher Molecular Weight COC Improves Puncture ResistanceSPE Polyolefins & FlexPackCon www.topas.com
  12. 12. Tensile Modulus (ASTM D882) MD TD 200,000 180,000 160,000 140,000 odulus (psi) 120,000 100,000 Tensile M 80,000 60,000 40,000 20,000 0 T5: PP / T1: TOPAS 6013 / T7: 6013+LLDPE & T8: 6013+LLDPE & T12: 36% TOPAS T16: 36% TOPAS T14: 21% TOPAS T18: 21% TOPAS LLDPE+LDPE / PP LLDPE 4.0 mil 6013+HDPE 4.5 6013+HDPE 3.0 6015 PP Coex 5013 PP Coex 6015 PP Coex 5013 PP Coex 6.0 mil mil mil COC Improves Film Stiffness By 50 – 200% Good Balance Between Machine and Transverse Directions (20 IPM)SPE Polyolefins & FlexPackCon www.topas.com
  13. 13. Tear Resistance (ASTM D1922) MD TD 3500 3000 2500 T a R s ta c (g m ) e r e is n e ra s 2000 1500 1000 500 0 T5: PP / T1: TOPAS 6013 T7: T8: T12: 36% T16: 36% T14: 21% T18: 21% LLDPE+LDPE / / LLDPE 4.0 mil 6013+LLDPE & 6013+LLDPE & TOPAS 6015 PP TOPAS 5013 PP TOPAS 6015 PP TOPAS 5013 PP PP 6.0 mil 6013+HDPE 4.5 6013+HDPE 3.0 Coex Coex Coex Coex mil mil Ordered Alignment Of COC Domains In Films Reduces Tear Resistance Low Tear Resistance Does Not Imply Poor DurabilitySPE Polyolefins & FlexPackCon www.topas.com
  14. 14. Retort Pouch PreparationSPE Polyolefins & FlexPackCon www.topas.com
  15. 15. Pouch Preparation Lamination ▶ Faustel Pilot Size Laminator ▶ 50 FPM Line Speed ▶ 48 Gauge Corona Treated PET Film Applied to All Untreated Test Films ▶ Retortable Henkel Adhesive (3.0 – 4.0 lb/ream Basis Weight) ▶ Dryer: 150ºF ▶ Nip: 160ºFSPE Polyolefins & FlexPackCon www.topas.com
  16. 16. Pouch Preparation Pouch Fabrication ▶ Pouch Machine: Shanghi Gaoqin Packaging Machinery FSD-600SZ ▶ 100 – 125 4-Side Seal Pouches per Test Film ▶ Size: 5.0 x 7.5 Inches ▶ Bottom Seal: ½-inch ▶ Side Seals: 3/16-inch ▶ Top Seal: 3/8-inchSPE Polyolefins & FlexPackCon www.topas.com
  17. 17. Pouch Preparation Pouch Filling and Sealing ▶ Pouch Filling Machine: Toyo Jidoki Model PMS ▶ Filled With 8 oz Of Water ▶ Pouches Sealed At 140ºC. ▶ PET Removed Prior To RetortSPE Polyolefins & FlexPackCon www.topas.com
  18. 18. Pouch Seal Strength (ASTM F88-05) TOPAS® Bottom Seal Side Seal Gauge Film Description COC (%) (gram/inch) (gram/inch) (mil) Seal Dimension (inch) 0.5000 0.1875 T5: PP / LLDPE+LDPE / PP 0 163 803 6.0 T1: TOPAS 6013 / LLDPE 70 2,765 1,266 4.0T7: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 20 2,200 1,242 4.5T8: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 20 2,916 2,008 3.0 T12: 36% TOPAS 6015 PP Coex 36 1,216 862 6.0 T16: 36% TOPAS 5013 PP Coex 36 1,442 933 6.0 T14: 21% TOPAS 6015 PP Coex 21 1,678 414 6.0 T18: 21% TOPAs 5013 PP Coex 21 1,389 753 6.0 Commercial Retort PET / adh / Foil / adh / Nylon / adh / cast PP 0 3,262 2,963 3.9 All Films Have Excellent Seal Strength COC Enhances Seal StrengthSPE Polyolefins & FlexPackCon www.topas.com
  19. 19. Retort Program: Standard 250ºF Program Temperature Sequence (ºF) Time (Minute) Pressure (psi) 1 220 6 20 2 250 10 30 3 250 60 30 4 220 8 25 5 80 8 25 6 80 20 15 Sudry Model APR-95 Pilot Retort Retort All Pouches In Still Water SpraySPE Polyolefins & FlexPackCon www.topas.com
