Struktol Rubber Lab. Project January 14, 2004
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1 Producers of Specialty Chemicals Struktol Company of America 201 E. Steels Corners Road P. O. Box 1649 Stow, Ohio Struktol Rubber Lab Project January 14, 2004 Subject: Determine if the efficiency of the cure system influences the activity of STRUKTOL ZB 47 in a NR silica system and N220 black. STRUKTOL SCA 985 was added to both systems. (Ref report 03035) Background: Initial work with ZB 47 was in systems that were with high sulfur and activated high accelerator and sulfur donor. This work looks at a conventional sulfur to accelerator level as well as a low sulfur and high accelerator system. No effort was made to match modulus. The ZB 47 was added with the cure system. No other changes were made in the other chemicals added to the compound. Conclusions: ZB 47 gives a significant reduction in viscosity for both silica and carbon black. The initial viscosity was higher for the CB system; however, the minimum viscosity torque was reduced more with ZB 47 in the silica system. Capillary viscosity for silica at high shear rates shows about a 30% reduction in apparent viscosity. The cure times for silica and carbon black where increased slightly for ZB 47. Reversion times were increased with the ZB 47. The carbon black was much faster curing and slower to revert. The various changes in the cure system reflected mostly in cured torque. Cured modulus shows an increase in state of cure for ZB 47 in both the silica and CB systems. The Firestone blow out data was limited by the softness of the stock and the sample distortion under load. When comparisons could be run, ZB 47 gave significantly longer running times. The general trend in rebound was a slight decrease at room temperature and more rebound at 100C for ZB 47. There was a rough correlation between these trends and the MER tan delta figures. There appears to be no serious change in activity in ZB 47 because of major changes in sulfur to accelerator ratios. Phone: (330) Fax: (330) Technical Services: Internet:
2 Formulae: Silica Ingredient SMR A VN ST. ACID ZNO TIO SUNOLITE PLURIOL NS WB STANPLAST SCA TMQ TOTAL: Note: 70 % fill factor, Cure was added to the second pass SULFUR MBS DPG VANAX A TBBS ZB Project Page 2
3 Formulae: N220 Ingredient SMR A N ST. ACID ZINC OXIDE TIO SUNOLITE PLUURIOL NS WB STANPLAST SCA TMQ TOTAL: Note: 70 % fill factor Cure was added in the second pass SULFUR MBS DPG VANAX A TBBS ZB Project Page 3
4 First Pass Compound Temperature ( C) Energy (WH) #1 2S, 3 Acc #2 ZB #3 2S, 1 Acc #4 ZB #5 1.5 S, 1.5 S #6 ZB #7 1 S, 2 Acc #8 ZB #9 2 S, 3 Acc #10 ZB #11 2 S, 1 Acc #12 ZB # S, 1.5 S #14 ZB # S, 2 Acc #16 ZB Rheometer Data: 160 C; 3 arc; 100 Range; 60 minutes Min Max T-2 Ts Torque Torque 2 T 50 T 90 reversion #1 2S, 3 Acc #2 ZB #3 2S, 1 Acc #4 ZB #5 1.5 S, 1.5 S #6 ZB #7 1 S, 2 Acc #8 ZB #9 2 S, 3 Acc #10 ZB >60 #11 2 S, 1 Acc #12 ZB # S, 1.5 S >60 #14 ZB # S, 2 Acc >60 #16 ZB >60 Project Page 4
5 Mooney Viscosity ML 100 C Initial Viscosity ML (1+4) #1 2S, 3 Acc #2 ZB #3 2S, 1 Acc #4 ZB #5 1.5 S, 1.5 S #6 ZB #7 1 S, 2 Acc #8 ZB #9 2 S, 3 Acc #10 ZB #11 2 S, 1 Acc #12 ZB # S, 1.5 S #14 ZB # S, 2 Acc #16 ZB Mooney Scorch 125 C Min Torque T 5 T 35 Cure Index #1 2S, 3 Acc #2 ZB #3 2S, 1 Acc #4 ZB >90 - #5 1.5 S, 1.5 S #6 ZB #7 1 S, 2 Acc #8 ZB #9 2 S, 3 Acc #10 ZB #11 2 S, 1 Acc #12 ZB # S, 1.5 S #14 ZB # S, 2 Acc #16 ZB Project Page 5
6 Sample Cure time (min) 160c Shore A Duro Tensile Data Unaged Tensile (MPa) Elongation (%) 100% Mod. (MPa) 200% Mod. (MPa) 300% Mod (MPA) #1 2S, 3 Acc #2 ZB #3 2S, 1 Acc #4 ZB #5 1.5 S, 1.5 S #6 ZB #7 1 S, 2 Acc #8 ZB #9 2 S, 3 Acc #10 ZB #11 2 S, 1 Acc #12 ZB # S, 1.5 S #14 ZB # S, 2 Acc #16 ZB Blow Out 550 lb. Weight; Throw; test until blow out. Sample Cure 160 C Durometer BLOW OUT #1 2S, 3 Acc MIN #2 ZB HRS 38 MIN #3 2S, 1 Acc WILL NOT RUN #4 ZB WILL NOT RUN #5 1.5 S, 1.5 S WILL NOT RUN #6 ZB WILL NOT RUN #7 1 S, 2 Acc WILL NOT RUN #8 ZB WILL NOT RUN #9 2 S, 3 Acc HRS 55 MIN #10 ZB HRS 14 MIN #11 2 S, 1 Acc WILL NOT RUN #12 ZB MIN # S, 1.5 S MIN #14 ZB MIN # S, 2 Acc MIN #16 ZB MIN Project Page 6
7 Rebound 0 DEGREES ROOM TEMP 100C #1 2S, 3 Acc #2 ZB #3 2S, 1 Acc #4 ZB #5 1.5 S, 1.5 S #6 ZB #7 1 S, 2 Acc #8 ZB #9 2 S, 3 Acc #10 ZB #11 2 S, 1 Acc #12 ZB # S, 1.5 S #14 ZB # S, 2 Acc #16 ZB Sample Tan delta / *room temp Mer: /Compression / Cylindrical 10 HZ Cmplx power *room temp Loss power *room temp Stiffness *room temp Tan delta / 100c Cmplx power *100c Loss power *100c Stiffness *100c #1 2S, 3 Acc #2 ZB #3 2S, 1 Acc #4 ZB #5 1.5 S, 1.5 S #6 ZB #7 1 S, 2 Acc #8 ZB #9 2 S, 3 Acc #10 ZB #11 2 S, 1 Acc #12 ZB # S, 1.5 S #14 ZB # S, 2 Acc #16 ZB Tan Delta is the average of 3 samples, each stock Cure time 160c Project Page 7
8 Capillary Rheometer Data 100C, 189 sec preheat Die L/D ratio: 15:1: 90 entrance angle: 1.5 mm orifice Apparent Stress (Pa) Apparent Viscosity (Pa-s) Apparent Stress (Pa) Apparent Viscosity (Pa-s) Shear rate 500/s 500/s 1000/s 1000/s #1 2S, 3 Acc 230, #2 ZB 163, #3 2S, 1 Acc 271, #4 ZB 182, #5 1.5 S, 1.5 S 253, #6 ZB 176, #7 1 S, 2 Acc 255, #8 ZB 181, Note: Capillary was run only on batches 1 thru 8. The scorch delay of 9-16 was marginal for viscosity testing; capillary testing was not run. Project Page 8
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