Sheet Extrusion Processing Guide

This information is intended for use only as a guide for the manufacture of Ingeo™ biopolymer sheet ranging between 8 – 50
mils (0.2 – 1.3 mm). Ingeo is generally not recommended for producing sheet less than 8 mils (0.2 mm) and the production of
heavy gauge sheet requires special consideration to heat transfer and sheet pinning systems. Because extrusion of Ingeo
sheet is complex, an experimental approach may be required to achieve optimal results.

1.0 Safety and Handling Precautions

All safety precautions normally followed in the handling and processing of melted thermoplastics should be followed.

As with most thermoplastics, melt processing and the variability of those conditions may result in minor decomposition.
Lactide, a non-hazardous gaseous irritant, is a minor by-product of Ingeo melt processing. Appropriate air testing should be
completed to ensure an acceptable Threshold Limit Value (TLV) of less than 5 mg/m3 is maintained. The use of process area
point source remediation measures such as monomer fume hoods or exhausts near the die are typically recommended.

Molten Ingeo is lower viscosity and sticks more readily to cloth, metal, brass and wood compared to other molten
thermoplastics. Be prepared for this when cleaning die faces, collecting molten patties and emptying purge containers. A
molten web will not release cleanly from a gloved hand so use caution when grabbing any stream or patty of Ingeo biopolymer.

Ingeo biopolymer is considered non-hazardous according to DOT (US Department of Transportation) shipping regulations.
When handling Ingeo resin at room temperature avoid direct skin and eye contact along with conditions that promote dust
formation. For further information, consult the appropriate MSDS for the grade being processed.

As with any melted thermoplastic waste, melted Ingeo waste should be allowed to cool before being placed into any waste
container to minimize fire risks.

2.0 Pellet Storage and Blending Recommendation

Ingeo resins should be stored in an environment designed to minimize moisture uptake. Product should also be stored in a
cool place at temperatures below 122°F (50°C).

Product that is delivered in cartons or super sacks should be kept sealed until ready for loading into the blending and/or drying
system. Bulk resin that is stored in closed silos and hoppers for extended periods (more than 6 hrs) should be kept purged
with dry air or nitrogen to minimize moisture gain. In the case of outside storage, if the product is supplied in boxes or other
non-bulk containers, the unopened container should be brought into the extrusion production area and allowed to equilibrate
for a minimum of 24 hours before opening to prevent excessive condensation.

3.0 Resin Properties

NatureWorks 2003D is the recommended Ingeo resin grade for sheet production intended for thermoforming applications.
Typical properties of 2003D are shown in the following table.

Resin Property Nominal Value

RV 3.9 – 4.1
Melting Point, °F (°C) 300 – 320 (150 – 160)
Glass Transition Temperature, °F (°C) 136 (58)
Crystallization Temperature, °F (°C) 212 – 248 (100 – 120)

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4.0 Materials of Construction

All metal parts in the extrusion process that are subjected to stagnant flow areas with molten polymer should be constructed of
stainless steel to minimize corrosion. This includes melt pump and filter assemblies and some transfer lines. Furthermore,
Ingeo biopolymer should not be left in the extruder, polymer filter, polymer transfer lines, dies or any other part of the extrusion
system at recommended or higher melt temperatures for extended periods. Below is a guideline for the recommended types of
steel that should be used in the extrusion system.

Part Steel Type

Melt pumps and bearings SUS440B
Pump blocks SUS631
Transfer lines SUS440C
Die Hard Chrome plated tool steel

If twin-screw extrusion with vacuum vent drying is used, SUS440C or similar corrosion-resistance material should be used for
screw elements, vacuum vent lines, and trap components. Contact your NatureWorks LLC Technical representative, for
additional recommendations on proper handling of lactide gasses and trapped lactide.

5.0 Drying
Ingeo resin can be successfully dried using most standard drying systems. Recommended conditions are provided for
standard desiccant based column dryers. For other drying system designs, additional information can be provided upon
request.

To prevent equipment corrosion, it is not recommended to dry or store hot Ingeo resin in carbon steel vessels (see Section
2.0).

