Polymer Degradation and Stability 86 (2004) 301e307

www.elsevier.com/locate/polydegstab

Degradation eects on the rheological and mechanical

properties of multi-extruded blends of impact-modied
polypropylene and poly(ethylene-co-vinyl acetate)
E. Ram rez-Vargasa,), D. Navarro-Rodr gueza, A.I. Blanqueto-Menchacab,
B.M. Huerta-Mart neza, M. Palacios-Meztaa
a
Centro de Investigacion en Qumica Aplicada, Blvd. Enrique Reyna 140, Saltillo, Coahuila 25100, Mexico
Facultad de Ciencias Qumicas UA de C, Blvd. V. Carranza y Jose Cardenas Valdes, Saltillo, Coahuila 25270, Mexico

Received 14 November 2003; received in revised form 12 March 2004; accepted 5 April 2004

Abstract
Polypropylene-(ethylene-propylene) heterophasic copolymer (PP-EP)/poly(ethylene-co-vinyl acetate) (EVA) blends of dierent
composition were multiply-extruded (nine cycles) in order to evaluate the degradation eects on the molecular weight as well as on
the rheological and mechanical properties. A decrease in molecular weight was observed in the rst three reprocessing cycles, then
this parameter remained almost constant in further recycling. Such initial decrease was attributed to chain scissions occurring mainly
in the PP-EP copolymer. As expected, the melt ow index increased with the number of processing cycles. Unlike the tensile
strength, which showed no clear tendency, the impact strength and elongation were improved with recycling. In particular, the
elongation showed a remarkable increase at EVA contents of 40 and 60 wt.%, that was apparently due to changes in morphology.
2004 Elsevier Ltd. All rights reserved.
Keywords: PP/EVA blends; Mechanical properties; Rheological properties; Recycling

1. Introduction
Plastics recycling has been successfully implemented
with primary processed materials resulting in economic
benets [1]. From environmental concerns the recycling
of wasted or rejected plastics is nowadays highly encouraged to reduce the increasing amounts of pollutants
[2]. In the plastics industry most recycling is done with
simple polymers, like homopolymers [3e6]. However,
important quantities of primary processed and wasted
materials are complex polymeric systems. Let us
consider the case of polymer blends, whose recycling
has been studied [7e12], but not as much as it should be,
taking into account their spectacular growth in applications in the last decades.

) Corresponding author. Tel./fax: C52-844-438-9839.

E-mail addresses: evargas@polimex.ciqa.mx (E. Ram rez-Vargas),
damaso@polimex.ciqa.mx (D. Navarro-Rodr guez).
0141-3910/$ - see front matter 2004 Elsevier Ltd. All rights reserved.
doi:10.1016/j.polymdegradstab.2004.04.023

An interesting class of blend is that prepared with

polypropylene (PP) and poly(ethylene-co-vinyl acetate)
(EVA), which are a semi-crystalline thermoplastic and an
elastomeric material, respectively. The EVA copolymer is
basically introduced as an impact modier for PP [13,14]
and it is dispersed as ne particles, whose shape and size
depend on two main competing factors: the coalescence
of small particles and the breaking of droplets; the latter
is induced by the high shear stresses produced during
blending. McEvoy and Krause [15] have proposed that
upon cooling, the molten EVA copolymer ows towards
the free volume generated during the PP crystallization,
leading to a phase interlocking between the two polymers. Thus, the simple solidication process produces a
kind of interfacial adhesion compatibility. Our previous
results indicate that compatibility in PP/EVA blends
is due not only to local interfacial interactions but also
to changes in the phase morphology [16]. If the PP is
modied with ethylene moieties, as is the case of the polypropylene-(ethylene-propylene) heterophasic copolymer

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E. Ramrez-Vargas et al. / Polymer Degradation and Stability 86 (2004) 301e307

