Review Of Rubber Mixing Effect On Polymer / Compound .
Review of Rubber Mixing&Effect on Polymer / CompoundPerformanceERIF 2017Vienna: 10. – 11. May
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionFormulaFormpro ingcessgnisxMi cesoprRaw materialsorvi alsh a e ribe te maTh wraofin Chth a nof e p gem ro si x cein sg sReview of MixingEffectson the processDr. Hans-Joachim Graf2
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusion Mixing gives reason to changes of ingredients and ofreactions between the ingredients Mixer behaves like a reactor In addition to mechanical work on distribution and dispersion Polymer Changes MW, MWD and LCB Radical reactions of polymer with Carbon Black Protection / Processing Aids Ingredients with functional groups reacting with polymer Acid / Base ReactionsDr. Hans-Joachim Graf3
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of Mixing MixingUS 2820836 AWhat is the goal of Mixing? Compound, which can beprocessed in the desiredmachines, turned into a part,which meets customerexpectations Viscosity of compound –processing Dispersion of Filler – physicalproperties Homogeneity Rheology – Cure kineticDr. Hans-Joachim Graf4
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of Mixing MixingWhat is the conflict in Mixing? Viscosity of compound: Viscosity correlates to MW:Performance – Higher is betterProcessing – Lower is better: IMHigher is better: CM, Extrusion Dispersion of Fillers Temperature rise through highshear correlates to: PolymerType / MWLoadingOil / FillerFillerType / SizeMW ( Type of Polymer),Filler (Type) / Oil loading Rheology – Cure kineticDr. Hans-Joachim Graf5
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Nijmann Vredestein Mixing Diagram Information Ram DownMixer under filledMasticationDr. Hans-Joachim GrafRam Down / Up / DownMixer slightly under filledMixing Oil injection6
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: Thesis Ebell Process factorsin order of importance Mixing Time or Mixing Unit Work Rotor Speed Mixer Temperature Ram Pressure Fill Factor (not independent from Ram Pressure)Dr. Hans-Joachim Graf7
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Sommer, R Handbook Mixing / molecular weightchange MW of different NRTypes coagulated andstabilized Bimodal MWdistribution MWD of 5 - 10Log M Mastication on Mill ofSMR 20 MW decreases Bimodal MWdistribution becomes abroad MWDr. Hans-Joachim Graf8
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusion Mixing of SBR:Dr. Hans-Joachim GrafSource: Thesis Ebell*)*) other factors neglected
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusion Mixing of SBR:Tensile strength (MPa)Dependence of physical properties on Mooneyviscosity of masticated SBR rubber and ontemperature of mastication.252322120 C160 C190 C21Mooney Viscosity (Mooney Units)Dr. Hans-Joachim GrafSource: Martin, RCT 1955Fig left: Thesis Ebell
Review of Mixing Mixing of SBR:Dr. Hans-Joachim GrafIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: Ebel, Thesis
Review of Mixing Mixing of SBR:Dr. Hans-Joachim GrafIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: Ebel, Thesis
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Ebel, Thesis Mixing of SBR: Mix Time over Unit Work & Rotor Speed Ram pressure 0.22 (left)- 0.80 (right)Design-Expert SoftwareFactor Coding: ActualOriginal Scale(median estimates)Mix TimeDesign points above predicted valueDesign points below predicted value453.8975.30500.00Actual FactorsC: Fill Factor 0.80D: Ram Pressure 0.40E: Temp Mixer 50.00300.00200.00100.0075.0069.0063.0057.0051.00B: Rotor SpeedDr. Hans-Joachim Graf1200.001125.001050.00975.00900.00825.00A: Unit Work750.00675.0045.00 600.00400.00Mix Time400.00Mix Time500.00X1 A: Unit WorkX2 B: Rotor Speed300.00200.00100.0075.0069.0063.0057.0051.00B: Rotor Speed1200.001125.001050.00975.00900.00825.00A: Unit Work750.00675.0045.00 600.00
