Recycling of Condensation Plastics: GPEC 2004 Paper Abstract #52

GPEC 2004 Paper Abstract #52:
Title: Cesa-extend a User Friendly Technology to Enhance Reprocessing and

Recycling of Condensation Plastics
Author(s): V. Karayan, Clariant Masterbatches, and M. Villalobos, Johnson Polymer
Recycling of condensation thermoplastics such as polyesters (PET, PBT),

polyamides (6, 6-6), polyurethanes, polycarbonates, and their blends, has found
severe limitations owing to a simple reason: the costs associated to current
process technology employed to revert MW degradation of these thermoplastics
renders the recycled products uneconomical and/or unsuitable for many
demanding applications. As a result, degraded post-consumer reclaimed plastics
is still the main recycle stream, mostly directed to low value added applications
such as fibers and film.
During 2003, Clariant Masterbatches and Johnson Polymer jointly introduced to

the market a family of chain extenders or "recycling aids" under the trademark
Cesa-extend. These additives are based on proprietary technology of multi-
functional acrylic oligomers formulated into masterbatches tailored for effective
and user-friendly use in different thermoplastic systems. Cesa-extend products
are characterized by their ability to dramatically increase the molecular weight, as
well as the mechanical and rheological properties of virgin, reprocessed, and
post-consumer recycled condensation plastics when used in very low
concentration in simple extrusion or injection molding equipment.
Multiple examples in which recycled feedstock has been enhanced with Cesa-
extend products during a simple extrusion step to meet demanding engineering
applications requirements will be given in the areas of polyesters, polyamides
and other thermoplastics.
Vahe Karayan PhD

Technical manager
Clariant Additive Masterbatches
382 Arbor Court
Winchester, VA 22602
PHONE: 540-665-1865 X 106
FAX: 540-665-2917
CESA-extend a New Technology to Enhance Reprocessing and Recycling
of Condensation Polymers
Vahe Karayan PhD, Clariant Additive Masterbatches, Marco Villalobos PhD, Johnson Polymers
INTRODUCTION:
Polyethylene terephthalate (PET) is an important commercial polymer used

widely in the manufacture of plastic products such as films, bottles, sheet and
other molded and extruded articles. In a life cycle, these materials experience
several process steps, from a synthesis process, followed by an extrusion step,
and a final processing step which may be another compounding extrusion
operation followed by thermoforming, blow molding, fiber spinning, or injection
molding in the molten state. All of these steps occur under high temperature
conditions which affect the molecular weight (MW), rheological properties, melt
strength and processing abilities. As a result recycled PET is mostly employed in
low-end applications or is reconstituted by a solid stating process that requires a
very large capital investment.
The current yearly consumption of recycled PET in the United States is about
700 million pounds. In recent years, increased attention has been focused on
improved methods of recycling the articles made from these polymers, with an
eye toward resource conservation and environmental protection.
CURRENT TECHNOLOGY:
There are a number of processes in the industry used to minimize loss in

molecular weight and maintain or even increase the molecular weight of the PET
for processing or recycling. Most of these processes employ as main processing
equipment either an extruder, a solid state polycondensation reactor, or both in
sequence, or similar equipment designed for melt or high viscosity material
processing.
As a critical component of any of these processes, chemical reactants known in

the industry as "chain extenders" are employed. Chain extenders are, for the
most part, functional molecules that during any or all of the described processing
steps are added as additives to the extruder or reactor with the purpose of "re-
coupling" polycondensate chains that have depolymerized to some degree.
Normally the chain extender has two or more chemical groups that are reactive
to the chemical groups formed during the molecular weight degradation process.
By reacting the chain extender molecule to two or more polycondensate
fragments it is possible to re-couple them thus decreasing or even reverting the
molecular weight degradation process.
In order to have efficient chain extension at reasonable residence times most of
the known chain extenders require the use of pre-dried polycondensate material,
operation at high vacuum, and varying amounts of catalyst and stabilizers, to be
employed during processing. Without these features the extent of molecular
weight increase is limited and the resulting product shows lower molecular weight
and less than desired properties.
As the functionality of the chain extender increases, so does the number of

polycondensate chains that can be coupled onto each chain extender molecule,
and thus its effectiveness in re-building molecular weight. However, it is easy to
see that as the functionality of these chain extenders increase so does the
degree of branching of the resulting product and the potential for onset of
gelation. The strong negative effects that extensive branching has on the degree
of crystallinity and thus on the mechanical properties of a semi-crystalline
polycondensate, as well as the negative implications of the presence of varying
amounts of gel in any product.
A need exists for chain extenders that may be used in any suitable process while
avoiding the processing limitations described above. Such chain extenders
provide substantial economic advantage in processing, reprocessing and
recycling of polycondensates over existing chain extenders and the methods for
their use.
CESA-extend a MULTIFUNCTIONAL OLIGOMERIC CHAIN EXTENDER:
One type of chain extender that has been effective in overcoming the problems
encountered are those based on epoxy-functional styrene acrylic copolymers
produced from monomers of at least one epoxy-functional acrylic monomer and
at least one non-functional styrenic and/or acrylate monomer. Clariant Additive
Masterbatches and Johnson Polymers Company have introduced a
multifunctional oligomeric chain extender masterbatch, CESA®-extend, to reduce
the degradation of PET due to process heat and moisture.
This product is particularly well suited for use with reprocessed or recycled
plastics. It is characterized by its ability to revert the post-processing molecular
weight decrease in different polycondensates from the minimum value reached
without chain extension, back to the initial molecular weight values or even larger
than the original molecular weight values. This is achieved without the incidence
of gel and without adverse effects on mechanical, thermal, or rheological
properties at a target polycondensate molecular weight.
CESA®-extend provides several benefits in a variety of applications. CESA®-