  20. 20. Pouch Appearance After 250ºF Retort ® TOPAS Seal Gauge Film Description COC (%) Leaks Coloration Appearance (mil) T5: PP / LLDPE+LDPE / PP 0 No leakage Discolored Slight stress on seals 6.0 Holes where water Stress on side and T1: TOPAS 6013 / LLDPE 70 sprayed None botom seals 4.0 T7: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 20 Many leaks Discolored Much stress on seals 4.5 T8: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 20 Many leaks Discolored Much stress on seals 3.0 T12: 36% TOPAS 6015 PP Coex 36 No leakage None Slight stress on seals 6.0 T16: 36% TOPAS 5013 PP Coex 36 No leakage None Slight stress on seals 6.0 T14: 21% TOPAS 6015 PP Coex 21 No leakage None Slight stress on seals 6.0 Stress on side and T18: 21% TOPAS 5013 PP Coex 21 No leakage Discolored at seals botom seals 6.0 Commercial Retort PET / adh / Foil / adh / Nylon / adh / cast PP 0 No leakage None Slight stress on seals 3.9 All PP Coextruded Films Survived 250ºF Retort Films T12 & T18 Were Very Strong After RetortSPE Polyolefins & FlexPackCon www.topas.com
  21. 21. Retort Program: Elevated 260ºF Program Temperature Sequence (ºF) Time (Minute) Pressure (psi) 1 220 4 15 2 250 2 30 3 260 2 30 4 260 60 30 5 200 3 30 6 140 2 25 7 80 2 20 8 80 20 15 Sudry Model APR-95 Pilot Retort Retort All Pouches In Still Water Spray Program Time Reduced From 112 to 95 Minutes Higher Retort Temperatures Increases ProductivitySPE Polyolefins & FlexPackCon www.topas.com
  22. 22. Pouch Appearance After 260ºF Retort TOPAS® Seal Gauge Film Description COC (%) Leaks Coloration Appearance (mil) T5: PP / LLDPE+LDPE / PP 0 No leakage Slight discoloration Stress on seals 6.0 T12: 36% TOPAS 6015 PP Coex 36 No leakage Slight discoloration Stress on seals 6.0 T16: 36% TOPAS 5013 PP Coex 36 No leakage Slight discoloration Stress on seals 6.0 T14: 21% TOPAS 6015 PP Coex 21 No leakage Slight discoloration Stress on seals 6.0 T18: 21% TOPAS 5013 PP Coex 21 No leakage Slight discoloration Stress on seals 6.0 Commercial Retort PET / adh / Foil / adh / Nylon / adh / cast PP 0 No leakage None Slight stress on seals 3.9 Films That Survived 250ºF Retort Were Retorted at 260ºF All Films Tested Survived Retort at 260ºFSPE Polyolefins & FlexPackCon www.topas.com
  23. 23. Retort ResultsSPE Polyolefins & FlexPackCon www.topas.com
  24. 24. Tensile Modulus (ASTM D882) Preretort Post 250 Post 260 200 180 160 140 Tensile Modulus (ksi) 120 100 80 60 40 20 0 T5: PP / T1: TOPAS T7: T8: T12: 36% T14: 21% T16: 36% T18: 21% LLDPE+LDPE 6013 / LLDPE 6013+LLDPE 6013+LLDPE 6015 / PP 6015 / PP 5013 / PP 5013 / PP / PP 6.0 mil 4.0 mil (MD / & 6013+HDPE & 6013+HDPE Coex (MD Coex (MD / Coex (MD / Coex (MD / (MD / TD) TD) 4.5 mil (MD 3.0 mil (MD / /TD) TD) TD) TD) /TD) TD) All Films Show Higher Stiffness Post Retort; Common Phenomenon Higher Stiffness Appears Proportional to COC Content (2 IPM)SPE Polyolefins & FlexPackCon www.topas.com
  25. 25. Tensile Strength (ASTM D882) Preretort Post 250 Post 260 8 7 6 5 Tensile Strength (ksi) 4 3 2 1 0 T5: PP / T1: TOPAS T7: T8: T12: 36% T14: 21% T16: 36% T18: 21% LLDPE+LDPE 6013 / LLDPE 6013+LLDPE 6013+LLDPE 6015 / PP 6015 / PP 5013 / PP 5013 / PP / PP 6.0 mil 4.0 mil (MD / & 6013+HDPE & 6013+HDPE Coex (MD Coex (MD / Coex (MD / Coex (MD / (MD / TD) TD) 4.5 mil (MD 3.0 mil (MD / /TD) TD) TD) TD) /TD) TD) Modest Change of Tensile Strength Post Retort Magnitude of Tensile Strength Is Proportional to COC Content & MW (2 IPM)SPE Polyolefins & FlexPackCon www.topas.com
