Producer of Specialty Chemical Struktol Company of America 201 E. Steel Corner Road P. O. Box 1649 Stow, Ohio 44224-0649 Struktol Rubber Lab December 19, 2003 Subject: To ee if activity of STRUKTOL ZB 47 change by the addition of ol SBR or carbon black to a NR, ilane, ilica tock. Submitted by: JVK- Ref. Exp. 01016. Concluion: The addition of either SBR or carbon black did not influence the activity. ZB 47 give ignificant improvement in mixing, vicoity and cured phyical a well a dynamic improvement in rebound, heat build up and evere load ditortion. Although the control reference tock how reverion, there wa little effect on over cure. ZB 47 tended to cure to a higher tate of cure. The cure ytem i a high accelerator, ulfur donor emi EV and ZB 47 make it ignificantly more effective Phone: (330) 928-5188 Fax: (330) 928-8726 Technical Service: 1-800-327-8649 Internet: www.truktol.com
Formulae: Ingredient NR NR-ZB47 NR-SBR NR-SBR- ZB47 NR-N330 NR- N330- ZB47 SMR 5 100 100 80 80 100 100 Duradene 740 0 0 20 20 0 0 A86 0.25.25.25.25.25.25 VN-3 57 57 57 57 57 57 N330 0 0 0 0 15 15 Stearic acid 2 2 2 2 2 2 Zinc oxide 4 4 4 4 4 4 TiO2 5 5 5 5 5 5 Sunolite 240 1.25 1.25 1.25 1.25 1.25 1.25 Pluriol 4000 1 1 1 1 1 1 60NS 3.5 3.5 3.5 3.5 3.5 3.5 WB-222 2 2 2 2 2 2 Stan pla 2000 4 4 4 4 4 4 SCA 985 2.5 2.5 2.5 2.5 2.5 2.5 ZB-47 0 5 0 5 0 5 TMQ 1 1 1 1 1 1 TOTAL: 183.50 188.50 183.50 188.50 183.50 188.50 Note: Firt pa: The rubber wa added with the A86 and prepeptizied for 30 econd, then the ret of the ingredient were added to the firt pa. The cure package wa added in the econd pa: Sulfur 2 phr, MBS 2 phr, DPG -.5 phr., DTDM -.5 phr Note: fill factor 70% - 70 rpm 4 minute Firt Pa Compound Temperature ( C) Energy (WH) NR 114 163 NR-ZB47 123 174 NR-SBR 144 203 NR-SBR-ZB47 133 184 NR-N330 143 201 NR-N330-ZB47 131 174 Page2
03035 MIX DATA NR - SILICA 10.0 350 Energy (KW) 8.0 6.0 4.0 2.0 300 250 200 150 100 50 Temp. ( F) Control - KW ZB-47 - KW Control - Temp. ZB-47 - Temp. 0.0 1 61 121 181 241 0 Time (ec) 03035 MIX DATA NR - SBR - SILICA Energy (KW) 10.0 9.0 8.0 7.0 6.0 5.0 4.0 3.0 2.0 1.0 0.0 1 61 121 181 241 Time (ec) 350 300 250 200 150 100 50 0 Temp. ( F) Control - KW ZB-47 - KW Control - Temp. ZB-47 - Temp. 03035 MIX DATA NR - SILICIA - BLACK 10.0 350 Energy (KW) 9.0 8.0 7.0 6.0 5.0 4.0 3.0 2.0 1.0 300 250 200 150 100 50 Temp. ( F) Control - KW ZB-47 - KW Control - Temp. ZB-47 - Temp. 0.0 1 61 121 181 241 0 Time (ec) Page3
Rheometer Data: 160 C; 3 arc; 100 Range; 60 minute Min Max Torque Torque T 2 T 50 T 90 T-2 reverion NR 18.88 84.62 4.92 7.50 8.75 14.17 NR-ZB47 8.45 84.94 5.17 9.25 10.83 29.58 NR-SBR 18.05 86.86 5.42 8.75 10.25 20.50 NR-SBR-ZB47 9.15 84.69 5.92 10.75 12.58 44.25 NR-N330 14.40 84.37 3.83 7.08 8.17 15.50 NR-N330-ZB47 11.39 87.69 3.67 6.67 8.33 35.67 Mooney Vicoity ML (1+4) @ 100 C Initial Vicoity ML (1+4) NR 78.5 67.2 NR-ZB47 56.0 43.4 NR-SBR 74.0 62.6 NR-SBR-ZB47 62.9 47.6 NR-N330 80.4 60.9 NR-N330-ZB47 70.0 55.0 Mooney Scorch ML @ 125 C Min Torque T 5 T 35 Cure Index NR 50.3 40.29 51.39 11.1 NR-ZB47 33.3 43.10 - - NR-SBR 50.7 49.65 - - NR-SBR-ZB47 34.5 49.67 - - NR-N330 50.9 25.34 43.94 18.6 NR-N330-ZB47 44.7 23.72 32.59 8.87 Page4
Tenile Data Unaged Sample Cure time (min) Shore A Duro Tenile Elongation (%) 100% 200% 300% (MPA) NR 11/160c 72 25.5 623 2.2 4.7 8.2 NR-ZB47 11/160c 72 24.9 595 3.0 6.1 10.0 NR-SBR 11/160c 72 24.1 628 2.2 4.5 7.7 NR-SBR-ZB47 13/160c 74 23.3 585 2.9 5.9 9.4 NR-N330 8/160c 68 25.5 596 2.4 5.7 10.3 NR-N330-ZB47 8/160c 68 26.2 604 2.7 6.1 10.5 Tenile Data Unaged 4X overcure Sample Cure time (min) Shore A Duro Tenile Elongation (%) 100% 200% 300% (MPA) NR 44/160c 74 25.9 632 2.2 4.8 8.6 NR-ZB47 44/160c 74 25.4 547 3.0 6.6 11.4 NR-SBR 44/160c 73 24.1 619 2.2 4.6 8.3 NR-SBR-ZB47 52/160c 75 22.5 543 2.7 5.8 10.0 NR-N330 32/160c 72 25.0 556 2.6 6.1 11.0 NR-N330-ZB47 32/160c 71 24.8 485 3.1 7.7 13.7 Page5