(PP-EP), the compatibility with the EVA copolymer is

improved, resulting in an enhancement of both, the
elongation and the impact strength in comparison with
PP/EVA blends [17]. Such improvement in compatibility
was attributed to the occurrence of specic interactions
between the ethylene groups of the PP-EP and EVA
copolymers.
The morphological and mechanical properties of PP/
EVA blends are well known. However, there are no
reports on their recycling. PP and EVA have been
recycled but separately or in combination with some
other polymer. PP in particular has been extensively
studied due to its numerous applications [18]. For instance, Gonzalez-Gonzalez et al. [19] have made multiple recycling (19 cycles) of PP under relatively high
temperature processing conditions (195e270 (C). According to these authors, the PP undergoes chain
scission by thermo-mechanical eects. In related work,
Incarnato et al. [3] have studied the rheological and
mechanical properties of recycled PP and its blends with
virgin PP. From correlations between molecular weight,
viscosity and the number of processing cycles the
authors concluded that multiply-recycled PP (even up
to 70 wt.%) can be blended with virgin PP without any
signicant detriment in properties. Camacho and
Carlsson [20] in recycling PP/HDPE blends have observed that up to the third extrusion the shear forces
induce chain scissions on the PP backbone, then the
molecular weight of this polymer remains almost
unchanged in further processing. It has been also
determined that the PP oxidizes rst, accelerating in
turn the oxidation of the HDPE. Other investigations on
the recycling of PP-based blends have been reported
[21]. On the other hand, few studies on the recycling of
EVA [22] or EVA-based blends [23] have been reported.
A good example is the work of Sultan and Sorvic [24] on
the recycling of EVA copolymers. These authors
observed a broadening in the molecular weight distribution curve that they associated with a recombination
of allyl radicals formed just after the thermal deacetylation of the EVA copolymer. At high EVA contents gel
formation was reported to occur.
The ow properties of polymer blends may turn out
complex because they depend on variables such as
composition, molecular weight and relative viscosity of
individual components, interaction or interfacial adhesion, size and shape of dispersed particles, among
others. However, without considering these variables
(except molecular weight and viscosity of individual
components), in the present study we have observed
clear tendencies in the eects produced by the multiple
recycling (nine cycles in a twin extruder) on the
rheological and mechanical properties of PP-EP/EVA
blends, in such a way that they were explained without
ambiguity in terms of concentration and number of
reprocessing cycles.

2. Experimental
2.1. Materials and preparation of blends
Starting materials were a heterophasic polypropylene-(ethylene-propylene) (PP-EP) copolymer provided
by Himont Inc. (PP-EP, Profax 7624). The main
characteristics of this copolymer are: Mn, 8.51!104;
Mw, 4.97!105; Ip, 5.8; Tm,120 and 165 (C and melt
ow index (MFI), 2.0 dg/min at 230 (C. The ethylene
content (8 wt.%) was determined by FTIR [17]. The
EVA copolymer was from Dupont Inc. (ELVAX 3174),
with the following characteristics: Mn, 6.17!104; Mw,
2.43!105; Ip, 3.9; Tm, 85.2 (C; MFI, 8.0 dg/min at
190 (C. The VA content of the EVA copolymer was
calculated from the acetic acid loss (12.6 wt.%, at
375 (C) measured by TGA. By using a calibration curve
(acetic acid loss versus vinyl acetate content) built with
EVA standards the determined VA content in the EVA
copolymer was 17.2 wt.% (see Fig. 1).
PP-EP/EVA blends were prepared at concentrations
of 80/20, 60/40 and 40/60 wt.%. Materials were handmixed before introduction into a Werner and Peiderer
twin screw extruder (model ZSK-30) with processing
temperatures ranging from 180 to 220 (C. Blends were
obtained as molten laments, which were solidied in
a water bath to be further pelletized. Blends were
subjected to a multiple reprocessing in the twin screw
extruder under the same conditions. The maximum
number of cycles was 9 and only the 1st, 3rd, 5th, 7th and
9th reprocessed blends were selected for characterization. Finally, multiple reprocessed blends were pelletized
and introduced into a Battenfeld injection moulding
machine (BA 750 CDK) with processing temperatures
ranging from 190 to 220 (C. Two types of standard
samples were obtained for mechanical testing.

40

30

20

10

y = 1.3341x + 0.3668

0
0

10

15

20

25

30

Fig. 1. Calibration curve for the determination of vinyl acetate content

in the EVA copolymer.

