HAAKE转矩流变仪在高分子材料中的应用

HAAKE转矩流变仪在高分子材料中的应用白伟2006年8月12日美国热电集团:简介24亿美金年销售收入2reportingsegments,6大部门超过10,000员工在全球30个国家开展业务HeadquarternearBoston,MAWaltham,Massachusetts,USAHeadquartersThermoKarlsruhe,GermanFacility

热电集团卡斯鲁贺德国工厂（原HAAKE哈克公司）13.200m2230EmployeesFullyintegratedsheetmetal,paint,prefabandwireharnesscapabilitiesCellularmanufacturingProductengineeringComplianceandregulatoryengineering-canprovide“consulting”Sales,marketing,service,financeUSAEuropeAsiaYourpartner

forMaterialCharacterization(MC)实验室加工生产Viscosimeters,rheometersandMeltflowsystemsfor

research,developmentandquality

control粘度计、流变仪、熔融指数仪等用于研究、开发和质量控制Torquerheometerswithsingle-andtwinscrew

extruders,mixerandpostexsystemsfor

scaleupinproduction转矩流变仪系统用于缩小比例模拟加工On-lineviscosimetersandrheometersfor

controllingofproductionviaviscosityandMFImeasurement在线流变仪YourPartnerfortheLaboratory(MC)粘度计旋转流变仪拉伸流变仪HandheldorbenchbasedviscometerstomeasureafluidsviscosityScientificdynamicrheometersforR&DandQCinalmostallmarketsforfluids,pastesandsolidsExtensionalviscometerforfluids(CaBER)ormeltsusingX-dieYourPartnerfortheProcessandProduction(MC)熔融指数仪转矩流变仪MeltFlowindexertomeasuretheMFIorMFRofpolymermeltsasameanstoQCModularPolyLabsystemwithmeasuringmixersandmeasuringextruderstosimulateproductionandverifyprocesses.MaterialCharacterization–ProcessandProduction微型双螺杆挤出机双螺杆挤出机在线流变仪Mini-CompounderandMini-Injection

Moulding

forsmallestamountsofmaterial(1to50g)TwinscrewCompounderfordevelopementandPilotplant

(50gto150kg/h)On-lineRheometerforcontinous

monitoringofviscosityandMIofPoly-mermeltsinProduction(20t/h)橡胶配方设计

聚合物在液体状态下进行加工:

(挤出、注射)

流动性（粘度）会影响加工过程和最终产品的质量:

转矩流变仪是按比例缩小的生产设备

(密炼机、挤出机、口模、辅机设备)测试过程模拟生产转矩流变仪系统

为什么使用转矩流变仪

?单螺杆挤出机测试器

喂料系统转子双螺杆挤出机测试器RheoDrive主机

+混合器/挤出机测试器

=PolyLabOS混合器测试器螺杆口模辅机设备各种传感器RheoDrive主机PolyLabOS转矩流变仪–NewDesignPolyLabOS转矩流变仪–NewDesignChangefromMixertoExtruderLaboratoryMixers

measuringprinciple32Shearingofatestsampleinaheatedmixingchamberwithcounterrotatingrotors测试所得结果:转矩熔体温度RotorsforRheomixmixers

混合器所用的转子BanburyrotorsRollerrotorsCamrotorsSigmarotorsMixer–

Rheogram

混合器－流变谱图Temperature

温度Energy能量Torque

转矩MixerTestMaterials:Polyolefins:

(PolyethylenePE

PolypropenePP)EngineeringPlastics:

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

加料峰M=Minimumpoint

最低点PolyViewRoutineevaluation

CurveType1曲线类型1

12345678910Torque转矩[Nm]Runtime运行时间ML0PolyViewRoutineEvaluation

Curvetype1LoadingPoint

加料峰

Detectscompletemixerloading.

Pointisonlyusedastimebaseforfurthercalculations

Torquevaluedependsontheloadingconditions

可得知物料的完全加入，加料峰只作为进一步计算的时间基点，转矩值和加料情况有关。Minimumpoint

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

加料峰V=Valleypoint

谷点

(startingpointofmeltingprocess熔融过程的起始点)F=Fusionpoint

熔点

(meltingprocessfinished

熔融过程结束)M=MinimumpointPolyViewRoutineevaluation

CurveType2

曲线类型2012345678910Torque[Nm]Runtime[minutes]LFVMLoadingPeak:

可得知物料的完全加入，加料峰只作为进一步计算的时间基点，转矩值和加料情况有关，受到加料速度和加料负载的影响。ValleyPoint:

显示PVC干粉开始熔融，此点对配方设计非常重要FusionPeak:

显示PVC干粉熔融结束，此点对配方设计非常重要.

由于摩擦生热，从此点开始，转矩逐渐降低MinimumPoint:

显示熔体粘度达到最低的时间PolyViewRoutineevaluation

CurveType2Materials:PVC(rigid)StabilitytestPVC干粉稳定性测试Pointdetection:L=Loadingpoint

加料峰V=Valleypoint谷点

(startingpointofmeltingprocess熔融过程的起始点)F=Fusionpoint熔点

(meltingprocessfinished

熔融过程结束)M=MinimumpointO=Onsetofdegradation

降解起始点D=Degradation

降解峰PolyViewRoutineevaluation

CurveType3

曲线类型3036912151821242730Torque转矩[Nm]Runtime运行时间[minutes]Stabletime稳定时间DOMSFVLPolyViewRoutineevaluation

CurveType3LoadingPeak:

可得知物料的完全加入，加料峰只作为进一步计算的时间基点，转矩值和加料情况有关，受到加料速度和加料负载的影响。ValleyPoint:

显示PVC干粉开始熔融，此点对配方设计非常重要FusionPeak:

显示PVC干粉熔融结束，此点对配方设计非常重要.

