Hytrel Extrusion Manual
Hytrel Extrusion Manual
Hytrel Extrusion Manual
Extrusion Manual
Introduction
The purpose of this manual is to present the latest information on
the extrusion of Hytrel® thermoplastic polyester elastomer resins.
It represents DuPont’s continuing effort to keep users of Hytrel®
up-to-date on extrusion data, processes and techniques.
Page
Melt Properties 1
Extruder Operation 6
General resin handling 6
Safety precautions 6
Moisture pick-up and drying 6
Drying 7
Start-up, shut-down and purging procedures 7
Equipment cleaning 8
Adding concentrates and pigments 9
Recycling of scrap 9
Extrusion Processes 10
General 10
Profile extrusion 11
Monofilaments 12
Rodstock 12
Melt casting 12
Free extrusion of tubing 13
Vacuum calibration (sizing) of tubing 13
Cover extrusion (“cross heading”) 15
Cast film, sheeting and fabric coating 16
Blown film 19
Lay-flat hose liner extrusion 19
Co-extrusion 20
Troubleshooting Guide 22
Many Hytrel® grades are suitable for extrusion processes.
Hytrel® Thermoplastic Polyester Elastomer
Selection of the most appropriate grade for a particular
Hytrel® thermoplastic polyester elastomers are block application, in terms of properties and serviceability, should
copolymers, consisting of a hard (crystalline) segment of be made by referring to the general Hytrel® product literature,
polybutylene terephthalate and a soft (amorphous) segment as well as “Engineering Polymers for Extrusion Applications,”
based on long-chain glycols. Properties are determined by the available from your DuPont Engineering Polymers representative
ratio of hard to soft segments and by the make-up of the or our website, plastics.dupont.com or hytrel.com.
segments. Most grades of Hytrel® do not contain or require
additives to enhance their properties, except for specific Processing considerations, as far as they relate to extrusion,
applications. In such cases, specially compounded grades, should also take into account the following points:
as well as masterbatches (concentrates) are available. • The softer grades are more suitable for free extrusion of
solid profiles. These are the Hytrel® types having Shore D
The grades of Hytrel® are grouped into four categories: hardness up to and including 55D, in particular those with low
1. Standard General Purpose grades, which exhibit versatile melt flow rates (MFR).
processing characteristics, are generally lower in cost, and • Complex profile extrusion using vacuum calibration dies is
are suitable for many extrusion applications; generally not possible with Hytrel®, although it may be pos-
2. High Performance grades, which can provide an extra sible to achieve acceptable results in certain “hollow” profiles
margin of mechanical performance for the more demanding with the harder grades or those with low MFR.
applications; • The hardest grades are best for vacuum calibration of
3. Specialty grades provide special properties or processing tubing. Those grades of shore D hardness 45D and above
characteristics; give excellent results in this process.
4. Masterbatches or concentrates contain relatively high • Intermediate properties may be obtained by mixing Hytrel®
concentrations of specific property-enhancing additives for types (pellet blending) before extrusion, provided that
blending with other grades of Hytrel®. A masterbatch appropriate processing conditions are used. However, it is
cannot be used by itself, it should be used in specified wise to consult your DuPont representative for specific
let down ratios. recommendations.
Hytrel® thermoplastic polyester elastomers are supplied as
cylindrical pellets, having a bulk density of about 700 kg/m3. Melt Properties
They are packaged in 25 kg multiwall paper bags with a
The ability to process Hytrel® by a specific extrusion technique
moisture barrier inner wall. Palletized units contain 40 bags,
depends largely on the characteristics of the melt, which
or 1000 kg net weight, wrapped in film on disposable wooden
are determined by the grade of Hytrel® selected, and by the
pallets. Most grades of Hytrel® are also available in bulk
processing conditions within the extruder.
packages with a moisture resistant liner. For details on bulk
quantities, contact your regional DuPont representative. Some general melt properties should be considered in extrusion
of Hytrel®:
• All grades have a relatively sharp crystalline melting point
Extrusion Applications and Grade Selection
which increases (and becomes sharper) with increasing
The excellent properties and processing characteristics of hardness and crystallinity.
Hytrel® qualify it for many demanding applications. Such • Melt viscosity is strongly dependent upon melt temperature,
properties as mechanical strength, durability, dynamic flex and this dependency increases with increasing hardness.
performance, fluid and chemical resistance, and wide service • Crystallization rate generally increases with increasing
temperature range, have brought benefits in many different hardness; therefore, the ability to supercool the melt without
extruded products, including: onset of crystallization decreases with increasing hardness.
• hose and tubing
Melt viscosity as a function of shear rate and temperature for
• belts
Hytrel® extrusion grades is shown in Figures 1 and 2.
• extruded profiles
• hose mandrels Hytrel® polymers have relatively flat viscosity vs. shear rate
• rope and cable covers curves, especially at the low shear rates which are typical for
• sheeting and films extrusion. This means, for example, that high shear screw and
• wire and cable die designs will not reduce the melt viscosity of Hytrel® as
much as with some other polymers, but may cause undesirable
local temperature increase (see section on “Screw Design” on
page 3).
Figure 1. Melt viscosity at processing temperature
10 4 TYPE TEMPERATURE, °C
HYTREL® 3078 190
HTR5612 BK320 HYTREL® G3548L 190
HYTREL® 4056 190
Apparent viscosity, pascal seconds
Figure 2. Apparent melt viscosity vs. temperature at a shear rate From Figure 2 it can be seen that a significant change in melt
of 100 s–1 viscosity can result from a relatively small change in melt
temperature. The extrusion melt temperature can therefore be
104 decreased (within limits) to provide greater melt strength for
improved stability of the extrudate. It also means that good
control of melt temperature is an important factor in successful
extrusion of Hytrel® resins.
HTR4275 BK320
HTR5612 BK320
4068
5556
General design of extruder
6356, 6358 Experience has shown that the best results with Hytrel® are
4056 6359FG, NC010 obtained with a single screw extruder design. Twin screw
HTR6108 7246, 7248
103 extruders tend to generate excessive shear, and are not recom-
mended. Vented machines are not necessary, since there are no
significant volatiles present in Hytrel®.
Safety devices Length-to-diameter ratios of 24:1 or higher, provide the best
As well as automatic current limitation in the extruder drive, melt quality for good extrusion.
the extruder should be equipped with the following protective Small clearances between the screw flights and the barrel wall
devices in order to prevent personal injury or damage to the are important to prevent backflow of molten resin and possible
extruder: surging in extruder output. It is suggested that clearances of
• A pressure transducer installed in the flow channel imme- 0.08 to 0.10 mm are maintained for extruders up to 50 mm
diately after the screw and before the breaker plate/screen screw diameter, or 0.10 to 0.16 mm for larger extruders. These
pack. The pressure indicator should have an alarm setting for clearances should be checked from time to time, and refurbish-
high pressure and ideally also a cut-out setting designed to ment of the screw or barrel carried out when necessary.
stop the extruder screw before any damage can occur.
Modern extruders are sometimes provided with an intensively
• As a further safety option, a high pressure rupture disc
cooled barrel feed zone containing axial or radial “grooves” to
should be installed in the same area as the pressure trans-
encourage positive feeding of granules. Some of these grooved
ducer, designed to rupture at a pressure above the alarm/
barrel designs have been found to cause excessive shear with
cut-out settings on the pressure indicator.
Hytrel® during the melting/compression stage, with consequent
• An ammeter, installed to show the drive motor current, can
rapid temperature build-up and high motor drive current. Other
be a useful indicator to help monitor start-up and running
problems may occur with the softer Hytrel® grades due to
torque on the screw. Abnormally high motor current normally
premature melting/sticking of the granules in the barrel grooves.
means insufficient temperature in parts of the extruder, and
Such barrels may therefore be unsuitable for processing Hytrel®.
low or fluctuating current may indicate feeding problems or
even wrong screw design for the material. It is recommended that the barrel is equipped with at least
four heat control zones (3 for small extruders) and the tempera-
Materials of construction ture of each zone controlled by a separate thermocouple and
Hytrel® thermoplastic polyester elastomer in the molten state is proportional control instrument. Efficient cooling should also be
non-corrosive to metals. Screws should have hardened (nitrided) provided by air blowers or water, independently controlled for
surfaces but need not be made from corrosion-resistant alloys. each zone.
