HAAKE轉矩流變儀在高分子材料中的應用

HAAKE轉矩流變儀在高分子材料中的應用白偉2006年8月12日美國熱電集團:簡介24億美金年銷售收入2reportingsegments,6大部門超過10,000員工在全球30個國家開展業(yè)務HeadquarternearBoston,MAWaltham,Massachusetts,USAHeadquartersThermoKarlsruhe,GermanFacility

熱電集團卡斯魯賀德國工廠（原HAAKE哈克公司）13.200m2230EmployeesFullyintegratedsheetmetal,paint,prefabandwireharnesscapabilitiesCellularmanufacturingProductengineeringComplianceandregulatoryengineering-canprovide“consulting”Sales,marketing,service,financeUSAEuropeAsiaYourpartner

forMaterialCharacterization(MC)實驗室加工生產Viscosimeters,rheometersandMeltflowsystemsfor

research,developmentandquality

control粘度計、流變儀、熔融指數(shù)儀等用于研究、開發(fā)和質量控制Torquerheometerswithsingle-andtwinscrew

extruders,mixerandpostexsystemsfor

scaleupinproduction轉矩流變儀系統(tǒng)用于縮小比例模擬加工On-lineviscosimetersandrheometersfor

controllingofproductionviaviscosityandMFImeasurement在線流變儀YourPartnerfortheLaboratory(MC)粘度計旋轉流變儀拉伸流變儀HandheldorbenchbasedviscometerstomeasureafluidsviscosityScientificdynamicrheometersforR&DandQCinalmostallmarketsforfluids,pastesandsolidsExtensionalviscometerforfluids(CaBER)ormeltsusingX-dieYourPartnerfortheProcessandProduction(MC)熔融指數(shù)儀轉矩流變儀MeltFlowindexertomeasuretheMFIorMFRofpolymermeltsasameanstoQCModularPolyLabsystemwithmeasuringmixersandmeasuringextruderstosimulateproductionandverifyprocesses.MaterialCharacterization–ProcessandProduction微型雙螺桿擠出機雙螺桿擠出機在線流變儀Mini-CompounderandMini-Injection

Moulding

forsmallestamountsofmaterial(1to50g)TwinscrewCompounderfordevelopementandPilotplant

(50gto150kg/h)On-lineRheometerforcontinous

monitoringofviscosityandMIofPoly-mermeltsinProduction(20t/h)橡膠配方設計

聚合物在液體狀態(tài)下進行加工:

(擠出、注射)

流動性（粘度）會影響加工過程和最終產品的質量:

轉矩流變儀是按比例縮小的生產設備

(密煉機、擠出機、口模、輔機設備)測試過程模擬生產轉矩流變儀系統(tǒng)

為什么使用轉矩流變儀

?單螺桿擠出機測試器

喂料系統(tǒng)轉子雙螺桿擠出機測試器RheoDrive主機

+混合器/擠出機測試器

=PolyLabOS混合器測試器螺桿口模輔機設備各種傳感器RheoDrive主機PolyLabOS轉矩流變儀–NewDesignPolyLabOS轉矩流變儀–NewDesignChangefromMixertoExtruderLaboratoryMixers

measuringprinciple32Shearingofatestsampleinaheatedmixingchamberwithcounterrotatingrotors測試所得結果:轉矩熔體溫度RotorsforRheomixmixers

混合器所用的轉子BanburyrotorsRollerrotorsCamrotorsSigmarotorsMixer–

Rheogram

混合器－流變譜圖Temperature

溫度Energy能量Torque

轉矩MixerTestMaterials:Polyolefins:

(PolyethylenePE

PolypropenePP)EngineeringPlastics:

(PS,PA,PC,PEEK,LCP)Pointdetection:L=Loadingpoint

加料峰M=Minimumpoint

最低點PolyViewRoutineevaluation

CurveType1曲線類型1

12345678910Torque轉矩[Nm]Runtime運行時間ML0PolyViewRoutineEvaluation

Curvetype1LoadingPoint

加料峰

Detectscompletemixerloading.

Pointisonlyusedastimebaseforfurthercalculations

Torquevaluedependsontheloadingconditions

可得知物料的完全加入，加料峰只作為進一步計算的時間基點，轉矩值和加料情況有關。Minimumpoint

可得到最低熔體粘度Materials:PVC(rigid)Pointdetection:L=Loadingpoint

加料峰V=Valleypoint

谷點

(startingpointofmeltingprocess熔融過程的起始點)F=Fusionpoint

熔點

(meltingprocessfinished

熔融過程結束)M=MinimumpointPolyViewRoutineevaluation

CurveType2

曲線類型2012345678910Torque[Nm]Runtime[minutes]LFVMLoadingPeak:

可得知物料的完全加入，加料峰只作為進一步計算的時間基點，轉矩值和加料情況有關，受到加料速度和加料負載的影響。ValleyPoint:

顯示PVC干粉開始熔融，此點對配方設計非常重要FusionPeak:

顯示PVC干粉熔融結束，此點對配方設計非常重要.

