Improved Aging Characteristics of Crosslinked Polymer Modified Asphalt Binders

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1 Improved Aging Characteristics of Crosslinked Polymer Modified Asphalt Binders Petersen Asphalt Research Conference Thirty-Seventh Annual Meeting July17-19, 2000 Laramie, WY Presented by Dennis Krivohlavek Andres Rangel TexPar Laboratories, Claremore, OK

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3 Project Objectives Examine Data from Typical Road Formulations Examine Data from Typical Shingle Formulation

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5 Project Objectives Examine Data from Typical Road Formulations Rolling Thin Film Oven Test Pressure Aging Vessel Long Term Heated Storage Properties

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7 Project Objectives Examine Data from Typical Shingle Formulations Physical Test Data Weathering

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9 Test Protocol to Generate Data for Typical Road Formulations

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11 Rolling Thin Film Oven Test RTFOT DSR on RTFOT BBR on RTFOT

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13 Pressure Aging Vessel PAV DSR on PAV BBR on PAV

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15 Long Term Heated Storage Properties Sample Stored at 325 F Sample Tested Weekly Test Parameter - Elastic Recovery

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17 Typical Road Formulation Starting Asphalt = PG (actual) SBS = 3.0% by Weight Linear Structure 30% by Weight Styrene About 110,000 Molecular Weight Cross-linking Agent = 0.10% by Weight

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19 Critical Passing Temp., C G*/sind Critical Passing Temperature of ORIGINAL and RTFOT Original RTFOT No X-link YES X-link

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21 Critical Passing Temp., C BBR S-Value Critical Passing Temperature of PAV and RTFOT -26 RTFOT PAV No X-link Yes X-link

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23 Critical Passing Temp., C BBR m-value Critical Passing Temperature of PAV and RTFOT 0 RTF OT PAV No X-link Yes X-link

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25 Long Term Heated Storage Elastic Recovery Test Protocol Pull Rate = 5cm/min Elongation = 20cm Relaxation time = 5 minutes Test Temperature = 10 C Read Final Value (cm) at 60 minutes %ER = ((20-Final Value)/20)x100

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27 Formulation for Long Term Storage Testing Starting Asphalt = PG (actual) Two Levels of Cross-Linking Agent 0.10% by Weight 0.20% by Weight SBS = 0.50% by Weight Radial Structure 25% by Weight Styrene About 130,000 Molecular Weight

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29 Percent Elastic Recovery Elastic Recovery Over Time % X- link 0.20% X- link wk 1 wk 2 wk 3 wk 4 wk Number of Weeks Stored at 325 F

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31 Test Protocol for Typical Shingle Formulations

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33 Physical Tests on Formulations R&B Softening Point 4 C & 25 C Brookfield Viscosity PAV Cold Temperature Mandrel Bend Test Weathering

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35 Ring & Ball Softening Point R&B Soft Point by ASTM D 36 R&B Soft Point on Formulation As Mixed PAV (at 30hrs) Residue

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37 Penetration Penetration by ASTM D 5 Penetration, 4 C, 200g, 60s, on Formulation As Mixed PAV (at 30hrs) Residue Penetration, 25 C, 100g, 5s, on Formulation As Mixed PAV (at 30Hrs) Residue

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39 Rotational Viscosity Brookfield Viscometer by ASTM D 4402 Test Temperature = 375 F Rotational Viscosity run on Formulation As Mixed PAV (at 30hrs) Residue

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41 Pressure Aging Vessel PAV run for 30hrs on Formulation Including Filler in Formula Ring & Ball Softening Point Penetration at 4 C & 25 C

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43 Weathering Spark Test - Failure End Point in Accelerated and Outdoor Weathering of Bituminous Materials by ASTM D 1670 Artificial = Xenon Arc by ASTM D 4798 Outdoor = Panel Exposure at Tampa, FL

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45 Weathering Test Protocol Spark Test Cold Temperature Mandrel Bend Test Weathering Sample Panel Observation Weathering Sample Panel Preparation by ASTM D 1669

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47 Spark Test ASTM D-1670 Artificial = Xenon Arc by ASTM D 4798 Outdoor = Panel Exposure at Tampa, FL