In-line drying is essential. It is recommended that Ingeo biopolymer should be dried to a maximum of 250 ppm of moisture as
measured by a Karl Fischer method. A moisture level lower than 250 ppm will positively affect the stability of the biopolymer
and will increase the viscosity stability over time at elevated temperatures. Processes that have unusually long residence
times or result in melt temperatures greater than 465°F or 240°C should only extrude Ingeo biopolymer at moisture levels less
than 50 ppm for maximum retention of molecular weight and physical properties. Material is supplied in foil-lined containers
dried to less than 400 PPM as measured by NatureWorks LLC internal method. The resin should not be exposed to
atmospheric conditions after drying. Keep the package sealed until ready to use and promptly dry and reseal any unused
material. The drying table below can be used to estimate the drying time needed. Air or nitrogen based desiccant drying
systems can be used at the recommended temperatures. Typical Ingeo drying conditions are shown in the following table.

Typical Ingeo Raw Material Drying Conditions

Typical Settings
Dry pellets Pellets with
received in 2000 ppm
Drying Parameter barrier liner moisture
Residence Time (hours) 2 4
Air Temperature °F (°C) 194 (90) 194 (90)
Air Dew Point °F (°C) - 40 (-40) - 40 (-40)
Air Flow Rate, CFM/lb resin (m3 / hr - kg resin) > 0.5 (1.85) > 0.5 (1.85)

Typical desiccant dryer regeneration temperatures exceed the melt point of Ingeo resins. To prevent issues with pellet
bridging, sticking or melting, the drying system should be verified to ensure temperature control is adequate during operation
as well as during regeneration cycles since valve leakage is common in many systems.

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6.0 Melt Extrusion

Prior to introducing Ingeo biopolymer into any melt processing system, the system should be properly cleaned and purged to
prevent any polymer cross contamination. Insure that the feeding & blending equipment is thoroughly cleaned & free from dust
and contamination and all metal magnets have been wiped clean. Insure that all hang-up areas such as elbows transitions
drain ports, filters and slide gates have all previously run dust and granules completely removed. The purging procedures
below are recommended for optimal removal of other polymers.

6.1 Ingeo Biopolymer Purging Procedure

Following PP or PS in your system

1. Introduce a high melt flow PP (5 - 8 MFR) or PS (6 –10) first at normal PP or PS conditions, then reduce
temperatures to recommended Ingeo temperatures. Purge for at least 7x average residence time. Let system empty
as much as possible.
2. Turn off extruder and completely clean all hoppers, elbow, slide gates, dryers, hopper loaders bins, hopper loader
filters and material conveying lines of residual PP. Load Ingeo into material handling system.
3. Transition to Ingeo biopolymer and purge, again, for a minimum 7x the average residence time. Change screen pack
when it becomes obvious that primarily Ingeo is exiting the die.
4. At the completion of a trial run, purge all Ingeo from the extrusion system, using a moderate to low melt index PP or
PS.

Following PET, PA, or HDPE in your system

1. It is critical to clean the material handling system of PET, nylon and high molecular weight HDPE to assure that these
materials do not inadvertently feed into the extruder during or after the purging process.
2. Purge with low MFR (e.g., <1) transition resin at normal PET operating temperatures. PET and Ingeo are temperature
incompatible, so the transition resin is one that can be processed at the high temperatures of PET and the low
temperatures of Ingeo. Suggested transition resins include PP, crystal PS, and PETG. Purge for at least 7x average
residence time, much of the time at the typical PET production rate. (~30 minutes). Let system empty as much as
possible. Clean out the hopper as much as possible.
3. Introduce a higher melt flow transition resin of the same type (5 - 8 MFR) and change to normal Ingeo operating
temperatures. Ingeo is a relatively low viscosity resin, so the grade of transition resin that is viscous enough to push
PET or nylon out of the extruder at the high extrusion temperatures will be too viscous for Ingeo to push it out at the
lower extrusion settings. This is why a transition to a higher melt flow transition resin is suggested: to have a viscous
version to push out the PET, PA or HDPE and a low viscosity version that the Ingeo will push out well.
4. Purge for at least 7x average residence time. Let system empty as much as possible.
5. Extrusion operations familiar with PETG processing may find success purging using a single PETG grade (similar to
Eastman copolymer 6763) for a minimum of 40 minutes. Then reduce temperatures to Ingeo conditions.
6. Turn off extruder and completely clean all hoppers, elbow, slide gates, dryers, hopper loaders bins, hopper loader
filters and material conveying lines of residual resin pellets, flake, dust, and floss. Load Ingeo into material handling
system.
7. Transition to Ingeo and purge, again, for a minimum 7x the average residence time. Change screen pack when it
becomes obvious that primarily Ingeo is exiting the die. Be sure to flush screen pack completely during the change.
Screen pack should be between 40- 125 mesh for optimal performance. The lower mesh screen will result in reduced
melt temperatures exiting the die.
8. At the completion of a trial run, purge all Ingeo from the extrusion system, using a moderate to low melt index resin
that processes well between 400 and 450°F (205-230°C), initially using the Ingeo temperature settings and extrusion
rates.