extend can be used as a substitute for solid state polymerization in recycling of
PET. Compounders can benefit from improved compatibility with other types of
plastics such as other polyesters, polycarbonate, polyamide, etc. Converters can
benefit from improved extrusion blow molding and melt strength, injection blow-
molding crystallinity and toughness in blow molding operations. In foamed sheet,
benefits can be expected due to countered effects of endothermic foaming
agents. In industrial fabrics the use of these chain extenders can improve coating
adhesion, tenacity and melt strength. The following data will show the influence
of the use of CESA-extend on the melt strength and processability of recycled
PET.
OBJECTIVE:
A series of laboratory experiments were conducted to determine the effect of the

addition of CESA-extend on the die sag and processability of PET extruded
sheet.
EQUIPMENT:
A 27 mm Leistritz twin screw extruder with an 8” sheet die fitting and down
stream pick up rolls were used for the experiments.
The pick up rolls were aligned to the same height as the extruder die lip, and the
distance between the two was kept constant at 6.25 inches apart. This distance
was determined by extruding a 100% virgin PET and the process was stabilized
without tearing the sheet or approaching the die lip so close that the sag was
eliminated.
The distance between the die lip and the floor was measured as 41.25 inches,
the RPM of the extruder and the speed of the pick up rolls were kept constant at
90 RPM and 4.3 ft/min respectively. The melt temperatures were also kept
constant at 453°F, torque and discharge pressures were recorded and reported
for each experiment (table 1).
EXPERIMENTS:
Once these reference conditions were set, a series of extrusions were run with
the addition of two different CESA-extend masterbatches, one was a
masterbatch in a PET carrier (CESA-extend 9930), and the other was a styrenic
carrier masterbatch (CESA-extend 1598). After each run was stabilized the
distance between the floor and the lowest sag point in the film between the die lip
and the pick up rolls was measured and recorded (table 2). Each test sample
was dried at 200°F for six hours and the moisture contents were measured to be
below 100 ppm.
Table 1:
Sample Description % Torque Discharge

Pressure PSI
Sample 1 100% PET 55 70

Sample 2 0.25% CESA-extend 9930 49 90
Table 2:
Sample Description Sheet To Floor Sag Die Sag

(inches) (inches) Reduction
Sample 1 100% PET 39.5 1.75 -

Sample 2 0.25% CESA-extend 9930 39.5 1.75 0.00%
Sample 4 1.00% CESA-extend 9930 40.25 1 42.86%
Sample 7 0.50% CESA-extend 1598 40 1.25 28.57%
OBSERVATIONS & CONCLUSIONS:
The results in tables 1 and 2 show that the addition of either of the CESA-
extend masterbatches slightly reduces torque, and increases die pressure ,
resulting in improved and eventual elimination of the sag observed when no
A D D IT IO N o f C E S A -e x te n d v s D IE S A G
1 .8
1 .6
1 .4
1 .2
DIE SAG in inches
9930
0 .8 1598
0 .6
0 .4
0 .2
0
0 0 .2 5 0 .5 1 2
% C E S A -e x te n d
Figure 1:
CESA-extend has been added to the PET (Photo 1 & 2). The CESA-extend
with the styrenic masterbatch is slightly more effective compared to the PET
carrier based masterbatch, at 0.25% of either carrier masterbatch shows no
effect in the case of the PET carrier masterbatch, compared to 14.29% less sag
with the styrenic carrier masterbatch (fig. 1 & 2).
The virtual elimination of the severe die lip sag demonstrates the positive effect
of CESA-extend on the melt strength and dramatic improvement in processing
capability of PET sheet.
Figure 2:
% SAG REDUCTION vs % CESA-extend
100
2 100
57.14
1
42.86
% CESA-extend
28.57
0.5 1598
14.29
9930
14.29
0.25
0
0
0 0
0 10 20 30 40 50 60 70 80 90 100
% SAG REDUCTIO N
Photo 1:
Photo 2:

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GPEC 2004 Paper Abstract #52:

Title: Cesa-extend a User Friendly Technology to Enhance Reprocessing and

Author(s): V. Karayan, Clariant Masterbatches, and M. Villalobos, Johnson Polymer

Recycling of condensation thermoplastics such as polyesters (PET, PBT),

During 2003, Clariant Masterbatches and Johnson Polymer jointly introduced to

Vahe Karayan PhD

Polyethylene terephthalate (PET) is an important commercial polymer used

There are a number of processes in the industry used to minimize loss in

As a critical component of any of these processes, chemical reactants known in

As the functionality of the chain extender increases, so does the number of

CESA-extend a MULTIFUNCTIONAL OLIGOMERIC CHAIN EXTENDER:

CESA®-extend provides several benefits in a variety of applications. CESA®-

A series of laboratory experiments were conducted to determine the effect of the

Sample Description % Torque Discharge

Sample 1 100% PET 55 70

Sample Description Sheet To Floor Sag Die Sag

Sample 1 100% PET 39.5 1.75 -

% SAG REDUCTION vs % CESA-extend

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