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49 Cold Temperature Mandrel Bend Test Bar size = 1 x 4 x 1/8 Mandrel = 1 Diameter Bend Rate = 2 Seconds Bars per Formula = 5 Pass Criterion = 4 of 5 Bars at Temp

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51 Sample Panel Observation Observations on Xenon Arc and Outside Panels Performed at: 500hrs 1,000hrs 1,500hrs 2000hrs 2,500hrs 3,000hrs 3,500hrs 4,000hrs

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53 Shingle Mixing Procedure Asphalt and Polymer High Shear Mixed at 375 F Until Polymer Digested (about 2hrs) Cross-link added and Reacted for Four Hour (4hr) Minimum Filler Added - Mixed Until Homogeneous or about 15 to 30 Minutes Material Tested

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55 Shingle Formulations Formula D-N D-Y R-N R-Y A C Diblock SBS Radial SBS Cross-link % Filler Above Blend

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57 Physical Test Data As Mixed Test D-N D-Y R-N R-Y Soft Pt, F Pen, 4 C Pen, 25 C B-Visc, cps 5,375 6,877 6,600 3,875

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59 Viscosity, cps at 375 F Brookfield Viscosity of Formulations As Mixed D-N D-Y R-N R-Y

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61 Physical Test Data from PAV Test D-N D-Y R-N R-Y Soft Pt, F Pen, 4 C Pen, 25 C

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63 Diblock SBS Cold Temperature Mandrel Bend Test Sample, F D-N D-Y As Mixed PAV

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65 Temperature at Failuer, F Diblock SBS Cold Temperature Mandrel Bend Test D-N D-Y As Mixed PAV

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67 Radial SBS Cold Temperature Mandrel Bend Test Sample, F R-N R-Y As Mixed PAV 70 40

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69 Temperature at Failuer, F Radial SBS Cold Temperature Mandrel Bend Test D-N D-Y As Mixed PAV

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71 Weathering Observations on Test Panels

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73 Formula D-N Spark Test Results at 2,500 Hours Sample Failure at >26 Grids with Sparkthrough Points

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75 Formula D-Y Spark Test Results at 2,500 Hours

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77 Formula R-N Spark Test Results at 2,500 Hours

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79 Formula R-Y Spark Test Results at 2,500 Hours

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81 Sample Panel Observation Values Value Observation Description 1 Severe Alligatoring 2 Moderate-to-Severe Alligatoring 3 Moderate Alligatoring 4 Slight Cracking 5 Moderate Crazing 6 Light Crazing 7 Slight Crazing 8 No Crazing

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83 Outside Panels Ranked by Observation Over Time Khrs 0.5Khrs 1.0Khrs 1.5Khrs 2.0Khrs 2.5Khrs 3.0Khrs 3.5Khrs D-N D-Y R-N R-Y

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85 Xenon Arc Panels Ranked by Observation Over Time Khrs 0.5Khrs 1.0Khrs 1.5Khrs 2.0Khrs 2.5Khrs D-N D-Y R-N R-Y

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87 Formula D-N Xenon Arc Results at 2,500 Hours

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89 Formula D-Y Xenon Arc Results at 2,500 Hours

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91 Formula R-N Xenon Arc Results at 2,500 Hours

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93 Formula R-Y Xenon Arc Results at 2,500 Hours

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95 Conclusions - Road In Typical Road Formulations, Aging May Be Improved by the use of Cross-linking Agents Better Retention of Elastic Recovery Reduced Aging under RTFOT Conditions Greatly Improved Temperature Results under Both RTFOT and PAV

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97 Conclusions - Roofing In Typical Roof Shingle Formulations, Aging and Weathering Show Improvement by the use of Cross-linking Agents Maintained Softening Point at Reduced Polymer Loading Significantly Lower Failure Temperature on Mandrel Test

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99 Conclusions - Roofing continued Resistance to Xenon Arc Weathering Significantly Improved Outdoor Weathering Shows Similar Trends; Test Still in Progress

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101 Acknowledgments Ken Grzybowski and PRI Asphalt Technologies for Their Test Work, Professional Support and Guidance Terry Arnold, Dale Kelly and Henry Romagosa for Their Assistance and Review Richard Ziesmer and Ysabel DaCosta for Their Efforts in Generating Data WRI and the Petersen Asphalt Research Conference for Allowing the Authors to Present Our Data

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