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Ebel, Thesis Mixing of SBR: Dump Temperature over Unit Work & Rotor Speed Ram pressure 0.22 (left)- 0.80 (right)Design-Expert SoftwareCoding: ActualDumpTempFactorDump Temp75.00DumpTemp75.00150Design Points16992B: Rotor SpeedB: Rotor Speed14569.00X1 A: Unit WorkX2 B: Rotor Speed63.00135130Actual Factors140C: Fill Factor 0.80D: Ram Pressure 0.40E: Temp Mixer 45.0045.00600.00675.00750.00825.00900.00A: Unit WorkDr. Hans-Joachim 25.00900.00A: Unit Work975.001050.001125.001200.00
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Ebel, Thesis Mixing of SBR: Tensile over Unit Work & Rotor Speed Ram pressure 0.22 (left)- 0.80 (right)Design-Expert SoftwareTensileFactor Coding: Actual75.004.479.00X1 A: Unit WorkX2 B: Rotor Speed63.007.0010.0069.00B: Rotor SpeedB: Rotor Speed69.00Tensile75.00TensileDesign Points12.40Actual FactorsC: Fill Factor 0.808.00D: Ram Pressure 0.40E: Temp Mixer 45.0045.00600.00675.00750.00825.00900.00A: Unit WorkDr. Hans-Joachim 25.00900.00A: Unit Work975.001050.001125.001200.00
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Ebel, Thesis Mixing of SBR: Tensile: Predicted versus Actual (left) Mooney Viscosity: Predicted versus Actual (right)Design-Expert Software1/Sqrt(Tensile 0.50)Design-Expert SoftwareMooney ViscPredicted vs. ActualColor points by value of1/Sqrt(Tensile 0.50):0.45Predicted vs. ActualColor points by value ofTemp alDr. Hans-Joachim Graf0.400.4523250.0060.0070.00Actual80.0090.00
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: Ebel, ThesisDesign-Expert SoftwareFactor Coding: ActualOriginal Scale(median estimates)Overlay PlotX1 A: Unit WorkX2 B: Rotor SpeedActual FactorsC: Fill Factor 0.80D: Ram Pressure 0.40E: Temp Mixer 069.00B: Rotor SpeedMix TimeDump TempMooney ViscTensileDesign 75.001050.001125.001200.00A: Unit Work Mixing of SBR: Unit Work over Rotor Speed Tensile at 10.3 MPa (max. value) Mixing time 210 – 230 sec Mooney viscosity ML(1 4) 100 C: 65 – 67 Mooney UnitsDr. Hans-Joachim Graf
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingDesign-Expert SoftwareFactor Coding: ActualML(1 4)100Design points above predicted valueDesign points below predicted value62Source: Kreuzwieser, ThesisDesign-Expert SoftwareFactor Coding: ActualML(1 4)100Design points above predicted valueDesign points below predicted value6245456560ML(1 4)100Actual FactorA: Mastication 30.0065X1 B: mixingX2 C: rotor speedActual FactorA: Mastication : rotor speed4.1041.0035.0060ML(1 4)100X1 B: mixingX2 C: rotor : mixing3.50C: rotor speed4.1041.0035.003.50 Mixing of NR/SBR/BR: Ml(1 4)100 C over Mixing Time & Rotor Speed Mastication time 30 sec (left)70 sec (right)Dr. Hans-Joachim GrafB: mixing
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Kreuzwieser, ThesisDesign-Expert SoftwareFactor Coding: ActualE spec. MixingDesign points above predicted valueDesign points below predicted value571Specific Mixing Energy over Mooney Ml(1 4)100 C600600179X1 B: mixingX2 C: rotor speed40030020010065.0059.0053.0047.00C: rotor speed41.0035.003.504.104.705.305.906.50B: mixingSpecific Energy [Wh/kg]500E spec. MixingActual FactorA: Mastication 50.00Ml(1 4) vs E spec Mix500400300200100444648505254565860Mooney - ML(1 4)100 C [MU] Mixing of NR/SBR/BR: Specific Energy Mix over Mixing Time & Rotor Speed (left) Correlation of Mooney with Specific Energy Mix (right)Dr. Hans-Joachim Graf6264