Notes:
1. It is critical that all drying and conveying/receiving systems be free of all PET and vacuumed to ensure that there is
no remaining polymer dust, before adding Ingeo biopolymer. PET will not melt at Ingeo operating temperatures and
will block screens, if it is present in the system.

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6.2 Extrusion
A general-purpose single-screw extruder, 24 to 36:1 L/D with feed-throat cooling is acceptable for processing Ingeo.
Generally, shorter extruders will result in a lower melt temperature and less sag at the exit of the die. A mixing section is
generally recommended along with static mixers in the product line prior to the die to ensure temperature uniformity as well as
optimum additive dispersion and melt polymer homogeneity. For single-screw extrusion systems, melt pumps are
recommended for sheet profile consistency. The following table shows a typical melt profile for Ingeo.

Typical Ingeo Biopolymer Extrusion Conditions

Standard Temperature Reverse Temperature
Section Profile, °F (°C) Profile, °F (°C)
Feed throat 113 (45) 113 (45)
Zone 1 355 (180) 430 (220)
Zone 2 375 (190) 410 (210)
Zone 3 390 (200) 390 (200)
Melt pump 390 (200) 390 (200)
Die 375 (190) 375 (190)

Note 1: In some instances where the extruder contains a screw not specifically designed for Ingeo biopolymer, a reverse
temperature profile has proven to be beneficial to reduce melt temperature and reduce extruder motor load.

Note 2: Temperatures are only starting points and may need to be altered. Target Ingeo melt temperatures (after melt pump)
should be in the range of 210±10°C (410±20°F). Ingeo resins should not be processed at temperatures above 240°C (464°F)
due to excessive thermal degradation.

6.3 Additives
Color concentrates, slip and anti-block agents are best added as a masterbatch at 15-30 wt% in Ingeo resins and controlled
dosing the required amount of dried masterbatch into the feed throat of the running extruder. Some potential additives are
inappropriate for extrusion with Ingeo because they are hygroscopic or hydrated salts (e.g. calcium carbonate) that would lead
to severe Ingeo molecular weight degradation and property loss.

6.4 Filtration
Standard screen pack configurations are recommended to protect melt pumps and dies from incidental contamination that may
occur during material handling. Screen mesh sizes of 40 - 125 mesh are generally sufficient. Finer filtration leads to excessive
shear-heating with Ingeo and should be avoided.

7.0 Sheet Casting

Most conventional sheet dies have successfully been used to extrude Ingeo sheet. External deckles should be avoided if
possible since there is the possibility of resin degradation behind the deckles. This will lead to a constant supply of low Mw
resin at the edge and may result in edge instability. The die gap should be set at approximately 10% greater thickness, or
alternatively 1 to 2 mils more (25-50 microns more) than the desired sheet thickness. It is very important to establish a flat
extrudate from a well adjusted die gap when pneumatic nips are used at the casting and polishing roll stand. A hydraulic nip
will be better suited to flatten the web (resulting from an inconsistent die gap across the die width) than will a pneumatic nip
because the pressure required to exert flatness becomes greater than a pneumatic nip is capable of especially with lighter
gauges of sheet (i.e., 10-15 mils or 250 to 375 microns).

