Producers of Specialty Chemicals Struktol Company of America 1 E. Steels Corners Road P. O. Box 19 Stow, Ohio 9 www.struktol.com High Surface Area Silica in High Performance Tread with Next Generation Struktol Process Additives (STRUKTOL CY 8 and STRUKTOL KK 9) and STRUKTOL SCA 98 (Tetrasulfide) Struktol Rubber Lab Project 9 Part 3 Paul Danilowicz Benny Bezilla Phone: (33) 98188 Fax: (33) 9887 Technical Services: 183789 Email: customerservice@struktol.com
Next Generation Struktol Process Additives STRUKTOL KK 9 Blend of fatty acid derivatives DP C Zn % STRUKTOL CY 8 Blend of fatty acid derivatives DP 97C Zn ~8% 1 High Surface Area Silica in High Performance Tread with Next Generation Struktol Process Additives SCA98 (Tetrasulfide) Struktol Rubber Lab Project 9 Part 3 Paul Danilowicz Benny Bezilla Struktol Company of America 1
Outline Formulations Mix Spec Mix Data Physical Property Data Conclusions 3 Formulations First Pass 1 3 INGREDIENT MASS MASS MASS MASS MASS DURADENE 71B 3. 3. 3. 3. 3. TAKTENE N SCA 98 Tetrasulfide ZN..... ST ACID PPD SUNDEX 79 ZS PMP 7 7 7 7 7 KK 9 CY 8 TOTAL 3 3 3 3 3
Formulations Second Pass 1 3 MB 1 3 MB 3 MB 3 3 MB 3 MB 3 TOTAL 3 3 3 3 3 Formulations Final Pass 1 3 MB 1 3 MB 3 MB 3 3 MB 3 MB 3 DPG..... CBS..... SULFUR 1.7 1.7 1.7 1.7 1.7 TOTAL 3.1.1.1.1.1 3
Mix Spec First Pass mix spec ( rpm, fill factor 7%) SECONDS ADD RUBBER 3 SECONDS ADD 1/3 SILICA SECONDS ADD 1/3 SILICA 9 SECONDS ADD SILANE, OIL, CARBON BLACK, ADDITIVES AND REST OF SILICA 18 SECONDS OR F RAM LIFT 3 SECONDS OR 3F BRUSH AND SWEEP SECONDS OR 3F DISCHARGE ROTOR SPEED RPM AT DISCHARGE 3 PSI nd pass mix spec for batch rotor speed started at 1 rpm, at 3F changed rotor speed to rpm fill factor 7%) SECONDS ADD all MB 3F AUTO RAM LIFT, CHANGE ROTOR SPEED TO RPM DISCHARGE 7 MINUTES AFTER ROTOR SPEED Mix spec final pass for batch ( % fill factor) SECONDS ADD ALL RUBBER 1 SECONDS ADD CURES SECONDS BRUSH AND SWEEP SECONDS OR F DISCHARGE ROTOR SPEED 77 RAM PRESSURE 3 PSI 7 Mixing Observations Temp ( C) Probe Temp(ºC) Energy (WH) First pass comments 1 17.9 77 BATCH (KK 9) phr 1 17.1 33 BATCH 3 (KK 9) phr 1 17. 3 BATCH (CY 8) phr 1 17.1 BATCH (CY 8) phr 1 17. Significant Reduction in mix energy with Struktol Additives 8
Mixing Observations KW 18 1 1 1 8 9 Part 3 Mix Data #1 KW # KW #1 Temp # Temp 1 1 11 181 1 31 Time (Sec.) 18 1 8 Temp. ( C) Mixing Time Reduced with Struktol Additives Mixing Peaks Shifted with Struktol Additives 9 Mixing Observations KW 18 1 1 1 8 9 Part 3 Mix Data #1 KW #3 KW #1 Temp #3 Temp 1 1 11 181 1 31 Time (Sec.) 18 1 8 Temp. ( C) Mixing Time Reduced with Struktol Additives Mixing Peaks Shifted with Struktol Additives
KW 18 1 1 1 8 Mixing Observations 9 Part 3 Mix Data #1 KW # KW #1 Temp # Temp 1 1 11 181 1 31 Time (Sec.) 18 1 8 Temp. ( C) Mixing Time Reduced with Struktol Additives Mixing Peaks Shifted with Struktol Additives 11 KW 18 1 1 1 8 Mixing Observations 9 Part 3 Mix Data #1 KW # KW #1 Temp # Temp 1 1 11 181 1 31 Time (Sec.) 18 1 8 Temp. ( C) Mixing Time Reduced with Struktol Additives Mixing Peaks Shifted with Struktol Additives 1