The screw should have a rounded or conical tip to avoid “dead Screens and breaker plate
spots” in front of the screw where degradation of polymer could
A breaker plate of streamlined design (e.g., counterbored on
occur.
both sides) is usually clamped between the end of the extruder
A typical screw of the 3-zone, gradual transition type suitable for barrel and the head. It acts to convert the material from the
processing Hytrel® is shown in Figure 3. screw to a linear flow, and also develops some back-pressure
on the screw as well as supporting the screen pack made from
The use of complex designs incorporating high shear zones,
several layers of fine wire mesh. A screen pack is used for two
intense mixing devices, decompression zones, etc are not
purposes: to remove any impurities or unmelted material from
recommended for Hytrel®. They can cause excessive local heat
the melt stream; and, to ensure sufficient back-pressure at the
build-up due to intensive shearing action, and usually cause
end of the screw to help create a homogeneous melt and
difficulty in achieving the desired melt temperature, as well as
constant output pressure.
possible high motor drive torque.
The screen pack should consist of two 80 mesh or finer
However, certain designs of “barrier” screw have been found
screens, supported by a 40 mesh screen on the downstream
to be very successful with Hytrel®, particularly in achieving
side, next to the breaker plate. For critical operations, where
constant melt characteristics for critical extrusion operations
ultimate melt cleanliness is required, finer screens (120 or
(such as high speed tubing extrusion). Such screws are
150 mesh) can be used.
designed to separate the solid and molten phases of the
material while providing relatively gentle and controlled shear Regular replacement of screens will be necessary to avoid
over the “compression” section of the screw. excessive pressure drops developing across the screen pack,
and consequent loss of flow. Where fine mesh screens are
Internal screw cooling is not normally desirable for Hytrel®,
used, this replacement may be necessary every 12–24 hours of
although limited cooling of the screw in the feed zone has
running, or whenever an extended shutdown occurs, or when
been found to be successful in eliminating problems of irregular
there is a change of polymer type being extruded.
feeding (fall-off in output) in larger extruders.
W
D h1 PITCH h2
Typical Dimensions*
30 30 5.5 2 3.5
40 40 6 2.2 4
50 50 8 2.5 5
60 60 10 3 6
80 80 11 3.5 8
90 90 11 3.5 9
120 120 13 4 11
150 150 15 4.6 15
*For guidance only
Good external heating is essential in the breaker plate/ clamp Pressure indicators
area of the extruder. Sufficient heating capacity should be Melt pressure should be monitored during extrusion, particularly
provided to rapidly raise the temperature in this region during at start-up. Recording and monitoring of melt pressure during
start-up to the normal processing setting, in order to ensure that start-up will indicate if there is proper flow of the material or if
any residual polymer is thoroughly melted. Because the breaker a feed problem or freeze-off situation exists. During production,
plate (head clamp) area is usually such that a large amount of pressure changes will also indicate output and viscosity changes
heat is lost to the surrounding air, the heater design in this zone of the molten plastic.
is critical.
For accurate measurement and rapid response, a diaphragm-
Adaptor, head and die type transducer with electronic indicator is recommended. The
most common location for the transducer is immediately before
Both the adaptor and the head must be of a streamlined design.
the screen pack, since this is where high pressure is most likely
Flow channels should not contain sudden changes in cross
to be generated. However, it may also be advantageous to install
section, surface interruptions (caused, for example, by mis-
a second transducer in the extruder head area to indicate output
matched assembly joints or damage), or other effects which
pressure closer to the die.
might cause “dead spots.” Such small areas of flow stagnation
can give rise to localized polymer degradation and subsequent Long-term or short-term pressure fluctuations may influence the
release of degraded resin into the melt stream. Similar problems quality and uniformity of the product, and for this reason it may
can occur if flow velocity is reduced due to large cross sections be beneficial to continuously monitor melt pressure by linking
in some flow channels. the transducer output to a data logging device, or chart recorder.
Adequately sized heaters must be provided for the adaptor since Temperature controllers
it is generally a heavy piece of metal. It is especially important Relatively small temperature fluctuations in the extruder,
to control the temperature of the adaptor and head separately, particularly in the front end of the barrel, head, or die, can
since they usually differ greatly in size and energy requirements. greatly influence extrudate quality and output rate because
the melt viscosity of Hytrel® is strongly temperature dependent.
The die, where it extends beyond the extruder head, should also
Therefore, the type of temperature control device used is of
have its own thermocouple and temperature controller.
considerable importance.
For head and die designs for specific extrusion processes, such
To maintain optimum temperature control and a thermally homo-
as tubing extrusion, please refer to the appropriate process in
geneous melt, the controller should be of the proportioning or
the Extrusion Processes section of this manual.
P.I.D. type. An on-off controller is not recommended for use with
Hytrel®. A temperature fluctuation of more than ±2°C should be
Melt pumps
cause for concern; temperature variations of this magnitude can
Where used, melt pumps (gear pumps) can be successful in produce excessive viscosity fluctuations in the melt and unac-
providing a very constant output rate in processes such as high ceptable dimensional variability in critical extrusion processes.
speed tubing extrusion. They are usually installed before the If wide fluctuations in temperature readings are experienced, it
extruder head and fitted with pressure transducers both up- is possible that the heater capacity (wattage) is incorrect for the
stream and downstream, so that this pressure differential can be particular zone to which it is fitted, or that the controller is badly
used to control the extruder screw speed. Care should be taken tuned.
to ensure that the design of the melt pump does not cause ex-
cessive shear heat to be generated (for example, a small pump Temperature feedback to the controllers is provided by suitably
running at too high speed), otherwise the downstream melt positioned thermocouples in each temperature zone of
temperature may become excessive. the barrel, adaptor, head and die. It is important that these
thermocouples are positioned close enough to the melt stream
Instrumentation to accurately register the temperature of the metal immediately
surrounding the melt.
The function of an extruder is to pump molten thermoplastic
at a constant rate and temperature. Sophisticated instrumenta- Melt thermocouples
tion is a prerequisite for quality production. To gauge extruder Thermocouples that indicate the actual melt temperature of
performance it is important to determine the pressure and the extrudate (“mass temperature”) are useful when extruding
temperature of the melt, as well as to provide adequate Hytrel®. For rapid response they should be located either in the
methods of control. adaptor or, preferably in the die, as close to the melt stream as
possible.
The use of a hand-held needle pyrometer to check the actual Moisture pick-up and drying
melt temperature before start-up should be encouraged.
Hytrel® granules are supplied in moisture resistant packaging
Measurements should be made at normal running screw
with a moisture level of less than 0.1%. However, when
speed, after purging for sufficient time to allow temperatures
exposed to air, the granules pick up moisture, which may result
to stabilize.
in bubbles or streaks appearing in the extrudate.
Infra-red (non-contact) thermometers may also be used to
Even when only a relatively low level of moisture is present
check melt temperature when running, but should not be
(not enough to be visible in the melt), there is likely to be a
relied upon unless they have been previously checked against
loss of viscosity and possible loss of properties in the finished
a thermocouple (needle pyrometer) in the melt stream, since
product. This is because at temperatures above the melting
their effectiveness can be influenced by factors such as color
point, excessive moisture causes a degree of hydrolytic
and reflectiveness of the extrudate.
degradation of the polymer.
As with all thermoplastics, thermal burns from contact with It follows from the above that Hytrel® granules which have been
molten polymer are a potential hazard. exposed to atmospheric humidity for any significant time must
Compounding ingredients or additives may present hazards in be re-dried before use.
handling and use. Before proceeding with any compounding
or processing work, consult and follow label directions and
handling precautions from suppliers of all ingredients.
Figure 4. Moisture absorption at ambient temperature Figure 5. Recommended guidelines for drying Hytrel®:
drying time vs. temperature
1.0
0.8 HYTREL® 5556
0.6
150
0.4 .
