Haake PolyLab OS - Texas State University

Correlation - Mixer Test with ExtrusionTorqueExample: PVC-StabilityTime55

Application – Crosslinking Polymers56

Application – PVC Plastisol gelation57

Application – EPR Rubber58

Application – effect of different Carbon Black59

Analytical Test Methods for PolyLab OSElectrical Conductivity MeasurementThe Conductivity of rubber compounds as a measure for the dispersion ofcarbon black has been shown to be a reliable test method12334601Ram2Control Thermocouple3Rotors4Conductivity Sensor

Gas Flow Sensor for RheoMix MixersTeflon blockScreenGas OutletApplication:- Foaming Compounds- Degradation Tests61

Gas Flow Sensor - Measuring results62

The world leader in serving scienceSingle ScrewExtrusion Testing

PolyLab OS with Single Screw Extruder64

PolyLab Monitor Software – Single Screw Extruder View65

Rheomex Single Screw Extrudercollars for heating and coolingFeeding coolingScrew back-pressuresensor (optional)Sensor ports(2 standard, others optional)66

Rheomex Single Screw Extruder ApplicationsSingle Screw Extruders are generally used to:§§§§§melt and transport materialplasticizecompressvent / de-gasbuilding up pressureMeasuring of process variables:§§§§torquemelt temperaturemelt pressuremass flowOptimizing of process parameters:§§§§extruder speedtemperature profilepressurescrew design67

RheoMex Single Screw Extruder Models68

Screws for Single Screw tMeteringScrewVentingScrewMixingScrew69

Pressure built-up in a single screw extruderP3pressureP4P5P2P1barrel - length [L/D]011 14,57020,524,5

Rheomex 104 – 10:1 L/Dfor rubber application:FeedingrollMotor forroll feederZone 1(heating/cooling)Sensor portsrubber stripZone 2extruder barrel screw71feeding roll

Special single screw extruders for food extrusionèSpecial grooved extruder barrel:non-wallsticking material can be extrudedExtruder barrelgroovesExtruder screw72

The world leader in serving scienceTwin ScrewExtrusion TestingTSE Technology PPT

PolyLab Monitor Software – TSE View74

Processing with Twin Screw Extruders§Plasticizing (PVC)§Alloying or Grafting of co-polymers§Mixing - Dispersion - Homogenizing of PigmentsAdditivesPlasticizers Cross-Linking agents Flame Retardants UV Stabilizers§Degassing (venting) of monomers, oligomers, solvents§Incorporation of fillers and reinforcing agents such as: §Calcium Carbonate / TalcWood FlourGlass / Carbon Fibers, etcChemical Reactions: Polymerization – Polycondensation - PolyadditionCooking - Gelling75

Feeding Material into Twin-Screw ExtrudersCounter-rotatingCo-rotating76

Multiple Twin Screw Options to fit any need§ Co-Rotating Design (Rheomex PTW series) Most widely used type TSE in polymer industryGood for Shear Sensitive MaterialsCompounding of Masterbatch or Color ConcentratesBest design when venting is required or multiple feed pointsFlexible Screw and Barrel design – modular designControlled Feeding is required§ Counter Rotating Design (Rheomex CTW series) Narrow Residence Time distribution (good materials like PVC)Fully Self Wiping – creates high shear & high pressureNo controlled feeding is necessaryCo-Rotating Design (Rheomex PTW series)77

Modular Split Barrel, Segmented Screws16mm24mmParallel Co-RotatingTwin Screw Extruders78

Flexible Screw Profiles with Segmented ScrewsSpecifically designed for LabScale systems to maintain goodfree-volume to diameter ratioand channel depth79

Flexibility to Meet Process Requirements80

Twin Screw Agitator ElementsCONVEYINGMIXINGFeed Screws 30 deg Forward 60 deg Forward 90 deg Alternatezero 60 deg Reverse---- Star / Toothedzero Reverse Feed Screw-------- Access TSE Technology PPT81

PolyLab Twin Screw Extruder Models82

PolyLab PTW16 XL§ Horizontally split, with a lift-off topthat can be opened for ease ofcleaning, simple removal of thescrews and visualization of themelting process.§ The segmented top barrel part isbuilt with 4D modules to be easilyreconfigured by the user.§ Barrel segments are available forfeeding solids, liquids and forventing.83

PTW16 SpecificationsMax Temperature350ºC (optional 450ºC)Max Pressure100-150 Bar*Warm Up Time10 minutes averageMinimum Sample100 to 200 gramsMaximum ThroughputFrom 0.5 kg/hr - Up to 10 kg/hrMaximum Agitator Speed1100 rpmBarrel Length25:1 and 40:1 L/D ratioScrew Center Distance12.5mmScrew Channel Depth3.3mm* Use Melt Pump for higher pressure requirements84