  26. 26. Yield Elongation (ASTM D882) Preretort Post 250 Post 260 30 25 20 Yield Elongation (%) 15 10 5 0 T5: PP / T1: TOPAS T7: T8: T12: 36% T14: 21% T16: 36% T18: 21% LLDPE+LDPE 6013 / LLDPE 6013+LLDPE 6013+LLDPE 6015 / PP 6015 / PP 5013 / PP 5013 / PP / PP 6.0 mil 4.0 mil (MD / & 6013+HDPE & 6013+HDPE Coex (MD Coex (MD / Coex (MD / Coex (MD / (MD / TD) TD) 4.5 mil (MD 3.0 mil (MD / /TD) TD) TD) TD) /TD) TD) Modest Reduction In Yield Elongation Post Retort Yield Elongation Is More Asymmetric Pre – Vs. Post RetortSPE Polyolefins & FlexPackCon www.topas.com
  27. 27. T5: After & Before Retort / DMA Sample: AL1367-9 Topas multi-L film File: C:TADataDMAQ306AL1367_9.001 Size: 21.5500 x 6.3500 x 0.1500 mm DMA Operator: RTC Method: Topas-Blend-TempSwe Run Date: 05-Jul-2006 07:54 Comment: AL1367-9 Topas multi-L filmm Instrument: 2980 DMA V1.7B 1000 1000 137.89°C 100 ] Storage Modulus (MPa) ] Loss Modulus (MPa) 100 1 ] Tan Delta 10 [ 10 0.1 [ [ 1 1 0.1 30 50 70 90 110 130 150 170 Temperature (°C) Universal V4.1D TA Instruments PP - LLDPE+LDPE - PP Discoloration After Retort At 250ºF High Modulus Retained Over Broad TemperatureSPE Polyolefins & FlexPackCon www.topas.com
  28. 28. T1: After & Before Retort / DMA Sample: AL1367-5 Topas multi-L film File: C:TADataDMAQ306AL1367_5.001 Size: 19.4800 x 6.3500 x 0.1500 mm DMA Operator: RTC Method: Topas-Blend-TempSwe Run Date: 30-Jun-2006 12:35 Comment: AL1367-5 Topas multi-L film Instrument: 2980 DMA V1.7B 1000 100 ] Storage Modulus (MPa) ] Loss Modulus (MPa) 100 1 10 ] Tan Delta [ 10 0.1 1 [ [ 157.25°C 1 0.1 30 50 70 90 110 130 150 170 Temperature (°C) Universal V4.1D TA Instruments 70% 6013 COC + 30% LLDPE Commercial Steam Sterilization Film Softens Gradually Up To Glass Transition TemperatureSPE Polyolefins & FlexPackCon www.topas.com
  29. 29. T7: After & Before Retort / DMA Sample: AL1367-3 Topas blend film File: C:TADataDMAQ306AL1367_3.001 Size: 18.3000 x 6.3500 x 0.1000 mm DMA Operator: RTC Method: Topas-Blend-TempSwe Run Date: 30-Jun-2006 10:52 Comment: AL1367-3 Topas blend film Instrument: 2980 DMA V1.7B 1000 1000 122.80°C 100 ] Storage Modulus (MPa) ] Loss Modulus (MPa) 100 1 ] Tan Delta 10 [ 10 0.1 [ [ 1 1 0.1 30 50 70 90 110 130 150 170 Temperature (°C) Universal V4.1D TA Instruments 5-Layer 6013 / LDPE + 6013 / HDPE Blended Blown Film 4.5-mil, Failed Retort at 250ºF Glass Transition Temperature Occurs at RetortSPE Polyolefins & FlexPackCon www.topas.com
  30. 30. T8: After & Before Retort / DMA Sample: AL1367-4 Topas blend film File: C:TADataDMAQ306Al1367_4.001 Size: 19.9700 x 6.3500 x 0.1000 mm DMA Operator: RTC Method: Topas-Blend-TempSwe Run Date: 30-Jun-2006 11:46 Comment: AL1367-4 Topas blend film Instrument: 2980 DMA V1.7B 1000 1000 108.56°C 100 ] Storage Modulus (MPa) ] Loss Modulus (MPa) 100 1 ] Tan Delta 10 [ 10 0.1 [ [ 1 1 0.1 30 50 70 90 110 130 150 170 Temperature (°C) Universal V4.1D TA Instruments 5-Layer 6013 / LDPE + 6013 / HDPE Blended Blown Film 3.0-mil, Failed Retort at 250ºF Glass Transition Temperature Occurs Significantly Below RetortSPE Polyolefins & FlexPackCon www.topas.com
  31. 31. T12: Before & After Retort / DMA Sample: AL1367-1B Topas blend film File: C:TADataDMAQ306AL1367_1B.001 Size: 23.7900 x 6.3500 x 0.1000 mm DMA Operator: RTC Method: Topas-Blend-TempSwe Run Date: 30-Jun-2006 09:11 Comment: AL1367-1 Topas blend film Instrument: 2980 DMA V1.7B 1000 100 149.45°C ] Storage Modulus (MPa) ] Loss Modulus (MPa) 100 1 10 ] Tan Delta [ 10 0.1 1 [ [ 1 0.1 30 50 70 90 110 130 150 170 Temperature (°C) Universal V4.1D TA Instruments 36% TOPAS 6015 Slight Discoloration, But Excellent Integrity After Retort at 250ºF Stiffer At Much Higher Temperatures vs. TOPAS 5013SPE Polyolefins & FlexPackCon www.topas.com