R.H
0 %
Moisture gain, weight (%)
10
140
0.2
Temperature, °C
R.H. 130
0.1 50%
0.08
Max. (most grades)
0.06 120
0.04
110
Max. (low melting
0.02 point grades)
100
0.01
0.1 0.2 0.4 0.6 1 2 4 6 10
90
Time, hr 0 1 2 3 4 5 6 7 8
Time (hr)
= drying of G-type (e.g.: G5544).
= drying of all other types.
Drying
As explained above, Hytrel® thermoplastic polyester elastomer
must be dry before processing. When used immediately from Start-up, shut-down and purging procedures
sealed undamaged bags, it may be possible that the moisture Start-up
level is below the recommended limit of 0.08%, however in Start-up technique is important, as it involves the safety of both
order to guarantee the elimination of potential problems due to operating personnel and the equipment.
moisture, it is strongly recommended that all resin is routinely
dried. In circumstances where bags are damaged or material Start-up techniques vary depending on whether or not the
from opened bags or regrind is used, the resin must be dried. machine is clean.
A. Clean machine
In many cases, hot air ovens may not be adequate. It is strongly
recommended that dehumidifying (desiccant) dryers are To start up a clean, empty extruder, set the temperature control-
employed, in order to ensure effective drying under all ambient lers for the die, head, adaptor and barrel zones at the recom-
humidity conditions. mended operating temperatures for the particular resin grade
being used (refer to processing data in Table 2).
Particularly in the case of critical extrusion operations, such as
vacuum calibration of tubes to small tolerances, it has been At this time the operation of the heaters and controllers should
found that extruder output may fluctuate slightly with changing also be checked. When all zones reach their operating tem-
moisture levels and temperature of the granules in the hopper. peratures, they should be allowed to “soak” for 30–60 minutes
For this reason, again, the use of a dehumidifying drier under (depending on the size of the extruder) before feeding resin to
conditions of fixed temperature and granule residence time is the screw. Turn on the feed throat cooling water.
always recommended. When all heating zones have been at their set temperatures
The dryer should either be directly mounted on the machine for 30–60 minutes, turn on the screw at slow speed
hopper (hopper dryer) or, if it is a separate unit, should incorpo- (5 to 10 rev/min) and start feeding resin through the hopper.
rate automatic material transfer to a sealed feed hopper. When the melt appears at the die it should become smooth
and glossy after a few minutes, and both the melt temperature
Drying time and temperature will depend on the initial moisture and head pressure should level out.
level in the material, as well as the type of dryer or oven used.
However, general guidelines for drying Hytrel®, which are based It is desirable to use a hand-held needle pyrometer to monitor
on laboratory and industrial experience, are shown in Figure 5. melt temperature at start-up. The extruder pressure and motor
amperage should be checked and monitored.
When the melt quality appears to be uniform and there is no Shut-down and purging procedures
sign of any lumps or bubbles, increase screw speed to normal For brief stoppages of 30 minutes or less, no action is required,
running speed to check final melt quality and temperature other than a short purge with new resin after start-up.
before starting production.
If the extruder is to be shut down for longer periods, empty the
If a melt pump is being used, then the start-up procedure barrel and turn off the heaters. It can be advantageous to purge
may be slightly different to the above — please refer to the a small quantity of a low melting point Hytrel® grade (such as
equipment supplier’s guidelines. 4056) through the extruder immediately before shutting down.
This will help minimise purging time on start-up. If the extruder
B. Full/partly full machine
is so equipped, barrel cooling may be used to cool the residual
Sometimes the extruder has been shut-down after extruding
melt rapidly and prevent any polymer degradation. During the
another polymer, and may be partly filled with that material. In
next start-up, any material contained in the machine should be
this case, the melting point of the residual polymer should be
expelled and not used. Venting of gases which may be gener-
considered during start-up.
ated should be considered (see Safety Precautions).
Be careful when starting a full machine to prevent bridging in the
Purging with polyethylene or other polymers is not normally
feed section, localized overheating (which may result in polymer
advised, except just prior to strip-down of the equipment for
degradation), and cold spots (plugs of unmelted resin occurring
cleaning (see Cleaning). This is because it can take a long period
primarily in the adaptor or head zones).
after start-up to completely eliminate traces of polyethylene
Set all controllers (with the exception of the first barrel zone, from the Hytrel®.
which can be set to its normal running temperature) to a value
Any purging should be done with temperatures set to a value
which is 10–20°C above the nominal melting point of the grade
which is above the melting point of the resin being purged.
to be processed (refer to Table 2). If the residual material in the
machine has a melting point which is above that of the new Special purging compounds (e.g., cast acrylic resins) may be
resin, then the controllers should be set higher than the melting used to purge the extruder. Since these resins are often cross-
point of the old material. linked, or behave in such a way that they do not melt, but only
soften, it is normally necessary to remove the head by separat-
When the controllers have reached these temperatures and
ing at the breaker plate before purging. If this is not done, un-
have been held for 30–60 minutes, slowly increase the screw
safe drive torque and pressures may result which may damage
speed to about 10 rev/min until molten polymer flows from the
the machine or injure the operators.
die. It is important at this time to check for any excessive die
pressure or drive motor current which may indicate a plug of
unmelted resin. Start feeding fresh resin through the hopper, Equipment cleaning
again checking for excessive pressures or motor current. Run Occasional dismantling and cleaning of the extruder screw,
the extruder slowly while purging with fresh resin for up to adaptor, head and die components is recommended. The
30 minutes, or until a flow of clean and homogeneous molten optimum frequency for these strip-downs will depend on the
polymer is obtained. number of start-up/shut-down operations and the number of
different resins which have been used in the extruder.
During the purging process, the screw speed should occasion-
ally be increased to normal operating speeds, or above, for short Cleanout procedure consists of purging the extruder with high/
periods. This will help to release any old degraded or unmelted medium density polyethylene or polypropylene and then remov-
resin from the internal surfaces of the extruder. ing the die, adaptor, and head from the extruder. With the head
removed, the screw and barrel may then be cleaned by running
When a smooth flow of clean molten polymer with no lumps
the machine while feeding a suitable cleaning compound (e.g.,
of old or degraded material has been obtained, all temperatures
cast acrylic type) through the machine. The adaptor, head and
should be re-set to normal running settings, and slow purging
die should be completely dismantled for cleaning.
continued until the temperatures have re-stabilized.
Complete removal of the screw for thorough cleaning is
At this point, melt temperature should be checked using a
essential from time-to-time, since it is the only way to ensure
needle pyrometer, with the screw speed at the desired
that hard particles of degraded polymer and other residues are
running speed.
properly removed from the screw and barrel surfaces.
The larger quantities of resin can then be removed from the sion of Hytrel®, but performance of individual products need
screw and other components by scraping while still hot. to be tested by the user. Let-down ratios of 1–3% are typically
This may be followed by wire brushing or the use of special used for most color masterbatches.
scouring pads. If need be, the screw should be polished to
Masterbatches based on PE, Nylon, PVC or other resins are
remove carbonized residue from the root of the screw. A
generally not recommended, although acceptable results
rotating wire brush attached to an extension rod on a suitable
may be found with LDPE based masterbatches in non-critical
power tool should be used to clean along the full length of the
applications. Some powder and liquid pigments have been
extruder barrel.
evaluated with Hytrel® and may give acceptable results,
Stubborn residue may be removed from the head and die parts however they are not as convenient to use as masterbatches.
by burning with a propane torch; this method, however is not
For black pigmentation, especially where good outdoor aging is
generally encouraged, since flammable and toxic gases may
required, the use of Hytrel® 40CB or 41CB is always preferred.
be formed. A much superior method is to immerse the parts
in a hot fluidized sand bath, or by using cleaning ovens which
are specially designed for the purpose. With suitable fume Recycling of scrap
extraction, these methods are fast and thorough, and parts are The good thermal stability and completely thermoplastic nature
left ready for re-installation. of Hytrel® allows use of scrap (regrind) from the extrusion pro-
cess. Hytrel® can be reground and blended with virgin polymer
Adding concentrates and pigments at a level up to approximately 50%, assuming the polymer has
Concentrates been correctly processed. At all times, care should be exer-
DuPont offers several concentrates for use with Hytrel®; cised to ensure that it has not been degraded and is free from
these are: contamination.