由于摩擦生热，从此点开始，转矩逐渐降低MinimumPoint:

显示熔体粘度达到最低的时间OnsetofDegradation

降解起始点

显示材料开始降解，这对加工稳定性非常重要

它可以使用最低转矩的相对百分比值来设置

Stabletorquepoint

稳定转矩点

显示转矩达到平稳的时间

它由降解起始点决定Stabletime

稳定时间

在稳定转矩点和降解起始点之间的时间

它告诉我们对物料的加工时间和稳定性DegradationPeak

降解峰

显示降解达到最高值

没有太大的实际意义，仅用于降解率的计算

PolyViewRoutineevaluation

CurveType3Materials:

PVC–granulate(Stabilitytest)

X–linkingmaterials

(PE,Rubber,Thermoset)

PVC粒状，交联材料（PE、橡胶、热固性塑料）Pointdetection:

L=Loadingpoint

S=StableTorque

M=Minimumpoint

O=OnsetofDegradation

D=DegradationRuntimePolyViewRoutineevaluation

CurveType4and5

TorqueLMODSStabletimeApplication:PVC稳定性测试Rheomix600p,RollerRotorsTemp:170°C,n:60rpm,m:65ga:PVCDry-Blendwith1,9%Stabilizerb:PVCDry-Blendwith2,0%StabilizeraabbSANwithCarbonBlack碳黑对SAN的影响Torque[Nm]Time[min]Rheomix600,RollerRotorsTemp.:230°C,m:58g,n:40rpmSAN&30%CarbonBlack2SAN&30%CarbonBlack1Rubber-CompoundswiththesameMooneyViscosity门尼粘度相同的橡胶Batch1Batch2Rheomix600,BanburyRotorsTemp.:130°C,n:60rpm,m:63g应用-增塑剂对PVC的影响2Rubber-Compoundsn=70rpmn=5rpmRheomix600p,Banbury-RotorenTemp.:130°C,m:80gTime[min]Torque[Nm]Compound1Compound2Batchdifferensationwithspeed-program应用-不同转速对物料的影响Production-ImprovementwithLab-MixersTorque[Nm]Energy[kJ]Time[min]Energy2Energy1Torque1Torque2ProductionofHot-Melts:procedure1:A+B+Cprocedure2:A+C+B应用－对生产过程进行改进ThermosetMixerRheomix540

(principlesketch)

FrontplatewithmeltthermocoupleConical

CentrebowlBackwallConical

RotorsBushingswithO-rings....GasFlowSensorforRheomix

气体流量传感器Teflonblock特弗伦挡板Gas-Outlet排气口Screen滤网Application:foamingCompounds

发泡材料degradationtests

降解测试MeasuringresultsGasflowsensorTheConductivityofrubbercompoundsas

ameasureforthedispersionofcarbon

blackismostimportant.Studiesonthe

finalcompoundsbyuseofclassicallaboratory

instrumentshavebeenreported(e.g.Carbon

Co.,FortWorth).

Gettingthoseinformationduringthemixing

mixingprocesscouldbeofgreatimportance

forqualitycontrolandwastereduction.

ThermoHaakehasdonethefirststep

inalaboratoryscaledmixerwithan

integratedConductivitySensor.

Theresultslookpromising!

Integrated

ConductivitySensorConductivityMeasurementforRubber

CompoundQualification电导率测试Rheomexsinglescrewextruder

单螺杆挤出机FeedingcoolingSensorports

(2standard,othersoptional)Screwback-pressure

sensor(optional)collarsforheatingandcoolingSinglescrewextruders

forPolyLabSystem:TwinscrewExtruder双螺杆挤出机Counter-rotatingRheomexTwinscrewExtruders:反向双螺杆挤出机

Defined

residencetime(goodfori.e.rigidPVC)

Selfcleaning

Nocontrolled

feeding

needed

Highshearing

Highpressure

builtupCo-rotatingRheomexTwinscrewExtruders:同向双螺杆挤出机

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流延膜设备吹膜设备OpticalQualityTestingSystem

光学检测系统

LightningDeviceCCD-CameraPolymer

filmPCwithevaluation

softwareMeasuringprinciple:ImageprocessorControlmonitorfor

CCDVideosignalOQT-GraphicaldisplayofthedataanddefectsScreenlifetest

滤网寿命测试

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出口膨胀测试*100%Dieswell=D-d

ddetectingelasticpolymerbehaviourCapillaryDies

毛细管口模Slitcapillary

Die狭缝毛细管口模Rodcapillary

Die圆棒毛细管口模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不同的螺杆组合对产品粘度的影响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

其他口模及设备圆孔口模管材口模医用管材口模（导尿管、输液管）GARVEY口模电缆包覆口模纺丝口模过滤口模相关的牵引装置各种喂料器水槽、切粒机等Example:CompoundingMeteringFeederforPEEKPelletsCabonFiberRoving(endless)Pelletiser

VaricutT=380°C20-40%C-Fiber(wt/wt)NewTwinScrewsPTW24/28p2modularModels28Dand40Dupto1100rpm...Happycustomers锥形双螺杆结构:同向和反向旋转自动回流控制系统回流通道中粘度测量气动、手动喂料系统inertgasflushHigh–Tempertureupto420°C数字图形显示manualandcomputercontrolNewbeltd