gel troubleshooting - tappi...• automatic die control • static mixer position • hang ups in...
TRANSCRIPT
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2007 PLACE Conference
September 16-20
St Louis, MO
Gel Troubleshooting
Presented by:Lou PifferSenior Sales EngineerDavis-Standard, LLC
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Definition of a Gel• Film Imperfections or defects developed
during forming due to disturbances in the polymer flow
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Classification of Film Imperfections
• Contamination• Un-melt• Un-mix• Thermal degradation
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OriginsGels can be created or introduced
during • Polymerization• Equipment-Screw Design• Fabrication
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Contamination
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Gauge Bands/Gels
• Contamination– Fiber
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Fiber Gel After Melting
Gel
Polarized light (w/ 1/4 filter)
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Gauge Bands/Gels
• Contamination– Fiber– Resin Contamination
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Resin Contamination
• Polyolefin• More Crystalline• Thermally stable• Adhesion through
oxidation• 600°F - 630°F
processing temperature
• Acid functional groups
• Less Crystalline• Not thermally stable• Adhesion through
vinyl acetate groups• 450°F processing
temperature
LDPE EVA
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Cross Contamination Solutions
• Better Housekeeping• Better purging• Work with resin companies
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Gauge Bands/Gels
• Contamination– Fiber– Resin Contamination
• Un-melt and un-mix
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Hot Stage Microscopy
• Slowly heat sample to above melting point.
• Transmit light through cross-polarized filters.
• Observe melting point of film/gel and note any birefringence effects.
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5050°°CC 150150°°CC 5050°°CC
Unmixed GelUnmixed Gel
Unmixed Gel Characterization
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Gauge Bands/Gels
• Contamination– Fibers– Cross contamination w/other Polymers
• Un-melt & un-mixed– Bad Concentrate
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MixingMaster Batch Concentrates
• Compatibility of base resin• quality of dispersive mixing
– agglomerates
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Gauge Bands/Gels
• Contamination– Fibers– Cross contamination w/other Polymers
• Un-melt & un-mixed– Bad Concentrate– Blends with different melting rate
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MixingPolymer Blends and Additives
• Thermodynamic compatibility of components (conductivity)
• Large differences in melting points of blend components
• Large viscosity ratios between minor and major components
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Gauge Bands/Gels
• Contamination– Fibers– Cross contamination w/other Polymers
• Un-melt & un-mixed– Bad Concentrate– Blends with different melting rate– Fluff
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Contiguous Solids Melting
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Gauge Bands/Gels
• Contamination– Fibers– Cross contamination w/other Polymers
• Un-melt & un-mixed– Bad Concentrate– Blends with different melting rate– Fluff– Bad temperature profile
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Gauge Bands/Gels
• Contamination– Fibers– Cross contamination w/other Polymers
• Un-melt & un-mixed– Bad Concentrate– Blends with different melting rate– Fluff– Bad temperature profile– Inconsistent granular size
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Gauge Bands/Gels
• Contamination– Fibers– Cross contamination w/other Polymers
• Un-melt & un-mixed– Bad Concentrate– Blends with different melting rate– Fluff– Bad temperature profile– Inconsistent granular size– Screw design
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Screw Design
• Improper design for the resin can contribute to:– SBB causing encapsulation of un-melt
solids– SBB also causes non uniform mixing
history– Not providing enough shear to melt resin
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CONVENTIONALSCREW
MELTPOOL
Observed Solid Bed Break-up
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Gauge Bands/Gels
• Contamination– Fiber– Resin Contamination
• Un-melt and un-mix• Thermal degradation
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Polymer Degradation is a Function of
Time
Shear Conditions
Temperature
All polymers degrade as a function of time, temperature, and shear conditions
Degradation Gels
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Types of Polymer Degradation
• Thermal - High temperatures• Chain Scission - High stress fields• Cross-linking - Un-saturation• Oxidation - Oxygen
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Example of crosslinking
O
C
CH3
O
m
O
C
CH3
O
m
HeatO
C
CH3
O
m
*
O
C
CH3
O
m
• Ethylene Vinyl Acetate (EVA)– -(CH2-CH2)m-(CH-CH3COO)-
• Temperature causes decarboxylation which result in releasing Acetate, CO2, and primary free radicals
Free Radical
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EVA Degradation
• Creates acetic acid at LDPE process temperatures.
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EVA - Effect of Over Heating...
O
C
CH3
O
m
O
C
CH3
O
m
HeatO
C
CH3
O
m
*
O
C
CH3
O
m
• Ethylene Vinyl Acetate (EVA)– -(CH2-CH2)m-(CH-CH3COO)-
• Temperature causes decarboxylation which result in releasing Acetate, CO2, and primary free radicals
Free Radical
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Side Reaction
O
C
CH3
O
m
* O
C
CH3
O
m
O
C
CH3
O
m
m+
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5050°°CC
MeltMelt
150150°°CC
Lightly crosslinkedLightly crosslinked
5050°°CC
Lightly Crosslinked Gel
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What does crosslinked mean?
• Too much energy provided to the polymer.
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Too much heat
• Shear
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Cross Section of Single-Screw ExtruderCross Section of Single-Screw Extruder
Z6-----------------------------------------------------------------------------Z1
drive
gearbox
solidfluid/solidstate of material: fluid
melt generator melting/plasticating
conveying
output and metering zonealternative-mixing
transition orcompression
feed zonepressureutilize
melt generator
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Too much heat
• Shear• Heaters
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Too much heat
• Shear• Heaters
– T/C not in bottom of well
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T/C Location
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Too much heat
• Shear• Heaters
– T/C not in bottom of well• Extruder Residence time
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drive
heaters-coolers
cooling
screw
HEAT TRANSFER IN AN EXTRUDER
Enthalpy of
Resin
Mechanical
Energy
Heat in/Cold out
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Gel Hang-up at adapter
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Gauge Bands/Gels
• Fibers/Contamination• Cross contamination w/other Polymers• Un-melt• Cross-Linked• Oxidation
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Oxidized Gel
Gel
Oxidized Gel at 130 C with polarized light (w/ 1/4 filter)
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Oxidized Gels
• Formed very rapidly in the presence of oxygen
• Corrective Action– Improve stabilizer package– Reduce exposure to oxygen during
processing– Reduce Temperature
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Oxidation of resin
• Incorrect shut down (not capping die)• Incorrect start-up with cleaned die
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Gauge Bands/Die Lines
• Hang up of gels • Temperature variation• Automatic die control• Static Mixer position• Hang Ups in flow path
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Gel Hang-up at adapter
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Solving Gel Problems• Identify the source of the Imperfection
– Un-melt– Degradation (Cross link or Oxidized)– Contamination (Dust, Dirt, Fiber)– Agglomeration (Color, Additives)
• Find the Source– Resin– Equipment– Blends/Additives
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Tools to detect gel problems
• Hot stage microscopy• IR analysis• Chemical Analysis• DSC unit
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Thank YouPRESENTED BY
Lou PifferSenior Sales EngineerDavis-Standard, LLC
Please remember to turn in your evaluation sheet...