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Kreuzwieser, ThesisDesign-Expert SoftwareFactor Coding: ActualExtr PressDesign points above predicted valueDesign points below predicted value84Design-Expert SoftwareFactor Coding: ActualExtr 50rpm 100 CDesign points above predicted valueDesign points below predicted value584460605580Actual FactorA: Mastication .00C: rotor speed41.004.1065.006.5059.005.9053.004.7035.00 85X1 B: mixingX2 C: rotor speedExtr PressActual FactorA: Mastication 50.00Extr 50rpm 100 CX1 B: mixingX2 C: rotor speedB: mixing3.505.3047.00C: rotor speed4.7041.00B: mixing4.1035.003.50Mixing of NR/SBR/BR: Extrusion over Mixing Time & Rotor Speed Extruder Output at 50 rpm is invariant towards head-pressure.Dr. Hans-Joachim Graf57.866.0X1 B: mixingX2 C: rotor speedActual FactorA: Mastication 50.0064.0E xtr O utput(Extrusion Experiment at constant Screw speed 50 rpm) Extrusion Motor power consumption (Nm) (left) Extrusion Head Pressure (bar) (right)Design-Expert SoftwareFactor Coding: ActualExtr OutputDesign points above predicted valueDesign points below predicted 3047.00C: rotor speed4.7041.004.1035.003.50B: mixing
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingMixing of NR/SBR/BR: Tensile Strength over Mixing Time & Rotor Speed Mastication time has little to none influenceDesign-Expert SoftwareFactor Coding: ActualTSDesign points above predicted valueDesign points below predicted value19.916.220.0X1 B: mixingX2 C: rotor speed19.0Actual FactorA: Mastication 50.0018.0TS Source: Kreuzwieser, Thesis17.016.065.006.5059.005.9053.005.3047.00C: rotor speedDr. Hans-Joachim Graf4.7041.004.1035.003.50B: mixing
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Kreuzwieser, ThesisDesign-Expert SoftwareFactor Coding: ActualCB DispersionDesign points above predicted valueDesign points below predicted value90Design-Expert SoftwareFactor Coding: ActualCB DispersionDesign points above predicted valueDesign points below predicted value9020120CB Dispersion100Actual FactorA: Mastication 30.0080Actual FactorA: Mastication : rotor speed4.7041.004.1035.00 3.50B: mixingMixing of NR/SBR/BR: CB Distribution over Mixing Time & Rotor Speed 30 sec Mastikation time – (left)50 sec Mastikation time – (right) 70 sec Mastikation time – (lower 0C: rotor speed4.7041.004.1035.0020120X1 B: mixingX2 C: rotor speedActual FactorA: Mastication 00C: rotor speed4.7041.004.1035.00Dr. Hans-Joachim GrafB: mixing3.50Design-Expert SoftwareFactor Coding: ActualCB DispersionDesign points above predicted valueDesign points below predicted value90C B D isp ersionX1 B: mixingX2 C: rotor speed120X1 B: mixingX2 C: rotor speedCB Dispersion203.50B: mixing
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionDesign-Expert SoftwareFactor Coding: ActualOverlay PlotOverlay Plot65.00ML(1 4)100E spec. MixingE spec ExtrudExtr Motor PowerExtr Head PressTSCB DispersionDesign PointsDesign-Expert SoftwareFactor Coding: ActualOverlay PlotExtr Head Press: 60.000ML(1 4)100: 45.000CB Dispersion: 80.000TS: 19.00059.00Actual FactorA: Mastication 30.00C: rotor speedExtr Motor Power: 51.00053.00X1 B: mixingX2 C: rotor speedActual FactorA: Mastication 50.0047.0041.00Overlay Plot65.00ML(1 4)100E spec. MixingE spec ExtrudExtr Motor PowerExtr Head PressTSCB DispersionDesign PointsExtr Head Press: E65.000spec. Mixing: 