HAAKE轉(zhuǎn)矩流變儀在高分子材料中的應(yīng)用

HAAKE轉(zhuǎn)矩流變儀在高分子材料中的應(yīng)用白偉2006年8月12日美國(guó)熱電集團(tuán):簡(jiǎn)介24億美金年銷售收入2reportingsegments,6大部門(mén)超過(guò)10,000員工在全球30個(gè)國(guó)家開(kāi)展業(yè)務(wù)HeadquarternearBoston,MAWaltham,Massachusetts,USAHeadquartersThermoKarlsruhe,GermanFacility

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

forMaterialCharacterization(MC)實(shí)驗(yàn)室加工生產(chǎn)Viscosimeters,rheometersandMeltflowsystemsfor

research,developmentandquality

control粘度計(jì)、流變儀、熔融指數(shù)儀等用于研究、開(kāi)發(fā)和質(zhì)量控制Torquerheometerswithsingle-andtwinscrew

extruders,mixerandpostexsystemsfor

scaleupinproduction轉(zhuǎn)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(jì)旋轉(zhuǎn)流變儀拉伸流變儀HandheldorbenchbasedviscometerstomeasureafluidsviscosityScientificdynamicrheometersforR&DandQCinalmostallmarketsforfluids,pastesandsolidsExtensionalviscometerforfluids(CaBER)ormeltsusingX-dieYourPartnerfortheProcessandProduction(MC)熔融指數(shù)儀轉(zhuǎn)矩流變儀MeltFlowindexertomeasuretheMFIorMFRofpolymermeltsasameanstoQCModularPolyLabsystemwithmeasuringmixersandmeasuringextruderstosimulateproductionandverifyprocesses.MaterialCharacterization–ProcessandProduction微型雙螺桿擠出機(jī)雙螺桿擠出機(jī)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(shè)計(jì)

聚合物在液體狀態(tài)下進(jìn)行加工:

(擠出、注射)

流動(dòng)性（粘度）會(huì)影響加工過(guò)程和最終產(chǎn)品的質(zhì)量:

轉(zhuǎn)矩流變儀是按比例縮小的生產(chǎn)設(shè)備

(密煉機(jī)、擠出機(jī)、口模、輔機(jī)設(shè)備)測(cè)試過(guò)程模擬生產(chǎn)轉(zhuǎn)矩流變儀系統(tǒng)

為什么使用轉(zhuǎn)矩流變儀

?單螺桿擠出機(jī)測(cè)試器

喂料系統(tǒng)轉(zhuǎn)子雙螺桿擠出機(jī)測(cè)試器RheoDrive主機(jī)

+混合器/擠出機(jī)測(cè)試器

=PolyLabOS混合器測(cè)試器螺桿口模輔機(jī)設(shè)備各種傳感器RheoDrive主機(jī)PolyLabOS轉(zhuǎn)矩流變儀–NewDesignPolyLabOS轉(zhuǎn)矩流變儀–NewDesignChangefromMixertoExtruderLaboratoryMixers

measuringprinciple32Shearingofatestsampleinaheatedmixingchamberwithcounterrotatingrotors測(cè)試所得結(jié)果:轉(zhuǎn)矩熔體溫度RotorsforRheomixmixers

混合器所用的轉(zhuǎn)子BanburyrotorsRollerrotorsCamrotorsSigmarotorsMixer–

Rheogram

混合器－流變譜圖Temperature

溫度Energy能量Torque

轉(zhuǎn)矩MixerTestMaterials:Polyolefins:

(PolyethylenePE

PolypropenePP)EngineeringPlastics:

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

加料峰M=Minimumpoint

最低點(diǎn)PolyViewRoutineevaluation

CurveType1曲線類型1

12345678910Torque轉(zhuǎn)矩[Nm]Runtime運(yùn)行時(shí)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(jìn)一步計(jì)算的時(shí)間基點(diǎn)，轉(zhuǎn)矩值和加料情況有關(guān)。Minimumpoint

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

加料峰V=Valleypoint

谷點(diǎn)

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

熔點(diǎn)

(meltingprocessfinished

熔融過(guò)程結(jié)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(jìn)一步計(jì)算的時(shí)間基點(diǎn)，轉(zhuǎn)矩值和加料情況有關(guān)，受到加料速度和加料負(fù)載的影響。ValleyPoint:

顯示PVC干粉開(kāi)始熔融，此點(diǎn)對(duì)配方設(shè)計(jì)非常重要FusionPeak:

顯示PVC干粉熔融結(jié)束，此點(diǎn)對(duì)配方設(shè)計(jì)非常重要.

由于摩擦生熱，從此點(diǎn)開(kāi)始，轉(zhuǎn)矩逐漸降低MinimumPoint:

顯示熔體粘度達(dá)到最低的時(shí)間PolyViewRoutineevaluation

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

加料峰V=Valleypoint谷點(diǎn)

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

(meltingprocessfinished

熔融過(guò)程結(jié)束)M=MinimumpointO=Onsetofdegradation

降解起始點(diǎn)D=Degradation

降解峰PolyViewRoutineevaluation

CurveType3

曲線類型3036912151821242730Torque轉(zhuǎn)矩[Nm]Runtime運(yùn)行時(shí)間[minutes]Stabletime穩(wěn)定時(shí)間DOMSFVLPolyViewRoutineevaluation

CurveType3LoadingPeak:

可得知物料的完全加入，加料峰只作為進(jìn)一步計(jì)算的時(shí)間基點(diǎn)，轉(zhuǎn)矩值和加料情況有關(guān)，受到加料速度和加料負(fù)載的影響。ValleyPoint:

顯示PVC干粉開(kāi)始熔融，此點(diǎn)對(duì)配方設(shè)計(jì)非常重要FusionPeak:

顯示PVC干粉熔融結(jié)束，此點(diǎn)對(duì)配方設(shè)計(jì)非常重要.