Mixing Observations Temp ( C) Probe Temp(ºC) Energy (WH) Second pass comments Final pass comments 171 18.1 171 BATCH (KK 9) phr 17 18. 17 BATCH 3 (KK 9) phr 19 17.7 19 BATCH (CY 8) phr 178 18.8 178 BATCH (CY 8) phr 171 178. 171 Rheometer Curves Reduced viscosity and increased cure state with KK 9 1 7
Rheometer Curves Reduced viscosity and increased cure state with CY 8 1 Rheometer Curves 1 8
Rheometer Data 1 C; 3 arc; range; 3 minutes Tech Pro Min Torque Max Torque Ts T T 9 T Reversion.3 71..8.38 11.7 BATCH (KK 9) phr 19.7 79.3 3.9.83 8.. BATCH 3 (KK 9) phr 17.3 79.9. 7. 8.88 8. BATCH (CY 8) phr 19.7 7.17 3.3.17 8.9 BATCH (CY 8) phr 17. 77. 3.83.8 8..7 Increased cure state and reduced minimum torque with KK 9 and CY 8 17 Mooney Viscosity ML (1+) @ C Aged Mooney Initial Viscosity ML (1+) Initial Viscosity 3 day ML (1+) Initial Viscosity 1 day ML (1+) Initial Viscosity 8 day ML (1+) 9. 9.9 19.. 19.3 7.8 MS 1 7. BATCH (KK 9) phr 1. 88. 1.7 9. 1. 9. 171.7 98.9 BATCH 3 (KK 9) phr 11. 8.9. 89.. 88. 1.9 91.7 BATCH (CY 8) phr 1.7 88.1 1.9 98.1 1. 98.9 17.3. BATCH (CY 8) phr 11.7 83.. 91. 1.7 93. 1.7 Decreased viscosity for better processability for KK 9 and CY 8 Better viscosity control with time providing more stable stock storage 9.1 18 9
Mooney Scorch ML @ 1 C Min Torque T T 3 Cure Index 8.8 1. 19.3.7 BATCH (KK 9) phr 81.7.1 3.. BATCH 3 (KK 9) phr 78. 7.9 37. 9.7 BATCH (CY 8) phr 8.1 3.91 3.98 9.7 BATCH (CY 8) phr 81.. 3.78.38 Scorch Safety Doubled with KK 9 CY 8 19 Tensile Data Unaged Cure Time @ 1 C Shore A Duro Tensile (MPa) Elongation (%) % Mod. (MPa) % Mod. (MPa) 3% Mod. (MPa) 17. 38.. 11.9 BATCH (KK 9) phr 7.1 399.8 7.1. BATCH 3 (KK 9) phr 7 19. 1.7. 1. BATCH (CY 8) phr. 379.8 7.7 1.8 BATCH (CY 8) phr. 3.7. 1.3 Increased Tensile, Elong. and Modulus with KK 9 and CY 8
Oven Aged Tensile 7 Hrs @ ºC Sample Shore A Pts. Change Tensile (Mpa) Pct. Change Elong. % Pct. Change % Mod. (Mpa) Pct. Change % Mod. Mpa Pct. change BATCH 1 (Control) 7 11 1.9 1.3 1. 8. 33.3 BATCH (KK 9) phr 77 1.1 9.9 18.9..7 BATCH 3 (KK 9) phr 77 1. 1.1 1.9..7 BATCH (CY 8) phr 7 1 1..3 19 8.3..7 BATCH (CY 8) phr 7 1. 3.7 17 9.9 7. 17.1 Better retention of aged properties with KK 9 and CY 8 1 Tear Strength ASTM D Die C N/MM BATCH (KK 9) phr BATCH 3 (KK 9) phr BATCH (CY 8) phr BATCH (CY 8) phr 3ºC 39..1 7.3 7.8.3 ºC 38.1 8..7.8. Tear Strength better with KK 9 CY 8 11
Heat Build Up lb. Weight;.3 Throw; minute test Cure time 1C Duro Temp.3 BATCH (KK 9) phr 7. BATCH 3 (KK 9) phr 7 9. BATCH (CY 8) phr 8. BATCH (CY 8) phr 7.8 Heat Build Up is equivalent 3 MER Tension/Compression/Cylindrical / 1 HZ COMPOUND BATCH (KK 9) phr BATCH 3 (KK 9) phr BATCH (CY 8) phr BATCH (CY 8) phr Tan delta/ average of 3 / 3c..1.1.1.19 Tan delta/ average of 3 / c.9...98.3 1
Spiral Mold Flow Cured at 1ºC Cure Weight 1 Weight Weight 3 Average Weight 1. 1.8 1.1 1.1 BATCH (KK 9) phr 1.9 1. 1. 1.3 BATCH 3 (KK 9) phr 1.79 1.7 1.98 1.73 BATCH (CY 8) phr 1.7 1.7 1. 1.87 BATCH (CY 8) phr 1.7 1.77 1.7 1.71 Significantly increased flow for better processability with KK 9 and CY 8 Conclusions Struktol Additives KK 9 and CY 8 Reduced mix energy and mix time. Increased cure state. Better scorch resistance. Higher tensile and modulus. Better tear. Reduced viscosity for better processability/ extrudability (less scrap/workaway).