Hytrel® 40CB, 41CB — Carbon black concentrates Chop scrap into chips approximately the same size as the origi-
Hytrel® 20UV — Ultraviolet light stabilizer nal pellets. Use a scrap grinder with well adjusted sharp knives,
Hytrel® 30HS — Heat stabilizer as Hytrel® is slightly rubbery by nature.
Hytrel® 51FR, 52FR — Flame retardant concentrates
Dry all regrind material and blend well with virgin polymer to
In all cases the concentrates are designed to be tumble blended ensure uniform quality.
with any grade of Hytrel® before extrusion, to enhance specific
properties. Further information and recommended let-down Melt Flow Rate (MFR or MFI) checks are a practical way to
ratios for blending of the concentrates is given in the relevant monitor quality of regrind on representative samples, and is a
individual product data sheets. useful quality control tool for both finished products and regrind
material.
With the exception of Hytrel® 52FR which has a melting point
of 205°C, all of the concentrates are dispersions based on a Melt Flow Rate, in effect, measures flow of molten polymer
low melting point Hytrel®. Even though they are normally used through a restricted orifice under standard conditions of material
in low concentrations as indicated above, three of the concen- pressure and temperature, and thus has an inverse relationship
trates — Hytrel® 30HS, 51FR and 52FR — have some hazards to viscosity: the higher the MFR, the lower the viscosity. Typical
or off-gasses associated with their active ingredients. Therefore values for various Hytrel® grades are given in Table 2. However,
these products require some special precautions when handling moisture content may significantly affect the result so it is
and processing, and the specific material literature should be essential that the regrind is dry before testing.
carefully studied. The difference in MFR between granules and finished product
Pigments or regrind is an indication of polymer degradation. As a general
Most Hytrel® grades are available in custom colors, based on a rule, scrap material should not be re-used if the melt index check
minimum order quantity. However, for many extrusion applica- shows a value which is more than about 30% above that for the
tions, it may be desirable to add pigments or color concentrates virgin material. In the case of properly processed Hytrel®, the
directly at the extruder. The most convenient way to do this is increase in melt flow rate obtained from regrind should be well
by means of a color masterbatch, in granule form. Ideally, these below this value.
masterbatches should be based on a low melting point grade of Further information on melt flow rate measurements can be
Hytrel®, and such masterbatches are available (for example, from obtained from your DuPont representative.
Wilson/Poly-One company). Some “universal” masterbatches on
the market have been found to give satisfactory results in extru-
Extrusion Processes However, it is important that temperatures in the clamp, adaptor,
head and die zones, as well as the melt pump (if used) should at
General all times be set to a value which is at least equal to the nominal
Many different extrusion processes have been successfully melting point of the grade of Hytrel® being processed, other-
used with Hytrel®, and most of these are covered in the wise cold slugs and skins of unmelted material may accumulate
following section. on the internal metal surfaces, and result in the release of lumps
The melting characteristics and temperature guidelines for of cold or degraded Hytrel® into the melt flow.
extrusion of various Hytrel® grades is given in Table 2 below, In fact, when starting up a machine which was previously shut
however there are also some more general points which apply down with residual Hytrel® in the head, these temperatures (and
to all Hytrel® extrusion processes. also the barrel zones) should be set at least 10°C higher than
As discussed under “Melt properties,” the viscosity the melting point (see section 5 “Start-up Procedures”) and only
of dry Hytrel® extrudate depends very much on the melt changed to normal running temperatures after purging out all old
temperature. It follows that melt temperatures (that is, actual material from the machine.
temperature of the molten polymer) should be just above Further adjustments of the melt temperature should normally
the nominal melting point to give the highest viscosity in then be made by alterations to the barrel temperatures only. In
processing. This is normally desirable in most (though not all) other words, the desired melt temperature should be achieved
extrusion processes. Typically, the actual melt temperature at the end of the screw, and the head and die zone settings
should be 10–15°C above the nominal melting point when should not be used to adjust melt temperature!
measured with a needle pyrometer held in the melt flow, and
Because of the viscosity/temperature relationship, it is important
the extruder running at normal operating speed.
that good control of temperature in each zone is maintained. This
The temperature profile used to achieve this will depend on the depends not only on having properly maintained and calibrated
individual extruder, and to a large extent on its screw design. instruments, but also on having correctly positioned and working
thermocouples and on other good operating practices.
Table 2
Hytrel® Extrusion Grades — Processing Conditions
Melt Typical temperature settings, °C Typical
Nominal flow, Center Center Adaptor, melt
Hytrel® melting index2, Rear rear front Front head and temperature,
grade point1, °C g/10 min barrel barrel barrel barrel die °C
4056 150 6 (190°C) 150–160 160–170 160–175 160–175 160–180 165–185
G3548L 155 10 (190°C) 150–160 160–170 160–175 160–175 165–180 170–190
G4078W 170 5 (190°C) 160–170 170–180 170–190 170–190 175–195 185–200
G4074 170 5 (190°C) 160–170 170–180 170–190 170–190 175–195 185–200
4068, 4069 193 9 (220°C) 190–200 200–210 200–215 200–215 205–220 205–230
4556 193 9 (220°C) 190–205 200–210 200–215 200–215 205–220 210–230
G4774 208 11 (230°C) 195–210 205–215 205–225 205–225 210–230 220–240
5556, 5586 203 8 (220°C) 195–210 205–215 205–220 205–220 210–225 215–235
5555HS 203 8 (220°C) 195–210 205–215 205–220 205–220 210–225 215–235
G5544 215 10 (230°C) 200–215 210–220 210–225 210–225 215–230 230–245
6356, 6358, 211 9 (230°C) 200–215 210–220 210–225 210–225 215–230 225–240
HTR8241, 211 4 (230°C)
HTR8163 210 5 (230°C)
7246, 7248, 218 13 (240°C) 205–220 215–225 215–225 220–235 220–235 230–245
8238 221 12 (240°C) 210–225 220–230 220–230 220–230 225–240 235–250
HTR8303 221 6 (250°C) 3
215–230 220–230 230–240 240–255 245–250 230–270
1
Differential Scanning Calorimeter (DSC), peak of endotherm
2
Nominal value — Test conditions: 2.16 kg load, temperature shown in parenthesis ( )
3
Nominal value — Test conditions: 10.0 kg load, temperature shown in parenthesis ( )
10
Attention to detail in other parts of the extrusion process While free extrusion is acceptable for simple “solid” shapes,
can also help prevent potential problems. Such factors as it may not be possible to achieve the desired profiles with this
fluctuating quenching water temperatures and water turbulence, technique where complex shapes or large changes in section
variations in haul-off speed, vibrations in mechanical equipment, are involved (for example, “U” channels or ribbed profiles).
and fluctuations in resin temperature in the hopper have all been In such cases, it may be desirable to arrange suitable guides
known to cause problems which may be wrongly attributed to or supports within the water bath which “hold” the shape of
the material or the extruder. the extruded profile until sufficiently solidified. However, this
technique may still not be adequate, particularly with the harder
Hytrel® grades where differential shrinkage can cause warp-
Profile extrusion
ing and distortion of certain profile shapes. Vacuum calibration
Solid and hollow profiles may be extruded successfully from may therefore be required, but — as discussed below — there
many Hytrel® grades, depending on the complexity and shape are limitations with vacuum calibration of profiles, particularly
required. regarding the grades of Hytrel® which are suitable, and the
By free extrusion complexity of the shape to be extruded.
Simple shapes, such as solid round or flat strip profiles, are best Hose mandrels
produced by horizontal free extrusion into a water bath, over a Hose mandrels are a specific case of a simple, solid round
suitable weir. This technique is relatively inexpensive in tooling, profile. Such mandrels in Hytrel® are widely used in the
and in many cases a simple flat plate die (in aluminium, for manufacturing process for rubber hoses.
example) can be simply fixed to the front of the extruder head,
by means of a suitable adaptor if necessary. Although these The control of diameter and ovality, is particularly important
plate dies can have the disadvantage of encouraging a and for this reason the following points have been found to be
build-up of stagnant polymer at the rear of the plate, which will helpful:
eventually degrade and cause problems during long extrusion • Melt temperature should be as close as possible to the
runs, they are nevertheless useful for prototyping and for shorter nominal melting point of the Hytrel® grade in use.
production runs (provided they are dismantled and cleaned • Use of a melt pump will help ensure constant extruder
after each run). Plate dies should have a thickness of 6–12 mm, output, which is important in maintaining dimensions to
depending on the profile size, and should be reduced locally to tight tolerances.