PTW16 XL 25:1 15D extension§ Flexible Length: not all applications require along extruder, such as shear sensitivematerials and 25D is long enough for basicapplications.§ Optional 15D barrel extension to enhancee.g. residence time (for reactive extrusion) ormultiple feed ports,§ Easy to use and change - less than 15minutes by operator!§ Software recognizes the Extension unit85

Rheomex PTW16 OSTwin Screw barrel with25D and 15D extension86

PTW16 OS - Maximum flexibility . feed ports. Length . screw design . split barrel87

PTW16 OS - Maximum flexibility . Split Barrel88

PolyLab PTW24§ Horizontally split, with a clam-shellbarrel top that can be opened forease of cleaning, simple removal ofthe screws and visualisation of themelting process.§ The segmented top & bottom barrelparts is built with 4D modules to beeasily reconfigured by the user.§ Barrel segments are available forcooling feeding solids, liquids andfor venting.89

PTW24 with Melt Pump90

PTW24 with 3 Strand Pelletizing91

PTW24 SpecificationsMax Temperature400ºCMax Pressure100-150 Bar*Maximum ThroughputFrom 2.0 kg/hr - Up to 50 kg/hrMaximum Agitator Speed1000 rpmMax Power/Torque11 kW – 52 NmBarrel Length28:1 and 40:1 L/D ratioScrew Center Distance18.75mmScrew Channel Depth5.15mmCooling Water Required20 liters/min* Use Melt Pump for higher pressure requirements92

Rheomex PTW24 – AdvantagesSegmented screwSidefeedingExtruder barrel: segmented and hinged93

CTW100 Conical Twin Screw – counter rotatingSupporting 20 yearlegacy of CTW100systems with DockingStation OSCTW100 OS with PolyLab94

CTW100 – Barrel RemovalSimple and Quick Barrel Removal95

Rheomex CTW100p96

Screw Geometries for CTW100Venting screwIntensive mixing screwStandard screw97

FeedersThe world leader in serving scienceDetailed Feeder PPT

Why use Feeders for Twin Screw Extrusion?§ The quality of the dispersive mixing is highly dependent on both theextruder RPM and the flow rate from the Feeders§ Starved feeding is necessary for Venting operations§ Multiple Feeders have many applications: For sequential or simultaneous feeding of non-similar materials like pelletsand powders that might segregate if batch fed in one hopper For downstream feeding of heat or shear sensitive materials To easily control the ratio of multiple ingredients by varying the feed rates99

HAAKE Metering Feeder§ Designed specifically to work with PolyLab systems§ Multiple feeders can be stacked over extruder feed port§ Compact – Easy to Use§ Wide Feed Range – Pellets & Powder Insert§ Control via PolyLab or eding tubeMotor with gearboxMetering screwClosure for CleaningExtruder100

Stackable HAAKE Metering Feeders101

Mini Twin Screw Feeder§ Volumetric or Gravimetricversion available§ Feed Rates as low as 50 gramsper hour – smallest twin screwfeeder on the market§ Multiple Feed Tubes & Screwsavailable to match materialrequirements102

Dosing (RotoTube) Feeder§ Micro-Feeder for Fine Grainmaterials§ Volumetric and Gravimetricversions available§ Feed Rates as low as 30 gram perhour§ Tilting System and Anti-Vibrationsupports built-in103

Force FeederApplications: Sticky Materials:- food extrusion- dough / ceramic compounds Materials that tend to “bridge”- some PVC Dry Blends Non-Flowing MaterialMotor- shredded film (fluff)- soap powderHopperForceFeedingScrewExtruderBarrel104

Example – 2 Feed Ports, 3 Feeders & Stuffer105

Extrusion RheologyThe world leader in serving scienceRheology Principles PPTDetailed Explanations for how PolyLabis used to measure rheology data

PolyLab versus standard Piston Capillary Rheometers§ Advantages Lower “entry cost” to have capillary rheology dataLower overhead costs long term (space, maintenance, etc)Melted/Mixed multiple components directly to rheologyEliminate an additional melting heat history for melt mixed compoundsSimulates “real-world” processes more closelyAvailability of Slit die for lower shear ratesAvailability of X-Die and “wedge” die for Extensional Rheology§ Disadvantage Uses more material than a piston type capillary rheometer Shear Rate range with TSE – use Melt Pump option107