  32. 32. T16: Pouches Before & After Retort Sample: AL1367-2 Topas blend film File: C:TADataDMAQ306AL1367_2.001 Size: 22.7000 x 6.3500 x 0.1000 mm DMA Operator: RTC Method: Topas-Blend-TempSwe Run Date: 30-Jun-2006 10:00 Comment: AL1367-2 Topas blend film Instrument: 2980 DMA V1.7B 1000 1000 139.37°C 100 ] Storage Modulus (MPa) ] Loss Modulus (MPa) 100 1 ] Tan Delta 10 [ 10 0.1 [ [ 1 1 0.1 30 50 70 90 110 130 150 170 Temperature (°C) Universal V4.1D TA Instruments 36% TOPAS 5013 Good Appearance After Retort At 250ºF. High Modulus Retained Over Broad TemperatureSPE Polyolefins & FlexPackCon www.topas.com
  33. 33. T14: After & Before Retort / DMA Sample: AL1367-10 Topas multi-L film File: C:TADataDMAQ306AL1367_10.001 Size: 18.6100 x 6.3500 x 0.1500 mm DMA Operator: RTC Method: Topas-Blend-TempSwe Run Date: 05-Jul-2006 09:04 Comment: AL1367-10 Topas multi-L film Instrument: 2980 DMA V1.7B 1000 1000 100 ] Storage Modulus (MPa) ] Loss Modulus (MPa) 100 1 124.83°C ] Tan Delta 10 [ 10 0.1 [ [ 1 1 0.1 30 50 70 90 110 130 150 170 Temperature (°C) Universal V4.1D TA Instruments 21% TOPAS 6015 Slight Discoloration, But Excellent Integrity After Retort at 250ºF Stiffer At Higher Temperatures vs. TOPAS 5013SPE Polyolefins & FlexPackCon www.topas.com
  34. 34. T18: Pouches Before & After Retort Sample: AL1367-11 Topas multi-L film File: C:TADataDMAQ306AL1367_11.001 Size: 14.5200 x 6.3500 x 0.1500 mm DMA Operator: RTC Method: Topas-Blend-TempSwe Run Date: 05-Jul-2006 09:49 Comment: AL1367-11 Topas multi-L film Instrument: 2980 DMA V1.7B 1000 1000 100 ] Storage Modulus (MPa) ] Loss Modulus (MPa) 100 1 ] Tan Delta 10 133.63°C [ 10 0.1 [ [ 1 1 0.1 30 50 70 90 110 130 150 170 Temperature (°C) Universal V4.1D TA Instruments 21% TOPAS 5013 Good Appearance After Retort At 250ºF. Package Maintains Integrity & Dimensional Stability.SPE Polyolefins & FlexPackCon www.topas.com
  35. 35. Pouch Burst Test: (ASTM D642-00) TOPAS® COC 250ºF Retort 260ºF Retort Film Description (%) Force (lb) Force (lb) T5: PP / LLDPE+LDPE / PP 0 729 424 T12: 36% TOPAS 6015 PP Coex 36 228 243 T16: 36% TOPAS 5013 PP Coex 36 311 372 T14: 21% TOPAS 6015 PP Coex 21 123 258 T18: 21% TOPAS 5013 PP Coex 21 706 943 Commercial Retort PET / adh / Foil / adh / Nylon / adh / cast PP 0 1,075 1,000 Burst Tester - Lansmont M13710 Pouches Containng COC Had Higher Force After Retorting At 260ºF vs. 250ºF TOPAS 5013 Enhanced Burst Bettter Than TOPAS 6015SPE Polyolefins & FlexPackCon www.topas.com
  36. 36. Gelbo Flex: (ASTM D392-93) Film ® Gauge TOPAS Film Description (mil) COC (%) Pre-Retort 250ºF Retort 260ºF Retort T5: PP / LLDPE+LDPE / PP 6.0 0 No Pinholes No Pinholes Pinholes T1: TOPAS 6013 / LLDPE 4.0 70 Pinholes Pinholes Pinholes T7: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 4.5 20 No Pinholes No Pinholes No Pinholes T8: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 3.0 20 No Pinholes No Pinholes No Pinholes T12: 36% TOPAS 6015 PP Coex 6.0 36 Pinholes No Pinholes No Pinholes T16: 36% TOPAS 5013 PP Coex 6.0 36 Pinholes No Pinholes No Pinholes T14: 21% TOPAS 6015 PP Coex 6.0 21 Pinholes Pinholes Pinholes T18: 21% TOPAS 5013 PP Coex 6.0 21 Pinholes Pinholes Pinholes Commercial Retort PET / adh / Foil / adh / Nylon / adh / cast PP 0 26 No Pinholes Not Tested No Pinholes Gelbo Flex Tester Model 500ES All Samples Flexed At 250 Cycles Pinholes Detected By Penetration Of Red Dye Through Film On To White Background Four COC Coextrueded Films Exhibit Excellent Durability & Flex Crack ResistanceSPE Polyolefins & FlexPackCon www.topas.com