3–5 mm where the profile may have a section which is relatively • The profile should enter the water bath smoothly, with no
thin. The actual dimensions if the die orifice should be roughly turbulence in the water flow at the point of entry.
2–3 times the dimensions of the finished profile, in order to • The profile should be supported underwater within the
provide enough draw-down of the melt during extrusion. This cooling bath by means of a “V” or “U” guide channel.
draw-down is necessary to give sufficient tension in the extru- • The use of a short initial cooling bath will ensure minimum
date to prevent sagging and fluctuations in dimensions. stretching of the profile between extruder die and haul-off
(“elastic band” effect). Additional cooling is provided after the
Normally, some modifications to the die orifice are necessary
first haul-off, before reaching a second haul-off or
after initial trials, in order to achieve the required distribution
capstan unit.
of material. With a simple plate die in aluminium, it is relatively
• The first haul-off should only apply light pressure in order to
easy to hand file or grind the die, for example to encourage ma-
avoid deformation of the shape while still warm.
terial flow to selected parts of the profile cross section.
• Harder Hytrel® grades (55D and above) tend to form
These techniques are particularly successful with the softer internal shrinkage voids in larger mandrel diameters (typically
Hytrel® grades, up to, say, 55D in hardness, and with the higher >12 mm), but this may be improved or eliminated by using
viscosity grades, extruded at lowest possible melt temperature hot water quenching in the first cooling bath (e.g., water
(within the limitations mentioned under “General” on page 10). at 70°C), or by alternating short sections of water and air
However, it should be noted that the final profile shape achieved cooling.
may be affected by changing grades, or by altering extrusion
speeds or temperature settings. Profiles by vacuum calibration (sizing)
This technique, which is well established for profiles in more
Of course more streamlined dies, made from hardened steel,
rigid polymers such as rigid PVC, polycarbonate, etc. has been
are preferable for longer runs, but the simple plate die can
found to be moderately successful with the harder Hytrel®
often be used as a basis for the design of the final die, or for
grades. Unfortunately, the softer types exhibit too much friction
prototype parts where the cost of a full production die may not
against the calibration die surfaces and tend to stick.
be justified.
11
Normally, this process can only be used for relatively simple continuously compensated by an additional flow of material
“hollow” profiles, where there is an internal hole or cavity which under pressure from the extruder. Furthermore, the slow
can be held at ambient pressure during the extrusion process movement of the Hytrel® shape through the cooling sections
via an airway in the extrusion mandrel (die core). of the die must be smoothly controlled, and a constant back
pressure on the melt must also be maintained by control of the
In this process, a “wet” calibration die system should be used,
take-off unit.
where the extrudate is lubricated by a film of water supplied
through a series of small (0.5–1.0 mm) holes drilled close Since the equipment for stock shape production tends to be
together around the entrance to the calibration die. Alternatively, rather specialized, it will not be described further in this manual.
a small slot can be used to provide the required film of water
at this point. The die entrance should be radiused (3–4 mm) Melt casting
and the whole internal surface finished by sand blasting, in The melt casting process may be used with Hytrel® to produce
order to give a “matte” surface which helps retain the water solid molded shapes using a simple low-pressure mold which is
lubrication film. filled from a suitable nozzle fitted to the extruder head.
Extruder die design should follow the principles above for free Although not many resins may be processed by this technique,
extrusion, although less draw-down can be used (depending it has been found that the combination of good thermal stability,
on the profile size and shape). The die land length should be relatively low shrinkage, and suitable viscosity characteristics
relatively short (typically 5–10 mm, depending on the profile make Hytrel® ideally suited to this process.
thickness) in order to prevent the extrudate being drawn away
The melt casting technique may be used (a) where large, thick
from the die wall at the die exit point.
parts would not be economically viable by injection molding
Monofilaments due to the excessive cycle times, or (b) where injection mold
tooling cost would be too high because of small numbers of
Monofilament extrusion is straightforward with the medium
parts required — melt cast tooling is relatively inexpensive, or
viscosity Hytrel® extrusion grades.
(c) for prototyping parts which might subsequently be made by
Equipment normally used with Nylon, PBT, and similar resins injection molding.
may also be used for Hytrel®, and for this reason it is not
A typical equipment set-up is shown in Figure 6. Note that
considered necessary to describe such equipment in detail here.
the mold may be one of several which are filled in turn on a
Processing temperatures may be somewhat higher for monofila-
carousel system, while others are undergoing the cooling or
ment extrusion than for most other extrusion processes, with
demolding stages. Although shown with a vertical feed from
typical melt temperatures being 20–30°C above the nominal
the extruder, it is also possible to utilise a horizontal feed
melting point of the particular Hytrel® grade in use.
channel from the extruder to the mold cavity.
For maximum process stability, the draw-down ratio, as
measured by the die diameter relative to the monofilament
Figure 6. Use of extruder for melt casting of Hytrel®
diameter, should be between 4:1 and 10:1 as the filament leaves
the first water quench bath.
EXTRUDER
The amount of filament orientation, and the temperatures for
further drawing and annealing should be determined by trials
which involve measurements of the required end-use properties
for the monofilament. TURN
DOWN DIE
Note: In both profile and monofilament extrusion, the use of a
melt pump can greatly assist dimensional control of the finished NOZZLE
profile. VENT VENT
Rodstock MOLD
The production of rodstock and other stock shapes in Hytrel®
is achieved by a special extrusion process, which is also used
SUPPORT TABLE OR CAROUSEL
for other polymers. Since the cross-sectional areas of these
products are relatively large, this limits the rate of cooling of the
section, and extrusion speeds are consequently very slow in
this process. It is essential to ensure that the shrinkage during
solidification of the material in the center of the shape is being
12
Figure 7. Free extrusion of tubing
CONTROLLED
EXTRUDER AIR SUPPLY SIZING RINGS
(optional)
air water
pump
TO DRAIN
13
The fine adjustment to tube dimension is achieved, however, by In general, 35D and 40D Hytrel® grades cannot be run success-
adjustment to the vacuum applied to the vacuum bath. fully by the differential pressure sizing method using either
plate die or the tubular die. Their very rubbery nature and slower
Suitable lubrication must be provided between the extruded
crystallization rate causes the polymer to bind or “grab” in the
polymer and the metal surface of the calibrator. Usually, this can
sizing die. In certain cases, however, it has been possible to
be accomplished by a fine water flow through small holes or
extrude large diameter, thin-walled tubes in these grades, using
slits at the front of the tubular die, or through an annular water
a calibration die under very low vacuum. Such tubes are used as
ring device at the entrance to the die.
liners for fire hoses and other lay-flat hoses.
The correct design of vacuum sizing die is very important, and
The correct extruder die and pin for tube extrusion should be
designs used for other polymers (nylon, polyethylene, etc) may
selected as follows:
not necessarily be suitable for Hytrel®.
1. The extruder die should be between 2 and 3 times the
A sizing die which has been found to work well with all
required tube outside diameter, for tubes up to about
Hytrel® grades over 40D hardness is shown in Figure 10.
20 mm diameter. Where larger diameters are to be made,
Please contact your DuPont representative for more detailed
the extruder die should be between 1.5 and 2 times the
design information.
tube outside diameter.
In all vacuum sizing operations there should be provision for fine 2. The extruder pin should then be selected so that the pin
adjustment of the vacuum, in order to accurately control and should be larger than the required inside diameter by a
maintain the external diameter of the extruded tube. Vacuum of factor which is slightly less than that which was used to
0.10 to 0.30 bar has been used successfully to maintain determine die diameter in (1) above.
accurate dimensional control of small diameter Hytrel® tubes.