444.034X1 B: mixingX2 C: rotor speedSource: Kreuzwieser, ThesisML(1 4)100: 45.000Extr Head Press: 65.000CB Dispersion: 80.000Extr Motor Power: 51.00059.00E spec. Mixing: 444.034TS: 19.000C: rotor speedReview of 906.503.504.104.70B: mixingDesign-Expert SoftwareFactor Coding: ActualOverlay PlotMixing of NR/SBR/BR: Factors: Mixing Time over Rotor Speed Response: Optimization 5.90ML(1 4)100E spec. MixingE spec ExtrudExtr Motor PowerExtr Head PressTSCB DispersionDesign PointsX1 B: mixingX2 C: rotor speedActual FactorA: Mastication 70.00Head Pressure / Specific Mixing EnergyCB- Dispersion / TS (Tensile strength) / Mooney Viscosity6.50CB -DispersionB: mixingOverlay Plot65.00Extr Head Press: 65.00059.00C : roto r s p ee d 5.30Extr Motor Power: 51.000E spec. Mixing: 444.034TS: 19.00053.0047.0041.0035.003.504.104.705.30B: mixingDr. Hans-Joachim Graf5.906.50
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: Kreuzwieser Thesis Mixing Time – VAW concentration Tire Tread CompoundDesign-Expert SoftwareFactor Coding: ActualOverlay PlotX1 B: Mix TimeX2 A: VAWMl(1 4) 100: 59.0004.203.50Ml(1 4) 100: 63.076EB: 500.184A: VAWMl(1 4) 100Fmax-FminEspec MixEspec EtrudM100M300TSEBDesign PointsOverlay Plot4.902.80TS: 12.000TS:11.000EspecMix : 142.000EB: 560.7482.10Fmax-Fmin: 0.5801.40TS0.70Mooney0.00126.00M100: 1.500135.00144.00153.00162.00171.00180.00B: Mix TimeDr. Hans-Joachim Graf24
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: Nijmann Vredestein Effect of Polymer Structure on Mixing Influence of branching Power consumption of the mixer and batch temperature in themixing phase due to EPDM LCB (Mixer: W&P, GK90E, RotorPES3)Dr. Hans-Joachim Graf25
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource:HJ Graf, KHK 2002GPC-MW Viscosity Drop during mixing Mastication of EPDMChange of MW Distributioncurve depends on MW andMWD Most rubbers showdecrease in viscosity, ifexposed to mechanicaland heat energy.Molecular weight curvewill change it size andform!GPC Eluation TimeDr. Hans-Joachim Graf26
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: S.Yu, H-J Graf1,0000dw t(M)/dlogM0,90000,8000Polymer "D"0,7000Polymer "D" ,003,504,004,505,005,506,006,507,00log (M) MW decrease of EPDM Due to mixing there is a shift ofGPC average MW(Note the GPC-MW / MooneyCorrelation) Polymers of different origin behavedifferent High MW Polymers effected morethan low MW PolymersDr. Hans-Joachim Graf27
Review of Mixing IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: HJ GrafMixing experiment with EPDM low (left) MW / high MW (right)Tensile strength [MPa]Dr. Hans-Joachim Graf28
Review of Mixing IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: HJ GrafMixing experiment with EPDM low (left) MW / high MW (right)Crack Growth 25 (top) / 35 (bottom) (mm/cycle 10 -5)Dr. Hans-Joachim Graf29
Function / Use of Process AidsMixing of CompoundMeeting a SpecificationCompound to CostMethods in DevelopmentCompound DoE&SimulationReverse DevelopmentCompound Exercises IntroductionEffects of mixing on PolymerIncorporation of FillersMixing of OilInteraction of IngredientsAcceleration in the mixer / millMixing Recipe Design in consideration of formulaSummarySource: HJ GrafMixing experiment with EPDM low (left) MW / high MW (right)Fatigue to falilure (cycles)Dr. Hans-Joachim Graf30
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: Cotten, RCT 58 Influence of CB PropertiesPolymer CB-441 at loading of CB 50 phrDr. Hans-Joachim Graf31
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: Cotten, RCT 58 Influence of CB PropertiesPolymer CB-441 at loading of CB 50 phrDr. Hans-Joachim Graf32