由于摩擦生熱，從此點開始，轉矩逐漸降低MinimumPoint:

顯示熔體粘度達到最低的時間PolyViewRoutineevaluation

CurveType2Materials:PVC(rigid)StabilitytestPVC干粉穩(wěn)定性測試Pointdetection:L=Loadingpoint

加料峰V=Valleypoint谷點

(startingpointofmeltingprocess熔融過程的起始點)F=Fusionpoint熔點

(meltingprocessfinished

熔融過程結束)M=MinimumpointO=Onsetofdegradation

降解起始點D=Degradation

降解峰PolyViewRoutineevaluation

CurveType3

曲線類型3036912151821242730Torque轉矩[Nm]Runtime運行時間[minutes]Stabletime穩(wěn)定時間DOMSFVLPolyViewRoutineevaluation

CurveType3LoadingPeak:

可得知物料的完全加入，加料峰只作為進一步計算的時間基點，轉矩值和加料情況有關，受到加料速度和加料負載的影響。ValleyPoint:

顯示PVC干粉開始熔融，此點對配方設計非常重要FusionPeak:

顯示PVC干粉熔融結束，此點對配方設計非常重要.

由于摩擦生熱，從此點開始，轉矩逐漸降低MinimumPoint:

顯示熔體粘度達到最低的時間OnsetofDegradation

降解起始點

顯示材料開始降解，這對加工穩(wěn)定性非常重要

它可以使用最低轉矩的相對百分比值來設置

Stabletorquepoint

穩(wěn)定轉矩點

顯示轉矩達到平穩(wěn)的時間

它由降解起始點決定Stabletime

穩(wěn)定時間

在穩(wěn)定轉矩點和降解起始點之間的時間

它告訴我們對物料的加工時間和穩(wěn)定性DegradationPeak

降解峰

顯示降解達到最高值

沒有太大的實際意義，僅用于降解率的計算

PolyViewRoutineevaluation

CurveType3Materials:

PVC–granulate(Stabilitytest)

X–linkingmaterials

(PE,Rubber,Thermoset)

PVC粒狀，交聯(lián)材料（PE、橡膠、熱固性塑料）Pointdetection:

L=Loadingpoint

S=StableTorque

M=Minimumpoint

O=OnsetofDegradation

D=DegradationRuntimePolyViewRoutineevaluation

CurveType4and5

TorqueLMODSStabletimeApplication:PVC穩(wěn)定性測試Rheomix600p,RollerRotorsTemp:170°C,n:60rpm,m:65ga:PVCDry-Blendwith1,9%Stabilizerb:PVCDry-Blendwith2,0%StabilizeraabbSANwithCarbonBlack碳黑對SAN的影響Torque[Nm]Time[min]Rheomix600,RollerRotorsTemp.:230°C,m:58g,n:40rpmSAN&30%CarbonBlack2SAN&30%CarbonBlack1Rubber-CompoundswiththesameMooneyViscosity門尼粘度相同的橡膠Batch1Batch2Rheomix600,BanburyRotorsTemp.:130°C,n:60rpm,m:63g應用-增塑劑對PVC的影響2Rubber-Compoundsn=70rpmn=5rpmRheomix600p,Banbury-RotorenTemp.:130°C,m:80gTime[min]Torque[Nm]Compound1Compound2Batchdifferensationwithspeed-program應用-不同轉速對物料的影響Production-ImprovementwithLab-MixersTorque[Nm]Energy[kJ]Time[min]Energy2Energy1Torque1Torque2ProductionofHot-Melts:procedure1:A+B+Cprocedure2:A+C+B應用－對生產過程進行改進ThermosetMixerRheomix540

(principlesketch)

FrontplatewithmeltthermocoupleConical

CentrebowlBackwallConical

RotorsBushingswithO-rings....GasFlowSensorforRheomix

氣體流量傳感器Teflonblock特弗倫擋板Gas-Outlet排氣口Screen濾網Application:foamingCompounds

發(fā)泡材料degradationtests

降解測試MeasuringresultsGasflowsensorTheConductivityofrubbercompoundsas

ameasureforthedispersionofcarbon

blackismostimportant.Studiesonthe

finalcompoundsbyuseofclassicallaboratory

instrumentshavebeenreported(e.g.Carbon

Co.,FortWorth).

Gettingthoseinformationduringthemixing

mixingprocesscouldbeofgreatimportance

forqualitycontrolandwastereduction.