Sheet forming is generally accomplished on a 3-roll stack. Vertical, inclined and horizontal roll stacks have all been used.
Since Ingeo has lower melt strength than conventional plastics, there is a slight advantage to inclined and horizontal roll stacks

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particularly at very high extrusion outputs. The initial roll gap should be approximately 1-inch (25-cm) lower than the die gap to
accommodate the slight droop that is common with Ingeo. The molten Ingeo web should contact the lower roll of the initial roll
gap as close as possible to the gap (nip point). This will reduce the possibility of air entrapment between the sheet and the roll
which will result sheet defects. Hydraulic roll stands are preferred to pneumatic since high nip pressures are possible. Ingeo
tends to solidify quickly. Approximately 800 – 900 pounds/linear inch of die (PLI) are required to prevent floating of the rolls
which would lead to an uneven polish. Pneumatic nips can be used but uniform die flow is required. Also, the pneumatic gap
needs to be set evenly at the desired final sheet thickness. In either case, Ingeo does not run well with a large bank at the gap.

Temperature profiles vary depending upon the output, melt temperature and roll diameters but in general, good starting points
for the roll control set point are:

Top roll 80 F / 25 C

Middle roll 100 F / 38 C

Bottom roll 120 F / 50 C

Excessive buildup of residual lactide can occur on the top and middle roll if there is not intimate contact between the molten
web and two rolls. Both gap management (adjust the die gap for uniformity across the die and adjust the nip gap) and low roll
temperatures can contribute to this. Of course, a too high a temperature will result in the web sticking to the rolls and give poor
quality sheet.

Because of Ingeo biopolymer’s inherent lower melt strength, the die should be positioned as close to the entrance nip as
possible and preferably slightly higher than the nip. This will minimize any early contact of the web onto the middle chill roll that
will result in air entrapment that results in small air bubbles and subsequent visual defects in the sheet. Ideally, the web should
contact the middle roll just as the web is entering the nip of the middle and top roll. The best quality sheet is achieved when
there are no or very minimal rolling banks at the top nip of the roll stand.

The thermal properties of Ingeo biopolymer, sheet thickness, line speed, and the heat transfer characteristics of the rolls will
dictate the maximum output rate of a particular roll stack. Ingeo pellets and sheet have the following thermal properties:

Glass Transition Temperature 136°F (58°C)

Amorphous 0.075 (3.1 x 10-4)
Thermal Conductivity, BTU/ ft-hr-°F (cal / cm-sec-°C)
Crystalline 0.11 (4.5 x 10-4)
Below Tg 0.29 (0.29)
Specific Heat, BTU/ lb °F (cal / g °C)
Above Tg 0.51 (0.51)

When making thinner gauge sheet (less than 15 mils or 0.38 mm), hydraulic nips are required to achieve a uniform polish on
the sheet. Pressures in the vicinity of 900 pounds / linear inch (160 kg / linear cm) of die are necessary to overcome the
viscosity of the rapidly cooling polymer.

8.0 Web Handling and Slitting

The stiffness of Ingeo is similar to PS and quite higher than either PP or even PET. Be careful of sharp edges particularly on
thick cast sheet. Heavy leather gloves should be worn to minimize the risk of cuts. The material also has high yield strength
and good tension control between unit operations is imperative. Edge trim is easily slit with rotary shear knives. In general,
razor knives give unacceptable performance, yielding a rough edge and numerous web breaks. If razor knives are used, the
cutting bed should be supported and the sheet should be slightly warm (about 125°F or 50°C).

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9.0 Regrind
Ingeo biopolymer regrind from edge trim and skeleton reclaim can be added back into the process provided that the regrind is
dry. A maximum of 40% amorphous regrind is recommended to ensure smooth extrusion operation. In addition, screw cooling
should be used through the first two flights of the transition zone (in single screw extrusion) when extruding amorphous regrind
to eliminate the possibility of material sticking to the screw and causing a screw blockage. Amorphous regrind can be
reincorporated as relatively dry material if the time period between exudation from the die as sheet and input of the ground
sheet into the extruder throat is just a few minutes. Amorphous regrind that has absorbed 2000 ppm moisture from the
atmosphere will require drying times of about 12 hours at 115°F (45°C) to approach 250 to 400 ppm moisture content. In warm
humid climates, the dryer may not be capable of drying the flake to 250 ppm at these low temperature settings necessary to
avoid agglomeration.