  37. 37. MVTR @ 37.8ºC; 100% R.H. (ASTM F1249-01) Post 250ºF Post 260ºF Pre-Retort Retort MVTR Retort MVTR TOPAS® MVTR (g/100 (g/100 in2 / (g/100 in2 / Film Description COC (%) in2 / day) day) day) T5: PP / LLDPE+LDPE / PP 0 0.157 --- 0.110 T7: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 20 0.211 0.200 0.176 T8: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 20 0.129 --- --- T12: 36% TOPAS 6015 PP Coex 36 0.074 --- 0.053 T16: 36% TOPAS 5013 PP Coex 36 0.071 0.050 --- Commercial Retort PET / adh / Foil / adh / Nylon / adh / cast PP 0 0.019 --- 0.031 Foil Based Commercial Retort Pouches Loses MVTR When Excessively Flexed COC Containing Structures Maintain Good MVTR After Retort COC Containing Structures Can Improve Post Retort MVTR Of Polyolefin FilmSPE Polyolefins & FlexPackCon www.topas.com
  38. 38. OTR @ 37.8ºC; 0% R.H. (ASTM D3985-02) Post 250ºF Post 260ºF Pre-Retort Retort OTR Retort OTR TOPAS® OTR (cc/100 (cc/100 in2 / (cc/100 in2 / Film Description COC (%) in2 / day atm) day atm) day atm) T5: PP / LLDPE+LDPE / PP 0 67 38 --- T7: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 20 71 85 --- T8: 5-Layer 6013 / LLDPE & 6013 / HDPE Blends 20 63 --- --- T12: 36% TOPAS 6015 PP Coex 36 22 --- 15 T16: 36% TOPAS 5013 PP Coex 36 26 35 --- Commercial Retort PET / adh / Foil / adh / Nylon / adh / cast PP 0 26 --- Fail Foil Based Commercial Retort Pouches Loses Barrier When Excessively Flexed COC Containing Structures Maintain Good OTR After Retort COC Containing Structures Can Improve Post Retort OTR Of Polyolefin FilmSPE Polyolefins & FlexPackCon www.topas.com
  39. 39. Summary & ConclusionsSPE Polyolefins & FlexPackCon www.topas.com
  40. 40. Film & Retort Pouch Property Comparative T5: PP / (LLDPE+LDPE) / PP T12: PP / (LLDPE+LDPE+6015) / PP (+) Slow Puncture Force (lb) 250 200 (+) MVTR @ 260ºF Retort (g/100in2 day) ( - ) Slow Puncture Energy (in-lb) 150 100 50 (+) MVTR Pre-Retort (g/100in2 day) 0 (+) MD Tensile Yield (ksi) (+) OTR @ Post Retort (cc/100in2 day atm) (+) TD Tensile Yield (ksi) (+) Glass Transition Temperature (ºC)SPE Polyolefins & FlexPackCon www.topas.com
  41. 41. TOPAS® COC – Conclusions & Benefits TOPAS COC Enhances Stiffness, Dimensional Stability & Package Integrity At Retort Temperatures TOPAS COC Enables Use Of PE, Especially LLDPE, In Retort Applications TOPAS COC Improves Moisture And Oxygen Barrier Properties Of Polyolefins COC Coextruded Structures With PP Are Most Effective TOPAS 6015 (Higher Molecular Weight and Tg) Is More Effective Than TOPAS 5013 For Property Enhancement. TOPAS 6017, Tg = 180ºC, Should Be Included In Future Development ProgramsSPE Polyolefins & FlexPackCon www.topas.com
  42. 42. Acknowledgments TOPAS® Retort Team: Adam Barton, Wolfram Goerlitz, Randy Jester, Tim Kneale, Robert Roschen, Bernd Sparenberg CEFPACK Consortium, Clemson University: Dr. Duncan Darby, Dr. Scott Whiteside & Ms. Pat Marcondes TOPAS® Cyclic Olefin Copolymer (COC) Your Clear Advantage in Retort. Any questions?SPE Polyolefins & FlexPackCon www.topas.com