ThermoHaakehasdonethefirststep

inalaboratoryscaledmixerwithan

integratedConductivitySensor.

Theresultslookpromising!

Integrated

ConductivitySensorConductivityMeasurementforRubber

CompoundQualification電導率測試Rheomexsinglescrewextruder

單螺桿擠出機FeedingcoolingSensorports

(2standard,othersoptional)Screwback-pressure

sensor(optional)collarsforheatingandcoolingSinglescrewextruders

forPolyLabSystem:TwinscrewExtruder雙螺桿擠出機Counter-rotatingRheomexTwinscrewExtruders:反向雙螺桿擠出機

Defined

residencetime(goodfori.e.rigidPVC)

Selfcleaning

Nocontrolled

feeding

needed

Highshearing

Highpressure

builtupCo-rotatingRheomexTwinscrewExtruders:同向雙螺桿擠出機

Mixingofshearsensitivematerial(i.e.Polyolefins)

Compounding,MasterbatchproductionVentingControlled

shearing

Flexiblescrewdesign

Controlled

feeding

necessary...Screwdesign......Feedports......SplitBarrelMaximumflexibility…...Lenght...PTW16OS-Maximumflexibility…PTW16OS-Maximumflexibility…25L/D+15L/D=40L/DScrews:

Segmented,withslip-onelements,allowingvariableconfigurationScrewdiameter:16mmCorotating,intermeshing

screwsScrewshafts:

Design:hexagonalMaterial:Heattreated,abrasionresistantTechnicalSpecificationsRheomexPTW16流延膜設備吹膜設備OpticalQualityTestingSystem

光學檢測系統(tǒng)

LightningDeviceCCD-CameraPolymer

filmPCwithevaluation

softwareMeasuringprinciple:ImageprocessorControlmonitorfor

CCDVideosignalOQT-GraphicaldisplayofthedataanddefectsScreenlifetest

濾網壽命測試

FPV(filterpressurevalue):Ps:Pmax:Mc:Filter-Pressure-Value

inbarpergrams[bar/g]Starting

pressure

inbarMaximum

pressureinbarPigmentweight

ingram

accordingEN13900-5(draft)Purgewith100gbasepolymerMasterbatchConditioningwithbasepolymerPressure

increaseinfrontofthe

filterpackagePmaxPsPmax-Pststtets:

determinationofbasepressurePs

andfillingofthe

hopper

with masterbatchmixture

t: Endofmasterbatchmixture andfillingofbasepolymer

te: Endofpressure

measurement andevaluationofmaximum pressure

PmaxFilterTestSoftwareLASER-BEAM(D)Capillary(d)DieswellMeasurement出口膨脹測試*100%Dieswell=D-d

ddetectingelasticpolymerbehaviourCapillaryDies

毛細管口模Slitcapillary

Die狹縫毛細管口模Rodcapillary

Die圓棒毛細管口模10,0E+3100,0E+31,0E+610100100010000Shearrate[1/s]ShearStress[Pa]101001000Viscosity[Pas]FlowcurveViscositycurveCapillarySoftware

Measurement

ResultsViscositycurvesofanABS

-CompoundTrueShearRate[1/s]Trueviscosity[Pas]SlitCapillarydieRodCapillarydie11010010001000010100100010000100000200°C230°C260°CViscositymeasurementsofaLDPEsampleInfluenceoftwinscrewdesignonproductviscosity不同的螺桿組合對產品粘度的影響ShearRate[1/s]Viscosity[Pa*s]ShearStress[Pa]Viscosity(optimizedscrewdesign)Viscosity(highsheared)ShearStress(optimizedscrewdesign)ShearStress(highsheared)ViscositymeasurementsoftwoLDPEsamplesR252,Slitcapillarydie,h=1.2mm,Temp.280oC

withthesameMFRvalue(4.0g/10min),butdifferentproductionbehaviour

其他口模及設備圓孔口模管材口模醫(yī)用管材口模（導尿管、輸液管）GARVEY口模電纜包覆口模紡絲口模過濾口模相關的牽引裝置各種喂料器水槽、切粒機等Example:CompoundingMeteringFeederforPEEKPelletsCabonFiberRoving(endless)Pelletiser

VaricutT=380°C20-40%C-Fiber(wt/wt)NewTwinScrewsPTW24/28p2modularModels28Dand40Dupto1100rpm...Happycustomers錐形雙螺桿結構:同向和反向旋轉自動回流控制系統(tǒng)回流通道中粘度測量氣動、手動喂料系統(tǒng)inertgasflushHigh–Tempertureupto420°C數(shù)字圖形顯示manualandcomputercontrolNewbeltd