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Hess, RCT 57 Properties of Carbon Black influencethe mixing process and the propertiesof the compound DOE with Carbon blacks DOE map according to available CBgradesCB-Dispersion on SBR 1500compound as a function of CBsurface area and DBPA at to differentmixing procedures CB and oil added separatelyCB added with blackSBR 1500 with60 phr CB37,5 phr oilAccording to modern DoE Programs: lack of statisticsignificance.Dr. Hans-Joachim Graf33
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSource: Hess, RCT 57 Addition of Oil In some rubbers oil mustbe added separately toachieve proper dispersionof CB SBR 1500 needs separateaddition of oil. Otherwise compound willnot take up enough shearfor dispersion According to modern DoE programslack of statistic significanceDr. Hans-Joachim GrafSBR 1500 Compound with10 phr, 25 phr and 40 phr Oil34
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of MixingSBR 1712 – Mixing dependent on CB DBPA-Absorption & N² Surface But the Statistic models are not significantDesign-Expert SoftwareFactor Coding: ActualMix Time 120rpmDesign points above predicted valueDesign points below predicted value6.6Design-Expert SoftwareFactor Coding: ActualMix Time 80rpmDesign points above predicted valueDesign points below predicted value7.83.04.18.0Mix Time 80rpmX1 A: DBPAX2 B: N²surfaceX1 A: DBPAX2 B: N²surface7.06.05.04.03.07.0Mix Time 120rpm Source: Hess, RCT .00125.00100.0046.0020.00Dr. Hans-Joachim Graf100.0072.0072.00B: N²surface125.0098.0098.00B: N²surface75.0046.0075.0050.00A: DBPA20.0050.00A: DBPA35
IntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionReview of Mixing Source: Hess, RCT 57SBR 1712 – Mixing dependent on CB DBPA-Absorption & N² Surface ? But the Statistic models are not significant Mix Energy to 95% Dispersion – Predicted vs Actual (left) But Correlation of Dispersion Index with Factors are significant (right)Design-Expert SoftwareMix Energy 95DIDesign-Expert SoftwareDisp-IndexPredicted vs. ActualColor points by value ofMix Energy 95DI:1800Predicted vs. ActualColor points by value . Hans-Joachim tual36
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource: Exxon Filler / Oil ratio of Rubber due to processing window in mixing Viscosity (or MW) dependent ability to load with carbon black andoilDr. Hans-Joachim Graf37
Review of MixingIntroductionMixing of SBRMixing of NR/BR/SBRMixing of EPDMCB Dispersion in SBRConclusionSource of Slide: Exxon Conclusion / Important to remember: SBR requires high rotor speed and longer mixing timeresp. Energy input NR (Blend) requires medium to high rotor speed andsufficient time for maximum performance.Temperature should be kept under control EPDM requires lower rotor speed and mixing time as shortas possible Carbon Black Dispersion experiment should be redeveloped (statistic significance not sufficient)We should redo this experiments!Dr. Hans-Joachim Graf38
viscosity of masticated SBR rubber and on temperature of mastication. Source: Martin, RCT 1955 Fig left: Thesis Ebell Mixing of SBR: Introduction Mixing of SBR Mixing of NR/BR/SBR Mixing
mechanical mixing (rotating, vibrating) hydraulic mixing pneumatic mixing pipeline mixing (turbulent flow, static mixer) Method of mixing fluids A –mechanical mixing using turbines B –mechanical mixing using blade impellers C –hydraulic mixing D –pneumatic mixing with stationary inputs
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