Complete Rheological CharacterizationFlowcurve LLDPE (220 C)10000Oscillation (RS Rheometer)Slit-Capillary (Rheocord)Viscosity1000Rod Capillary (Rheocord)100Molecular structure100.010.11Extrusion process10100Shearrate108Injection molding100010000100000

Extrusion Rheology Technique§ Extrusion Rheology requiresknowledge of the “shear stress”and “shear rate”.§ A well defined flow is created inthe Capillary Die which allowsthe pressure drop to beaccurately measured.§ The software uses this pressuredrop and the known geometry todetermine the shear stress.Slit Capillary Die§ ½ of the equation is now knownand next the “shear rate” portionmust be determined.Rod Capillary Die(higher shear rates)(lower shear rates)109

Extrusion Rheology Technique§ To determine the shear rate ½ of the equation, the volumetric flow ratemust be determined during the time interval the shear stress ismeasured.§ This can be done by weighing a timed interval sample in a variety ofmethods and then allowing the PolyCap software to use an input meltdensity to calculate the volumetric flow rate.§ Alternately, using a calibrated melt pump, the speed of the pumpdetermines the volumetric flow rate directly, independent of meltdensity. This is the optimal way to perform extrusion rheology butinvolves the significant cost of the melt pump.§ For occasional rheology needs, the weigh balance technique is by farthe most cost effective assuming the application need will tolerate thecompromises, like differing shear input due to ramping the extruderspeed to create different data point pairs.§ The PolyCap software also performs or applies corrections for entranceand exit effects (Bagley) and non-newtonian flow (Rabinowitsch).110

Extrusion Rheology Configurations15gPolyLab15gPolyLabPolyLabUsing any lab balance, sample ismanually Cut, Weighed, Input toPolyCap softwareUsing a balance connected toPolyLab, sample is manually Cut,weight auomatically goes intoPolyCapWith connected balance placedbeneath capillary die, extrudatecauses a weight gain with time thatPolyCap can detect either by: “HotKey” or Automatically.15g111

Extrusion Rheology ConfigurationsPro: all materials, lowest cost15gPolyLabCon: most labor/time intensivePro: works with any material15gPolyLabPolyLabCon: labor/time intensivePro: automatic mode only workswith materials that stay semi-molten15gCon: erroneous data if extrudate“pushes” on balance112

PolyLab / Melt Pump Setup for Capillary RheologyMelt Pump use providestotally automated testingwith constant extruderspeed (shear conditions)113

MeltPump OS§ Meters accurate flows and greatlydampens pressure pulsations andsurging§ Fully CAN controlled MeltPump§ 3 integrated CAN Temperaturecontrollers§ Digital Servo Motor for high accuracyeven at low speed (i.e. for accurate ratecontrol for viscosity tests at low shearrates)114

MeltPump OS§ Hand wheel for heightadjustment§ Remote control for manualspeed control§ Automatic speed control viamonitor software & capillarysoftware115

MeltPump OSExternal By-Pass Valve:§ MeltPump can be usedwith & without a By-Pass§ By-Pass can also beused independently fromthe MeltPump(i.e. for rheological testswith rigid PVC)116

Physical test methods – G’, G” f(ω)The viscosity spectra is measured with an axial oscillating rheometer in thepolymer melt. The sensor is mounted in a pressure port. (Ref.1) Themeasurement principle is oscillating squeeze flowPAVLabor117

Physical test methods– Extensional ViscosityUsing a patented die geometry (US6386016) with an extruder or melt pump,the shear viscosity and the elongation viscosity can be quantified. Thiscorrelates well with die swell. Example Ref 3 LDPE at 190 CDetailed Literature Available upon request118

Physical test methods– Extensional ViscosityLDPE: elongation die dataThus, the interest in usingthis data and measuringtechnique for processdevelopment and control.106shear / elongational viscosity [Pas]Extensional Properties ofpolymers are often showmuch greater change as anindication of morphology ormolecular weight changes.105150 C: elongation190 C: elongation104150 C: shear190 C: shear103selected working point for on-line control102110100shear / elongation rate [1/s]Hencky strain 3.35 for that die1191000

PressureExtensional Rheology Die - 0H2

Physical test methods – At-Line viscosity/MFIAt-line viscosity tests are performed with a capillary viscometer method (ΔP,ΔV). The melt is taken from the extruder and pumped in a separaterheometer (HAAKE ProFlow). Depending on the die used one can see MFR,viscosity curve or even extensional viscosity.Additional information available upon request121