Firetone Flexometer Blow Out 550 lb. Weight; 0.325 Throw; tet till it blow Sample Hardne Minute NR 66 18 min NR-ZB47 68 7 hour 20 min NR-SBR 66 39 min NR-SBR-ZB47 72 10 hour 35 min NR-N330 65 3 hour 16 min NR-N330-ZB47 68 115 hour 36 min Firetone Flexometer Build Up 250 lb. Weight; 0.325 Throw; 45-minute tet Sample Hardne Temp NR 66 112.5C NR-ZB47 68 101.5c NR-SBR 66 114.7C NR-SBR-ZB47 72 109.9C NR-N330 65 98.6C NR-N330-ZB47 68 89.1C Page6
Button were cured a follow: 1-22/320, 2 22/320, 3 22/320, 4-26/320, 5 16/320, 6 16/320 Rebound room temp Sample Tet 1 Tet 2 NR 41 41 NR-ZB47 36 37 NR-SBR 41 39 NR-SBR-ZB47 36 35 NR-N330 42 41 NR-N330-ZB47 41 41 Rebound 0 C Sample Tet 1 Tet 2 NR 18 16 NR-ZB47 18 12 NR-SBR 17 12 NR-SBR-ZB47 15 15 NR-N330 21 18 NR-N330-ZB47 17 17 Rebound 100 C Sample Tet 1 Tet 2 NR 56 52 NR-ZB47 59 57 NR-SBR 58 56 NR-SBR-ZB47 57 57 NR-N330 62 61 NR-N330-ZB47 65 62 Page 7
Producer of Specialty Chemical Struktol Company of America 201 E. Steel Corner Road P. O. Box 1649 Stow, Ohio 44224-0649 Struktol Rubber Lab (addendum) January 29, 2004 Subject: Background: Volume well i ometime ued to meaure crolink denity. In thi experiment cured ample were expoed to 1-week toluene olvent well at room temperature. Chemical probing wa done uing a reducing agent, which hould cleave polyulfide bond. The reducing agent Red-Al (Ficher) i available a a toluene olution. It wa diluted to 10% in dry toluene and freh reducing agent wa added once during the week aging. Concluion: ZB 47 influence the nature of the crolink. Significant reduction in welling occur by the addition of ZB 47 to thee compound. The reducing agent caue a large increae in well becaue of the cleavage of polyulfide bond. A expected over cure how a reduction in well which how that the crolink type change with time. SBR addition appear to change ome of the crolink ditribution on over cure more than the addition of carbon black. The improvement in crolink denity ugget that improved reaction of the ilane coupling agent to the rubber are taking place but thi experiment doe not prove that. There could alo be change to the tandard rubber-to-rubber crolink. Whether agent reduce all S-S bond i unknown. Note: When the tock well to about 1000% it i too flimy to meaure volume change. The weight increae for the 1x cure NR-ZB 47 ytem i in quetion. By: Dr. John Vander Kooi Phone: (330) 928-5188 Fax: (330) 928-8726 Technical Service: 1-800-327-8649 Internet: www.truktol.com
% Volume Swell 1X and 4X Cure No Reducing Agent 180.00 160.00 140.00 1X Cure 4X Cure 120.00 100.00 % 80.00 60.00 40.00 20.00 0.00 NR NR/ZB47 NR/SBR NR/SBR/ZB47 NR/CB NR/CB/ZB47 Figure 1 % 1200.00 1000.00 800.00 600.00 400.00 Toluene Toluene/Red Al D i o l v e d % Volume Swell 1X Cure Too Soft To Meaure D i o l v e d 200.00 0.00 NR NR/ZB47 NR/SBR NR/SBR/ZB47 NR/CB NR/CB/ZB47 Figure 2 Page 9
% Weight Gain 1X Cure 1200.00 Toluene 1000.00 Toluene/Red Al % 800.00 600.00 400.00 200.00 D i o l v e d D i o l v e d 0.00 NR NR/ZB47 NR/SBR NR/SBR/ZB47 NR/CB NR/CB/ZB47 Figure 3 600.00 500.00 Toluene Toluene/Red Al % Volume Swell 4X Cure 400.00 % 300.00 200.00 100.00 0.00 NR NR/ZB47 NR/SBR NR/SBR/ZB47 NR/CB NR/CB/ZB47 Figure 4 Page 10
700.00 600.00 Toluene Toluene/Red Al % Weight Increae 4X Cure % 500.00 400.00 300.00 200.00 100.00 0.00 NR NR/ZB47 NR/SBR NR/SBR/ZB47 NR/CB NR/CB/ZB47 Figure 5 Page 11