1.15 VACUUM
TANK
1.14 60 m/min
INTERNAL SURFACE
1.12
Ratio sizing die I.D. to tube O.D.
1.08 40 m/min
TUBE
EXIT ANNULAR
A 30 m/min
1.06 WATER
20 m/min OUTLET
10 m/min SLIT
1.04
0 m/min
FRONT
1.02 PLATE
5 10 15 20 25 30 35 40 45 50 60 70+
Tube O.D (mm)
FLANGE FOR
FIXING TO
VACUUM TANK
14
For example, to extrude a tube having 8 mm outside diameter • Constant water temperature (max. 5°C variation) in the
and 6 mm inside diameter, at a line speed of 30 m/minute: vacuum bath.
Extruder die diameter = 8 x 2.5 = 20 mm • Uniform temperature and moisture content of granules in
Therefore extruder pin = 6 x 2.3 = 13.8 mm the feed hopper. This is best achieved by the use of a hopper
drier system or a drier with automatic transfer of granules at
Selection of pin and die according to these guidelines will result constant temperature/moisture level to a sealed hopper.
in a Draw-Down Ratio in the range of 4 to 9, which has been
found to be optimum for Hytrel® tubing extrusion using the
vacuum sizing technique. Draw-down ratio (D.D.R., see formula Cover extrusion “cross-heading”
below) is defined here as the ratio of the cross-sectional area Most Hytrel® grades have been used to cover various types of
of the extrudate at the extrusion die-face, to the cross sectional product, including hoses, ropes, cables and wires. The basic
area of the finished tube. equipment required includes an extruder fitted with a suitably
Dd2 – Dm2 designed cross-head, a pay-off (or unwinding) system, incorpo-
D.D.R. =
Dt2 – Db2 rating a brake or tension control device, a water cooling bath,
Another important factor when choosing dies and mandrels and a variable speed haul-off or capstan, followed by an auto-
for making tubes from Hytrel® is the Draw-Ratio Balance (D.R.B., matic wind-up or coiling system.
see formula below). The ideal D.R.B. for Hytrel® is 1, meaning
The cross-head and die arrangement can be one of two types:
that the inside surface of the molten tube is drawn
the same amount as the outside surface. The range 0.9 to 1.1 • Cross-head with pressure (packing) die, or
is acceptable. • Cross-head with tubing (sleeving) die.
The draw-down ratio and the draw-ratio balance can be Pressure Die extrusion involves the extruded material coming in
calculated as follows: contact with the core (e.g.: hose, wire etc) within the die itself,
Dd ÷ Dt which results in some pressure being applied to the melt so that
D.R.B. =
Dm ÷ Db it tends to penetrate any interstices in the core material. This
technique is preferred where:
Where Dd = Diameter of die
Dm = Diameter of mandrel or torpedo • Good adhesion is required, or
Dt = Diameter of tube
• A smooth, regular, outer cover diameter is required over an
Db = Internal tube or bore diameter
irregular or rough inner core material.
Other factors which are worth special attention in vacuum
Figure 11 shows a typical pressure die arrangement.
calibration of tubes in Hytrel® include:
The diameter of the die should be approximately equal to the
• Optimum screw design to give constant output rate and
required cover diameter. The land length (E) should be between
minimum variation in melt temperature. Please refer to
1 and 3 times the final cover diameter, but considerably less for
section on Screw Design on page 4. This is particularly
very thin covers (where thickness is <0.5 mm).
important for high speed tubing extrusion, and where
accurate dimensions must be maintained over long lengths.
A special barrier screw design has been developed which
has been found to give excellent results with Hytrel® in Figure 11. Extruder head for pressure die covering
tubing extrusion and other critical processes. Details can be
provided through your DuPont representative.
• Use of a melt pump can also help to ensure constant output C
A
and hence accurate dimensional control.
B
• Lubricating water supply at uniform pressure to the sizing D
die. Ideally this should be from a header tank situated at
B
least one meter above the die, with flow being controlled and F E
A
monitored through a suitable flow meter. C
15
The clearance between the core to be covered and the bore of contact with the metal core, which may result in insufficient
the “torpedo” or mandrel should be between 1% and 5% of the penetration of the core material. Similarly, fibrous cores (e.g.,
core diameter (depending on the material and regularity of the textile rope or braiding) may need to be dried by passing
core surface). through a hot-air tunnel, or by storing the core material in a
warm, dry area prior to covering, in order to prevent moisture
The distance “F” between mandrel tip and die entrance should
blisters appearing through the Hytrel® cover.
be adjustable, but is normally set to be equal or greater than the
cover thickness being applied. • For high speed extrusion, particularly with thin wall covering,
it may be necessary to raise the head and die temperatures,
Tubing Die (sleeving) extrusion is illustrated in Figure 12. and possibly also the barrel temperatures, to achieve
In this technique, Hytrel® is extruded in the form of a tube, sufficient flow rate at acceptable melt pressure. Melt tem-
and is “drawn down” to meet the surface of the core material. peratures up to 40°C above the nominal melting point of
This is often achieved with the assistance of a vacuum which is most Hytrel® grades can be safely used to reduce melt
applied to the inside of the torpedo and acts through the bore viscosity, providing the design of adaptor, head, and associ-
of the mandrel (pin). The optimum draw-down ratio (D.D.R.) ated parts does not give rise to any hold-up spots where
is in the range of 5–20:1 and the die diameter and mandrel thermal degradation might take place.
diameter can be calculated from the selected draw-down ratio
• Although water temperature in the cooling bath is generally
as follows:
not critical (10–20°C is typically used), there may be cases
D.D.R.= Dd2 ÷ Dm2 where a more gradual cooling of the Hytrel® cover by using
Dc2 ÷ Dw2 hot water (e.g., 60°C) may be beneficial. This is sometimes
Where Dd = Die diameter the case with optical fibre sheathing, or small diameter
Dm = Mandrel diameter electrical conductors, where too fast crystallization caused
Dc = Diameter of covered core (rope, cable, etc.) by cold water may result in undesirable stresses in Hytrel®
Dw = Diameter of uncovered core when it cools.
The advantages of tubing die extrusion are: Cast film, sheeting and fabric coating
• Better control of cover wall thickness Cast film
• Easier to “strip” cover from core (eg: wire coating In the cast film process, molten Hytrel® is extruded through
applications). a slit die onto a polished metal roll — usually known as the
“quench roll” or “chill roll” — which serves to quench the
Some other points which may be important in cross head
hot melt. From the quench roll, the film passes around a series
extrusion with Hytrel®:
of other rolls designed to guide it and keep it wrinkle-free
• If a thermally conductive core material is being covered at wind-up. Figure 13 illustrates a typical cast film line.
(e.g., electrical conductor, steel braid hose, etc), it may be
necessary to pre-heat the core by passing through a flame or Films of Hytrel® thermoplastic polyester elastomer as thin as
hot-air tunnel before entering the cross-head. This will help 0.013 mm have been made by this method.
to prevent too rapid freeze-off of the melt when it comes in
Film thickness is controlled by the relationship between the
extruder output and surface speed of the quench roll.
Figure 12. Extruder head for tubing die covering
The quench roll is normally cooled internally by water. With
Hytrel®, hot water or hot oil may be used to control quench
temperature for some applications (see discussion on effect of
quench temperature on film properties, below). Tension control
C
A must be precise, and should be very light with the more flexible
B grades of Hytrel® in order to produce wrinkle-free film with good
D roll conformation (flatness across the roll). Air jets can be used
to pin the edges of the melt web to the chill roll, in order to mi-
nimise edge weaving and reduce neck-in. Take care that none of
E
the air flow reaches the die lips, since this could result in uneven
cooling of the die and poor dimensional uniformity in the film.
A = Die D = Core material (hose, wire, etc.)