  43. 43. NOTICE TO USERS: To the best of our knowledge, the information contained in this publication is accurate, however we do not assume any liability whatsoever for the accuracy and completeness of such information. The information contained in this publication should not be construed as a promise or guarantee of specific properties of our products. All technical information and services of TOPAS Advanced Polymers, Inc. are intended for use by persons having skill and experience in the use of such information or service, at their own risk. Further, the analysis techniques included in this publication are often simplifications and, therefore, approximate in nature. More vigorous analysis techniques and prototype testing are strongly recommended to verify satisfactory part performance. Anyone intending to rely on any recommendation or to use any equipment, processing technique or material mentioned in this publication should satisfy themselves that they can meet all applicable safety and health standards. It is the sole responsibility of the users to investigate whether any existing patents are infringed by the use of the materials mentioned in this publication. Properties of molded parts, sheets and films can be influenced by a wide variety of factors including, but not limited to, material selection, additives, part design, processing conditions and environmental exposure. Any determination of the suitability of a particular material and part design for any use contemplated by the user is the sole responsibility of the user. The user must verify that the material, as subsequently processed, meets the requirements of the particular product or use. The user is encouraged to test prototypes or samples of the product under the harshest conditions to be encountered to determine the suitability of the materials. Material data and values included in this publication are either based on testing of laboratory test specimens and represent data that fall within the normal range of properties for natural material or were extracted from various published sources. All are believed to be representative. These values alone do not represent a sufficient basis for any part design and are not intended for use in establishing maximum, minimum, or ranges of values for specification purposes. Colorants or other additives may cause significant variations in data values. We strongly recommend that users seek and adhere to the manufacturer’s current instructions for handling each material they use, and to entrust the handling of such material to adequately trained personnel only. Please call TOPAS Advanced Polymers, Inc. - hotline (859) 746-6447 x4400 for additional technical information. Call Customer Services at (859) 746-6447 x4402 for the appropriate Material Safety Data Sheets (MSDS) before attempting to process our products. Moreover, there is a need to reduce human exposure to many materials to the lowest practical limits in view of possible adverse effects. To the extent that any hazards may have been mentioned in this publication, we neither suggest nor guarantee that such hazards are the only ones that exist. The products mentioned herein are not intended for use in medical or dental implants.SPE Polyolefins & FlexPackCon www.topas.com

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