The world leader in serving sciencePost ExtrusionTesting Options

Cast & Blown Film applications§ Application:Accessories Needed: Any PolyLab ExtruderDieTake-off UnitPressure sensor(Screen package)(OQT 512) Small production of filmsTesting the processibillityTesting of additivesTesting and optimization ofprocessing conditions§ Results / Specimens for: Cast Film Video(older TSR take-off)123Gel / Fish-Eye testingPigment distributionColorSurface qualityTensile / Impact testingWeathering

PostEx - Tape, Sheet and Ribbon Take-OffNew Sheet & Ribbon TakeOff- New design to be used withHaake and Prism products- Two Options:2-Roll Take Off3-Roll Take Off- Easy access to the rollers- Easy handling- Height adjustable- Adjustable speed ratio between thesteel rollers and the take-off rollers forslight drawing or orientation124

Optional Winder for TSR125

Tape, Sheet and Ribbon DieèDie width:25/50/100/150 mmèDie gap:adjustable(standard: 0.2-1.2 mm)126èfixed die gap on requestèMax. temperature: 360 Cè1 measuring port

Angled Adapter for Downwards Sheet Casting127

Tape, Sheet and Ribbon Die for PVC PVC Sheet dies: 50mm, 100mm, Height 1mm designed using Moldflow (FEM) Simulation Optimizied Flow - Compact design – Fixed Die Lip128

Cast film applicationPVC sheets: good & bad129

PostEx - Blown-Film Take-OffBlown film take-offPolyLab System with extruder130

Blown Film Die§§§§§adjustabledie gapRing diameter 25mm (35mm)Pin diameter 24mm (34mm)Gap width 0-0.8 mmMeasuring ports 2Max. temperature 480 CBlown Film VideoAir131

PolyLab Blown Film Optical TestingWith optical testing unit OQTStrobe LightBlown film take offCCD-CameraPolyLab System with extruder132

Optical Test Methods – Film Quality / GelsWith a chilled take-off roll the melt ispulled from a sheet die andtransported over a line camera. Thespots are detected and statisticallyevaluated.Camera systemBlown Film Video133

Optical Quality Testing SystemMeasuring principle:Strobe LightControl monitor forCCD Video signalPolymerfilmImage processorPC with evaluationsoftwareCCD - Camera134

OQT- Image display of defects135

OQT- Graphical display of defects136

Optical Quality Testing System OQT 512Technical data:Camera:Frequency:Test area:Resolution:Options:CCD Area Camera4 pictures /second20 x 20 mm (standard)60 µm ( 20 x 20 mm test area)10 x 10 mm test area(30 µm resolution)100 x 100 mm test area(100 µm resolution)Number of size classes: 20Detection levels:2(differentation of fisheyes and black specks)137

Optical Quality Testing System OQT FS5Technical data:Camera:Line length:Inspection width:Resolution:CCD Line Camera2048 pixels (standard)20 to 2000 mmfrom 10 µmNumber of size classes: 10Detection levels:3(differentation of fisheyes and black specks)138

Compounding / PelletizingTest results:§ Production of small quantitiesof test materials for:Accessories Required:§ Any PolyLab extruder§ Pressure sensors§ (Screen pack - optional)§ Rod die Injection Molding Customer Trials & Samples Additive trials Horizontal Vertical Multistrand die§ Masterbatch development§ Processability of newpolymers§ Optimization of processingconditions§ Strand Cooling Waterbath Air Cooled Conveyer§ Pelletizer Strand type Die Face139

Rod/Strand Dies – Horizontal & Vertical§ Universal die for extrudability tests§ Strands for Pelletizing§ Nozzles available from:1mm - 6mm§ Two sensor ports for pressure- andtemperature-measurement§ Multi-Strand horizontal die also availablefor higher output pelletizingtesting of Processingadditives (Dynamar) atDyneon (NL) which preventbuild up at die exit.EPPM info nr. 34 6,3 / p12 (2004)140

Compounding / PelletizingVariCut PelletizerPelletizing Video141

Profile / Rubber ExtrusionAccessories Required:§ Any PolyLab Extruder§ Pressure sensor(s)§ Profile or Garvey die§ Conveyor beltTest results:§ Testing of the processability ofrubber,

Multi Range Torque Sensor 400Nm / 120Nm §Strain gauge principle §Dynamical Resolution Enhancement 60 Nm : 0.01 Nm 60 Nm : 0.1 Nm §Dual torque Sensors §The PolyLab Torque Sensor has non contact digital data transmission from shaft to casing (no brushes, no collector ring). This means no failure of transmission and it is maintenance free.