由于摩擦生熱，從此點(diǎn)開(kāi)始，轉(zhuǎn)矩逐漸降低MinimumPoint:

顯示熔體粘度達(dá)到最低的時(shí)間OnsetofDegradation

降解起始點(diǎn)

顯示材料開(kāi)始降解，這對(duì)加工穩(wěn)定性非常重要

它可以使用最低轉(zhuǎn)矩的相對(duì)百分比值來(lái)設(shè)置

Stabletorquepoint

穩(wěn)定轉(zhuǎn)矩點(diǎn)

顯示轉(zhuǎn)矩達(dá)到平穩(wěn)的時(shí)間

它由降解起始點(diǎn)決定Stabletime

穩(wěn)定時(shí)間

在穩(wěn)定轉(zhuǎn)矩點(diǎn)和降解起始點(diǎn)之間的時(shí)間

它告訴我們對(duì)物料的加工時(shí)間和穩(wěn)定性DegradationPeak

降解峰

顯示降解達(dá)到最高值

沒(méi)有太大的實(shí)際意義，僅用于降解率的計(jì)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(cè)試Rheomix600p,RollerRotorsTemp:170°C,n:60rpm,m:65ga:PVCDry-Blendwith1,9%Stabilizerb:PVCDry-Blendwith2,0%StabilizeraabbSANwithCarbonBlack碳黑對(duì)SAN的影響Torque[Nm]Time[min]Rheomix600,RollerRotorsTemp.:230°C,m:58g,n:40rpmSAN&30%CarbonBlack2SAN&30%CarbonBlack1Rubber-CompoundswiththesameMooneyViscosity門(mén)尼粘度相同的橡膠Batch1Batch2Rheomix600,BanburyRotorsTemp.:130°C,n:60rpm,m:63g應(yīng)用-增塑劑對(duì)PVC的影響2Rubber-Compoundsn=70rpmn=5rpmRheomix600p,Banbury-RotorenTemp.:130°C,m:80gTime[min]Torque[Nm]Compound1Compound2Batchdifferensationwithspeed-program應(yīng)用-不同轉(zhuǎn)速對(duì)物料的影響Production-ImprovementwithLab-MixersTorque[Nm]Energy[kJ]Time[min]Energy2Energy1Torque1Torque2ProductionofHot-Melts:procedure1:A+B+Cprocedure2:A+C+B應(yīng)用－對(duì)生產(chǎn)過(guò)程進(jìn)行改進(jìn)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(wǎng)Application:foamingCompounds

發(fā)泡材料degradationtests

降解測(cè)試MeasuringresultsGasflowsensorTheConductivityofrubbercompoundsas

ameasureforthedispersionofcarbon

blackismostimportant.Studiesonthe

finalcompoundsbyuseofclassicallaboratory

instrumentshavebeenreported(e.g.Carbon

Co.,FortWorth).

Gettingthoseinformationduringthemixing

mixingprocesscouldbeofgreatimportance

forqualitycontrolandwastereduction.

ThermoHaakehasdonethefirststep

inalaboratoryscaledmixerwithan

integratedConductivitySensor.

Theresultslookpromising!

Integrated

ConductivitySensorConductivityMeasurementforRubber

CompoundQualification電導(dǎo)率測(cè)試Rheomexsinglescrewextruder

單螺桿擠出機(jī)FeedingcoolingSensorports

(2standard,othersoptional)Screwback-pressure

sensor(optional)collarsforheatingandcoolingSinglescrewextruders

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

Defined

residencetime(goodfori.e.rigidPVC)

Selfcleaning

Nocontrolled

feeding

needed

Highshearing

Highpressure

builtupCo-rotatingRheomexTwinscrewExtruders:同向雙螺桿擠出機(jī)

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(shè)備吹膜設(shè)備OpticalQualityTestingSystem

光學(xué)檢測(cè)系統(tǒng)

LightningDeviceCCD-CameraPolymer

filmPCwithevaluation

softwareMeasuringprinciple:ImageprocessorControlmonitorfor

CCDVideosignalOQT-GraphicaldisplayofthedataanddefectsScreenlifetest

濾網(wǎng)壽命測(cè)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(cè)試*100%Dieswell=D-d

ddetectingelasticpolymerbehaviourCapillaryDies

毛細(xì)管口模Slitcapillary

Die狹縫毛細(xì)管口模Rodcapillary

Die圓棒毛細(xì)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(duì)產(chǎn)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(shè)備圓孔口模管材口模醫(yī)用管材口模（導(dǎo)尿管、輸液管）GARVEY口模電纜包覆口模紡絲口模過(guò)濾口模相關(guān)的牽引裝置各種喂料器水槽、切粒機(jī)等Example:CompoundingMeteringFeederforPEEKPelletsCabonFiberRoving(endless)Pelletiser

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