Twin-screw extrusion systems typically are less prone to sticking during extrusion and higher levels of amorphous
recycle/regrind.

Crystallized regrind has been added back to the process up to 100% with no loss of either process control or sheet properties.
Crystallizers should be operated at 100 C (212 F) and flake bed should be agitated sufficiently to prevent blocking. As with all
crystallizers, the unit should be seeded with previously crystallized pellets or flake and allowed to come to steady state before
amorphous material is fed into the unit.

©2015 NatureWorks LLC. All rights reserved. The information provided herein is provided in good faith, but no warranties,
express or implied, are provided with respect thereto. It is the responsibility of the users of Ingeo resin to determine the proper
conditions of use on their particular equipment and at their particular facilities. No rights under any patent of NatureWorks LLC
or any third party is granted or implied.

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Safety and Handling Considerations highly flammable, easily ignited by spark or flame, and can
also auto ignite. For polyesters such as PLA, thermal
Safety Data Sheets (SDS) for Ingeo biopolymers are decomposition producing flammable vapors containing
available from NatureWorks. SDS’s are provided to help acetaldehyde and carbon monoxide can occur in almost
customers satisfy their own handling, safety, and disposal any process equipment maintaining PLA at high
needs, and those that may be required by locally temperature over longer residence times than typically
applicable health and safety regulations. SDS’s are experienced in extruders, fiber spinning lines, injection
updated regularly; therefore, please request and review molding machines, accumulators, pipe lines and adapters.
the most current SDS’s before handling or using any As a rough guideline based upon some practical
product. experience, significant decomposition of PLA will occur if
polymer residues are held at temperatures above the
The following comments apply only to Ingeo biopolymers; melting point for prolonged periods, e.g., in excess of 24
additives and processing aids used in fabrication and hours at 175°C, although this will vary significantly with
other materials used in finishing steps have their own temperature.
safe-use profile and must be investigated separately.
Combustibility
Hazards and Handling Precautions
Ingeo biopolymers will burn. Clear to white smoke is
Ingeo biopolymers have a very low degree of toxicity and, produced when product burns. Toxic fumes are released
under normal conditions of use, should pose no unusual under conditions of incomplete combustion. Do not permit
problems from incidental ingestion or eye and skin dust to accumulate. Dust layers can be ignited by
contact. However, caution is advised when handling, spontaneous combustion or other ignition sources. When
storing, using, or disposing of these resins, and good suspended in air, dust can pose an explosion hazard.
housekeeping and controlling of dusts are necessary for Firefighters should wear positive-pressure, self-contained
safe handling of product. Pellets or beads may present a breathing apparatuses and full protective equipment.
slipping hazard. Water or water fog is the preferred extinguishing medium.
Foam, alcohol-resistant foam, carbon dioxide or dry
No other precautions other than clean, body-covering chemicals may also be used. Soak thoroughly with water
clothing should be needed for handling Ingeo biopolymers. to cool and prevent re-ignition.
Use gloves with insulation for thermal protection when
exposure to the melt is localized. Workers should be
Disposal
protected from the possibility of contact with molten resin
during fabrication. DO NOT DUMP INTO ANY SEWERS, ON THE
GROUND, OR INTO ANY BODY OF WATER. For unused
Handling and fabrication of resins can result in the or uncontaminated material, the preferred option is to
generation of vapors and dusts that may cause irritation to recycle into the process otherwise, send to an incinerator
eyes and the upper respiratory tract. In dusty or other thermal destruction device. For used or
atmospheres, use an approved dust respirator. contaminated material, the disposal options remain the
same, although additional evaluation is required. Disposal
Good general ventilation of the polymer processing area is must be in compliance with Federal, State/Provincial, and
recommended. At temperatures exceeding the polymer local laws and regulations.
melt temperature (typically 175ºC), polymer can release
fumes, which may contain fragments of the polymer, Environmental Concerns
creating a potential to irritate eyes and mucous
membranes. Good general ventilation should be sufficient Generally speaking, lost pellets, while undesirable, are
for most conditions. Local exhaust ventilation is benign in terms of their physical environmental impact, but
recommended for melt operations. Use safety glasses (or if ingested by wildlife, they may mechanically cause
goggles) to prevent exposure to particles, which could adverse effects. Spills should be minimized, and they
cause mechanical injury to the eye. If vapor exposure should be cleaned up when they happen. Plastics should
causes eye discomfort, improve localized fume exhausting not be discarded into the environment.
methods or use a full-face respirator.
Product Stewardship
The primary thermal decomposition product of PLA is
NatureWorks has a fundamental duty to all those that use
acetaldehyde, a material also produced during the thermal
our products, and for the environment in which we live.
degradation of PET. Thermal decomposition products also
This duty is the basis for our Product Stewardship
include carbon monoxide and hexanal, all of which exist
philosophy, by which we assess the health and
as gases at normal room conditions. These species are