B = Mandrel E = Land length
C = Melt
16
Figure 13. Typical cast film unit setup
RUBBER PULL
STRIP ROLL ROLLS TRIM REMOVAL
IDLER
SLITTER
DANCER-
LAY-ON
CHILL ROLL
TANGENT
IDLERS
WATER COOLING
CHILL ROLL (INDIVIDUAL)
TURRET WIND
Increasing quench temperature: Both mechanical and air pressure systems for applying roll
• Increases modulus and tensile strength force have been used. The sheeting thickness is controlled
• Increases haze by adjusting the “nip” between first and second rolls, while
• Decreases gloss controlling extruder output in order to maintain a small “rolling
• Decreases transparency bank” of molten melt in the nip.
Increasing air gap: The die lip opening should be 20 to 50% greater than the sheet
• Increases haze to be produced; a thinner sheet (within limits) can be made with
• Decreases gloss and transparency the same die opening by increasing roll speed. Melt tempera-
• Increases modulus and tensile strength ture should be kept as low as possible consistent with uniform
Increasing extrusion rate: extruder output, melt quality, and head pressures. The air gap
• Decreases haze should be the minimum permitted by equipment geometry. The
• Increases transparency and gloss melt “puddle” or bank of surplus resin between the roll “nips”
should also be kept small to minimise oxidative degradation, but
To avoid sticking, quench temperature should not exceed 50°C
if the bank is too small, it may result in “starving” of the rolls
for soft Hytrel® types (35D and 40D hardness). 80°C for 47D to
which will cause erratic dimensional variations in the sheet.
63D hardness grades, or 100°C for 72D and harder grades.
17
Figure 14. Extrusion of sheeting
PULL ROLLS
WIND-UP
EXTRUDER
INDIVIDUALLY HEATED TRIM ROLL TENSION ROLLS
OR COOLED
Roll temperatures should be individually controlled. Typical roll The melt contacts the substrate just prior to meeting the
temperatures for Hytrel® sheeting extrusion are as follows: chill roll which solidifies or quenches the melt. The melt web
usually extends beyond the edges of the substrate slightly,
Type of Hytrel® (Shore D hardness) Roll temperature, °C and therefore contacts both the chill roll and pressure roll at
this point. To avoid any tendency to stick on the pressure roll, it
35D and 40D 15 to 30 has proved effective to cover rolls with a coating of Teflon® FEP
47D to 82D 40 to 70 fluorocarbon resin.
The temperature of the first roll will be limited to the tempera- A chill roll of 300–600 mm in diameter is usually used in
ture at which the sheet sticks to the roll, and is normally kept as extrusion coating. The temperature of the chill roll is normally
low as possible. maintained between 20 and 40°C.
Fabric coating
The stability of the melt web before it contacts the chill roll
Fabric coating with Hytrel® can be achieved on a 3 or 4 roll
depends greatly on having the correct die gap set on the
coating line which is similar in principle to the sheeting extru-
extruder, as well as on the melt temperature, the air gap
sion line shown in Figure 14. The fabric is introduced above the
between die and roll nip, and on the line speed.
extruded Hytrel®, between the first and second rolls. A more
common set-up is the standard extrusion coating line shown in As for cast film extrusion, careful control of tension in the
Figure 15. In this process the melt is extruded through a slit die windup is very important to minimise wrinkling and ensure good
onto the fabric or other substrate in the nip between a chill roll roll conformation.
and pressure roll.
Figure 15. Typical extrusion coating line. Substrate is fed from the turret unwind at left. After preheating,
it is coated by extruder at laminator station (center). After cooling, stock is wound at right.
Tension nip
18
Blown film particularly the softer 35D and 40D hardness types, can also
Suitable Hytrel® grades may be processed with standard film be blown into films up to about 150 microns thick, at blow up
blowing equipment such as that shown in Figure 16. The higher ratios up to approximately 2.8:1, but anti-blocking agents such
melt strength of Hytrel® blow molding grades make them as Kemamide B* or Crodamide SR** (or similar products) may be
easier to handle, and allow films up to 250 microns to be required to prevent sticking of the film to itself and to the rolls.
produced with blow-up ratios of up to 3:1. Other Hytrel® grades,
Lay-flat hose liner extrusion
Thin wall Hytrel® hose liners are used for lining fire hoses
Figure 16. Extrusion of blown film
and other lay-flat hoses. Typical diameters range from
20 to 300 mm, and thickness from 0.2 to 0.7 mm. These thin-
DRIVEN PINCH ROLLS
wall liners can be made by either a horizontal vacuum sizing
technique, or by a vertical extrusion system. Normally, the softer
WIND UP Hytrel® types are used, as well as the blow molding grades,
COLLAPSING PLATE
which have been found particularly suitable because of their
high melt strength properties.
GUSSET BARS General extruder design for both processes is according to the
recommendations discussed elsewhere in this manual, and
temperature settings for particular Hytrel® grades are typical for
BLOWN TUBE GUIDE ROLLERS tubing extrusion.
AIR SUPPLY
WATER SUPPLY
SEPARATING
WALL AND SOFT VACUUM CHAMBER LUBRICATING
RUBBER SEAL WATER
FLOW CONTROL
EXTRUDER
WATER LEVEL
(Start-up)
WATER LEVEL
(Running)
SIZING DIE
19
Figure 18. Equipment for vertical extrusion
BLEED-OFF
LOW PRESSURE
AIR SUPPLY
60 mm EXTRUDER
EXTRUDER
HEAD
AIR AIR
IN COOLING
RING
HAUL-OFF
WATER WATER
WATER
WATER
OVERFLOW LEVEL WATER
IN
FLOOR LEVEL FREE TURNING ROLLERS
In practice, it has been found that due to the combination of d. Good vacuum control (liquid manometer used).
the large diameter and thin wall section, flotation occurs after e. Constant cooling water temperature.
the extrudate leaves the sizing die. This can create a problem in
In the vertical extrusion process, an extruder head is used which
maintaining a good vacuum seal.
turns the melt stream vertically downwards, and a tube is
To overcome this, a high water level is used at start-up and extruded and fed into a cooling tank located beneath the head.
when a vacuum is achieved and the tube is inflated, water is This method is shown diagramatically in Figure 18.
then drained to below the level of the sizing die. Cooling is
The diameter and wall thickness of the liner are controlled by
effected by water sprays which are directed onto the sizing die
applying a low positive air pressure through the center of the
and tube surface within the front tank section. No further cool-
mandrel (pin), and by adjustment of the extruder output relative
ing through the tank is required. There are several factors which
to the take-up speed. Various size liners can be made using the
are critical in order to achieve a consistent product. Of prime
same pin and die arrangement.
importance are:
The positive air supply used is very low pressure (approximately
a. Correct draw-down ratio (normally between 10 and 15:1).
25 kPa). A low pressure, high volume air blower is preferred
Extruder die diameter should be approximately 2.5 times
for this purpose, rather than a pressure reduced compressed
tube diameter.
air supply. Control of the internal pressure is then achieved by
b. Correct design of sizing die.
means of a bleed-off valve fitted at the connection between
c. Even flow and distribution of lubricating water at sizing die the low pressure air supply and the extruder head. A further
entry point. improvement is the provision of a return air channel through
20
the mandrel which allows air to circulate within the extruded Other polymers which have been successfully co-extruded with
tube, thereby giving improved internal cooling as well as better Hytrel® include Alcryn*, TPU, ABS, polycarbonate, PBT and PET.
pressure control. Best results are obtained by drawing down the Resins which are not normally considered to be compatible may
extruded tube to a smaller size than the extruder die, rather than still be co-extruded, provided that a suitable intermediate “tie
trying to increase its diameter with air pressure. layer” is used to provide a bond between the layers. DuPont
supplies a number of these “tie layer” resins in the Bynel®
Further details of both processes for extrusion of fire hose and
range.
other thin wall hose liners can be obtained from your DuPont
representative. Co-extruded profiles
One of the best applications for Hytrel® in coextrusion is as a
Co-extrusion flexible hinge between rigid profiles in PVC, ABS or PC. In this
Hytrel® may be co-extruded with several other resins for use in case, a grade such as 4056 may be co-extruded in such a way
many applications such as hose and tubing, profiles, sheeting that the rigid materials are vacuum calibrated (in the normal way)
and film. In this technique, Hytrel® is brought together with the but the Hytrel® section is simply water cooled and kept free
other resin (or resins) in a specially designed co-extrusion head from contact with the calibration die in order to prevent sticking.
where the different materials are fused to form distinct, well
Co-extruded (multilayer) tubes and pipes
bonded layers in a single extruded product.
