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Gel Troubleshooting

The document summarizes common causes of gels in plastic film production, including contamination, incomplete melting and mixing, thermal degradation, oxidation, and equipment issues. It discusses how gels can form from fiber contamination, cross-contamination between resins, poorly dispersed masterbatch concentrates, polymer blends with different melting properties, screw design problems, excessive temperature, shear or residence time in the extruder, oxidation during processing, and residual gels hanging up in the film die. Methods for identifying and addressing specific gel causes are also reviewed.

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88 views57 pages

Gel Troubleshooting

The document summarizes common causes of gels in plastic film production, including contamination, incomplete melting and mixing, thermal degradation, oxidation, and equipment issues. It discusses how gels can form from fiber contamination, cross-contamination between resins, poorly dispersed masterbatch concentrates, polymer blends with different melting properties, screw design problems, excessive temperature, shear or residence time in the extruder, oxidation during processing, and residual gels hanging up in the film die. Methods for identifying and addressing specific gel causes are also reviewed.

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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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2007 PLACE

Conference
September 16-20
St Louis, MO

Gel Troubleshooting

Presented by:
Lou Piffer
Senior Sales Engineer
Davis-Standard, LLC
Definition of a Gel
• Film Imperfections or defects developed
during forming due to disturbances in
the polymer flow
Classification of Film
Imperfections
• Contamination
• Un-melt
• Un-mix
• Thermal degradation
Origins
Gels can be created or introduced
during
• Polymerization
• Equipment-Screw Design
• Fabrication
Contamination
Gauge Bands/Gels
• Contamination
– Fiber
Fiber Gel After Melting

Gel

Polarized light (w/ 1/4 filter)


Gauge Bands/Gels
• Contamination
– Fiber
– Resin Contamination
Resin Contamination
LDPE EVA
• Polyolefin • Acid functional
• More Crystalline groups
• Thermally stable • Less Crystalline
• Adhesion through • Not thermally stable
oxidation • Adhesion through
• 600°F - 630°F vinyl acetate groups
processing temperature
• 450°F processing
temperature
Cross Contamination Solutions
• Better Housekeeping
• Better purging
• Work with resin companies
Gauge Bands/Gels
• Contamination
– Fiber
– Resin Contamination
• Un-melt and un-mix
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.
Unmixed Gel Characterization

50°C 150°C 50°C

Unmixed Gel
Gauge Bands/Gels
• Contamination
– Fibers
– Cross contamination w/other Polymers
• Un-melt & un-mixed
– Bad Concentrate
Mixing
Master Batch Concentrates
• Compatibility of base resin
• quality of dispersive mixing
– agglomerates
Gauge Bands/Gels
• Contamination
– Fibers
– Cross contamination w/other Polymers
• Un-melt & un-mixed
– Bad Concentrate
– Blends with different melting rate
Mixing
Polymer Blends and Additives
• Thermodynamic compatibility of
components (conductivity)
• Large differences in melting points of
blend components
• Large viscosity ratios between minor
and major components
Gauge Bands/Gels
• Contamination
– Fibers
– Cross contamination w/other Polymers
• Un-melt & un-mixed
– Bad Concentrate
– Blends with different melting rate
– Fluff
Contiguous Solids Melting
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
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
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
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
Observed Solid Bed Break-up

MELT
POOL

CONVENTIONAL
SCREW
Gauge Bands/Gels
• Contamination
– Fiber
– Resin Contamination
• Un-melt and un-mix
• Thermal degradation
Polymer Degradation is a
Function of
Time Temperature

Shear Conditions

All polymers degrade as a function of


time, temperature, and shear conditions
Degradation Gels
Types of Polymer Degradation
• Thermal - High temperatures
• Chain Scission - High stress fields
• Cross-linking - Un-saturation
• Oxidation - Oxygen
Example of crosslinking
m

• Ethylene Vinyl Acetate (EVA) O


C O
– -(CH2-CH2)m-(CH-CH3COO)- CH3

• Temperature causes
decarboxylation which result in
releasing Acetate, CO2, and primary
m

free radicals
m
O
m

C O
O CH3 O*
Heat
C O O
FreeC Radical
CH3 CH3
EVA Degradation
• Creates acetic acid at LDPE process
temperatures.
EVA - Effect of Over Heating...
m

• Ethylene Vinyl Acetate (EVA) O


C O
– -(CH2-CH2)m-(CH-CH3COO)- CH3

• Temperature causes
decarboxylation which result in
releasing Acetate, CO2, and primary
m

free radicals
m
O
m

C O
O CH3 O*
Heat
C O O
FreeC Radical
CH3 CH3
Side Reaction
m m

m
m

+
O* O O
C O C O C O
CH3 CH3 CH3
Lightly Crosslinked Gel

50°C 150°C 50°C

Melt Lightly crosslinked


What does crosslinked mean?
• Too much energy provided to the
polymer.
Too much heat
• Shear
Cross
Cross Section
Section of
of Single-Screw
Single-Screw
Extruder
Extruder

state of material: fluid fluid/solid solid

melt generator melting/plasticatin conveying


g
gear
box

Z6-----------------------------------------------------------------------------Z1
pressure
output and metering zonetransition
utilize or feed zone drive
alternative-mixing
compression
melt generator
Too much heat
• Shear
• Heaters
Too much heat
• Shear
• Heaters
– T/C not in bottom of well
T/C Location
Too much heat
• Shear
• Heaters
– T/C not in bottom of well
• Extruder Residence time
Heat in/Cold HEAT TRANSFER IN
out AN EXTRUDER
heaters-coolers

cooling Mechanical

Enthalpy of screw Energy

Resin
drive
Gel Hang-up at adapter
Gauge Bands/Gels
• Fibers/Contamination
• Cross contamination w/other Polymers
• Un-melt
• Cross-Linked
• Oxidation
Oxidized Gel

Gel

Oxidized Gel at 130 C with polarized light (w/ 1/4 filter)


Oxidized Gels
• Formed very rapidly in the presence of
oxygen
• Corrective Action
– Improve stabilizer package
– Reduce exposure to oxygen during
processing
– Reduce Temperature
Oxidation of resin
• Incorrect shut down (not capping die)
• Incorrect start-up with cleaned die
Gauge Bands/Die Lines
• Hang up of gels
• Temperature variation
• Automatic die control
• Static Mixer position
• Hang Ups in flow path
Gel Hang-up at adapter
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
Tools to detect gel problems
• Hot stage microscopy
• IR analysis
• Chemical Analysis
• DSC unit
Thank You
PRESENTED BY

Lou Piffer
Senior Sales Engineer
Davis-Standard, LLC

Please remember to turn


in your evaluation sheet...

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