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environmental information on our products and their standpoint of human health and environmental quality. To
intended use, and then take appropriate steps to protect help ensure our products are not used in ways for which
the environment and the health of our employees and the they were not intended or tested, our personnel will assist
public. customers in dealing with ecological and product safety
considerations. Your sales representative can arrange the
Customer Notice proper contacts. NatureWorks literature should be
consulted prior to the use of the company’s products.
NatureWorks encourages its customers and potential
users of its products to review their applications from the

NOTICE:
No freedom from infringement of any patent owned by NatureWorks LLC or others is to be inferred. No information in this
publication can be considered a suggestion to infringe patents.

The technical information, recommendations and other statements contained in this document are based upon tests or
experience that NatureWorks believes are reliable, but the accuracy or completeness of such information is not guaranteed.
Many factors beyond NatureWorks control can affect the use and performance of a NatureWorks product in a particular
application, including the conditions under which the product is used and the time and environmental conditions in which the
product is expected to perform. Since these factors are uniquely within the user’s knowledge or control, it is essential that the
user evaluate the NatureWorks product to determine whether it is fit for a particular purpose and suitable for the user’s method
of application. In addition, because use conditions are outside of NatureWorks control and applicable laws may differ from one
location to another and may change with time, Customer is solely responsible for determining whether products and the
information in this document are appropriate for Customer’s use and for ensuring that Customer’s workplace, use and disposal
practices are in compliance with applicable laws and regulations. NatureWorks LLC assumes no obligation or liability for the
information in this document.

NATUREWORKS MAKES NO WARRANTY, EXPRESS OR IMPLIED, REGARDING THE INFORMATION CONTAINED

HEREIN OR ITS PRODUCTS, INCLUDING BUT NOT LIMITED TO ANY WARRANTY AS TO ACCURACY OR
COMPLETENESS OF INFORMATION, OR ANY IMPLIED WARRANTY OF MERCHANTABILITY OR FITNESS FOR A
PARTICULAR PURPOSE.

NOTICE REGARDING PROHIBITED USE RESTRICTIONS: Unless specifically agreed to in writing by NatureWorks,
NatureWorks LLC will not knowingly sell or sample any product into any of the following commercial or developmental
applications (i) components of or packaging for tobacco products, (ii) components of products intended for human or animal
consumption, (iii) any application that is intended for any internal contact with human body fluids or body tissues, (iv) as a
critical component in any medical device that supports or sustains human life, (v) in any product that is designed specifically
for ingestion or internal use by pregnant women, (vi) in any application designed specifically to promote or interfere with
human reproduction, (vii) in microbeads, including those used in personal care/cosmetic applications, or (vii) to manufacture
bottles or bottle pre-forms in North America.

For additional information please contact NatureWorks via our

website on the tab called FAQ’s or by clicking here.
15305 Minnetonka Blvd., Minnetonka, MN 55345

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