Hytrel® can be successfully incorporated as one or more layers
By using co-extrusion, the finished product can combine the in a multilayer tube or pipe. It may be combined with other
advantages of two or more polymers in a cost effective way. grades of Hytrel®, or perhaps with Crastin® PBT or even Zytel®
The successful processing of Hytrel® in co-extrusion depends on nylon (with a suitable tie layer) to provide a specific combination
the following factors: of properties in the finished product.
• Compatibility of the two resins in terms of fusion or It may also be co-extruded as a thin layer in a PVC hose, for
“weldability.” example to provide a barrier against fluid permeation into the
PVC, or to prevent plasticizer extraction from the PVC. It could
• Closeness of melting points, or normal processing
also add heat resistance to the overall tube or hose.
temperatures.
In tube or pipe co-extrusion, the head and die temperatures
• Similarity of flow properties within the die (viscosity and
must take into account the melting point of each resin, and their
viscosity/shear rate relationship).
acceptable “processing windows.” Also, the design of the flow
• Design of the co-extrusion die. channels must respect each resin’s viscosity characteristics
— if their rheologies are not sufficiently close, it may be difficult
Experience has shown that Hytrel® is extremely compatible with
to ensure even flow behavior at the interface between the
most rigid and flexible PVC compounds, and equipment normally
polymers. As with co-extrusion of any material combinations,
used to co-extrude rigid and flexible PVC can give good results
the design of the co-extrusion head is critical.
where the flexible PVC is replaced with Hytrel®. The lower
melting point grades of Hytrel® must be used, however, as it is
normally necessary to limit the temperatures in the co-extrusion
*Registered trademark of Advanced Polymer Alloys (APA)
head to around 180°C in order to prevent degradation of the
PVC.
21
Troubleshooting Guide for Extrusion of Hytrel®
Blisters (on surface) 1. Substrate contains volatile substances 1. a. Pre-heat or dry substrate
when coating substrates (water, oil, etc.). (For example, when b. Clean substrate
coating textile materials) c. Increase extrusion rate
d. Decrease air-gap before cooling stage
e. Apply vacuum through mandrel
Deformed/Folded/
Warped extrudate 1. Uneven/insufficient melt tension 1. a. Increase draw-down ratio
b. Reduce melt temperature
c. Adjust die centering (tubes)
d. Hole in mandrel may be too large and should
be made smaller (cross-head covering)
2. Burr or other imperfection on die face 2. Remove imperfection
or pin
3. Draw rate too high (wire covering) 3. Reduce draw rate by lengthening cone (reduce
vacuum)
4. Draw-down ratio too high (tubes) 4. Reduce draw-down ratio
5. Uneven shrinkage (profiles) 5. a. Improve support of profile in water bath
b. Reduce melt temperature
c. Change to low shrinkage/slow crystallizing
grades of Hytrel®
22
Problem Probable Causes Suggested Solutions
Out of roundness — poor 1. Die out of round, pin/mandrel 1. Replace or re-machine die or pin
concentricity or deformed out of round or bent
extrudate (tubes or 2. Covering sags before freezing or 2. Generally, increase melt tension:
cross-head covering) extrudate sags before entering water a. Reduce temperature of melt
bath or sizing die b. Increase the rate of draw-down by either:
increasing extrusion rate, shortening the cone
length or increasing the draw-down ratio
(pin/die change)
3. Pressure applied by haul-off belts or 3. a. Reduce belt pressure
other take-up equipment is too high, b. Reduce payoff tension in cross-head extrusion
and causes deformation of the extrudate c. Increase cooling capacity to ensure that
extrudate is cold before it reaches haul-off/
wind-up equipment
23
Problem Probable Causes Suggested Solutions
Overloading of extruder drive 1. Rear barrel temperature too low 1. a. Raise rear barrel temperature
(excessive torque) b. Check thermocouple and controller of rear zone
2. Other temperature too low 2. Raise temperature
3. Incorrect screw design 3. Use correct screw design
4. Flow restrictions in head or adaptor/ 4. a. Check for cold plugs, etc.
screen area b. Increase adaptor/head temperatures
c. Check design of head
Surface roughness 1. Melt fracture (“sharkskin” or 1. Generally, reduce shear in die by:
roughness on surface) a. Reducing extrusion rate
b. Increasing die temperature
c. Increasing melt temperature
d. Increasing die opening/increasing
draw-down ratio
2. Die imperfections 2. a. Check for burrs, etc., and remove
b. Check for good finish on die and pin
3. Contamination 3. See “Contamination”
4. Wire or core vibration (cross-head 4. Use guides or pads to dampen vibration
covering)
5. Core/substrate not smooth 5. Check core/substrate
6. Build-up (deposits) on die face 6. a. Keep die face cleaned
b. Increase die temperature
7. Resin degradation — to determine if 7. See resin degradation as a cause of “bubbles”
roughness is due to melt fracture or
degradation, significantly slow down
the extrusion. If there is melt fracture,
it will disappear. Symptoms of
degradation (bubbles and discoloration)
will persist or become worse
8. Moisture in resin 8. See “bubbles”
9. Die temperature too low 9. Increase die temperature
24
Problem Probable Causes Suggested Solutions
Unmelted or frozen particles 1. Barrel temperature setting too low 1. Raise controller settings
in extrudate 2. Granules not melted early enough 2. a. Change temperature profile raising rear
in screw reducing front temperature if necessary to keep
acceptable melt temperature
b. Change screw to recommended design
3. Heater watt density too low (one 3. Change heater band to increease wattage
or more heaters is “on” most
of the time
4. Compression ratio of screw too low 4. a. Change screw to recommended design
b. Increase screen pack density
5. Inadequate screen pack 5. See 4 (b)
6. Cold spot(s) in extruder 6. a. Check operation of heaters, controllers,
and thermocouples and repair/recalibrate if
necessary
b. Raise temperatures or supply additional
heater capacity to barrel extension, adaptor,
breaker plate or die; use separate controllers for
each of these zones
c. Increase back pressure with screen pack
Voids (in center of section) 1. Too rapid cooling 1. Reduce cooling rate (use air cooling or alternate
water/air cooling)
2. Section too thick 2. Redesign to reduce thickness
3. Use of high shrinkage/fast 3. Use lower shrinkage or slower
crystallizing grade crystallizing grade
25
DuPont™ Hytrel®
For information on Engineering Polymers contact our regional headquarters or visit us on the web at plastics.dupont.com for the complete
listing of our offices around the globe.
North America
DuPont Engineering Polymers
Wilmington, Delaware, USA
Toll Free: (800) 441-0575
Tel: (302) 992-4592
Telefax: (302) 992-6713
E-mail us at: [email protected]
South America
DuPont do Brasil S.A.
Al. Itapecuru, 506 Alphaville
06454-080 Barueri-Sao Paulo
Tel: (5511) 4166-8299
Fax: (5511) 4166-8513
Asia Pacific
DuPont Kabushiki Kaisha
Sanno Park Tower, 11-1
Nagata-cho 2-chome
Chiyoda-ku, Tokyo 100-6111
Japan
Tel: (81-3) 5521 8500
Fax: (81-3) 5521 2595
Copyright © 2005 DuPont. All rights reserved. The information set forth herein is furnished free of charge and based on technical data that DuPont believes
The DuPont Oval Logo, DuPont™, The miracles of science™, Teflon®, Bynel®, to be reliable. It is intended for use by persons having technical skill, at their own risk. Because conditions
of use are outside our control, we make no warranties, express or implied, and assume no liability in
Crastin® PBT, Zytel® and Hytrel® are registered trademarks or trademarks connection with any use of this information. Nothing herein is to be taken as license to operate under or a
of E. I. du Pont de Nemours and Company or its affiliates. recommendation to infringe any patents.
K-09003-1 (8/06) Printed in the U.S.A. Caution: Do not use this product in medical applications involving permanent implantation in the human
body. For other medical applications see ”DuPont Medical Caution Statement.’