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E. Ramrez-Vargas et al. / Polymer Degradation and Stability 86 (2004) 301e307

3. Results and discussion

3.1. Characterization
In studies related to polymer recycling it is important
to characterize the initial parameters, which will be the
reference of any change or evolution. Common monitoring parameters in recycling are the initial viscosity of
pure components and its molecular weight (Mw), both
giving account of the chemical decomposition. The melt
viscosity as a function of shear rate for the PP-EP and
EVA copolymers is shown in Fig. 2. It can be observed
that at low shear rates (near MFI conditions), the
viscosity of the PP-EP is higher than the viscosity of the
EVA copolymer. With increasing the shear rate the viscosity of both copolymers becomes similar (crossing
point). A further increase in shear rate produces an
inverted behaviour compared to that observed at low
shear rates. Similar curves were already reported by
Gupta et al. [25] for similar polymers. However, in the

Log melt viscosity (poises)

The ethylene content of PP-EP copolymers was

determined by infrared spectroscopy by using a FTIR
spectrometer from Nicolet (model 550) with a resolution
of 4 cm1 and 30 scans. The procedure was similar to
that reported previously [17].
The thermal characterization of resins was carried out in a dierential scanning calorimeter (DSC)
from TA Instruments (model 2920). Thermograms
were obtained from 20 to 188 (C at a heating rate
of 10 (C/min under nitrogen atmosphere.
The vinyl acetate content was determined thermogravimetrically by using a thermal analyser (TGA) from
TA Instruments (model Q 500).
Molecular weight of virgin polymers and recycled
blends were determined by gel permeation chromatography in a GPC from Waters (Alliance GPCV-2000) at
145 (C using polystyrene standards.
Rheological measurements like melt ow index
(ASTM D1238) and capillary rheometry (ASTMD3835) were carried out in a plastometer from Tinius
Olsen (model UE4-78) and in a capillary rheometer
from Instron (model 4467), respectively. The apparent
shear stress and shear rate were corrected by using the
Bagley and Rabinowitsch expressions. The test temperature was 230 (C for all measurements.
Mechanical properties like the elongation at the yield
point and the tensile strength (ASTM-D638) were
determined in an Instron universal machine (model
4301). The impact strength (ASTM-D256) was obtained
in a Custom Scientic Instruments (model 137C).
Samples for impact strength were cooled at 30 (C
for 1 h and tested immediately.

4
PP-EP
EVA

1
2

2 .5

3 .5

4 .5

Log shear rate (1/s)

Fig. 2. Melt viscosity as a function of shear rate for PP-EP and EVA
copolymers.

present work, polymers showed closer values of viscosity, which is quite favourable for blending.
Unlike the recycling of simple polymers (homopolymers), changes in the molecular weight of polymers
blends become complex and dicult to analyse. In spite
of this diculty, in the present work the monitoring of
the Mw gave us a rough idea of the decomposition of
PP-EP and EVA copolymers. Initially, a mean molecular weight was determined for blends at dierent
composition. Fig. 3 shows the weight average Mw
versus the EVA content for all blend compositions. It
can be noticed that the resulting Mw is slightly smaller
that the theoretical Mw of simple blends (straight line).
This result indicate that, although not signicant, the
Mw is already aected by the mixing process used for
the preparation of blends.
3.2. Recycling eects on the molecular weight
of PP-EP/EVA blends
Fig. 4 shows the evolution of the Mw as a function of
the number of processing cycles. It can be noticed that in
the rst cycles ( from 1st to 5th), blends with higher PPEP content show the most prominent changes in
molecular weight. Then, from the 5th to 9th cycle,
changes in Mw were less pronounced. Dierences from
one blend to the other indicate that the decrease in Mw
depends on composition and taking into account that
pronounced changes occur at high PP-EP contents, the
6

Mw x 10-5

2.2. Techniques and methods

4
2
0
0

20

40

60

80

100

Fig. 3. Weight average molecular weight (Mw) as a function of EVA

content (wt.%).

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E. Ramrez-Vargas et al. / Polymer Degradation and Stability 86 (2004) 301e307

6
4
2
0
0

10

Cycles
Fig. 4. Weight average molecular weight as a function of the number of
reprocessing cycles.

chain scissions can be attributed without ambiguity to

this copolymer [19]. Even thought no evidence of crosslinking was observed (even for the blend with the highest
EVA content), this interpretation does not exclude that
such process may occur [24]. In such a case the measured
Mw may be a result of the antagonistic eects produced
by the chain scissions (PP-EP) and crosslinking (EVA).
As is well known, the rheological and mechanical
properties of polymeric materials depend strongly on the
molecular weight [26] and this in turn on the number of
recycling processes [19]. In polymer blends the multiple
recycling also aects the overall morphology. The eects
on in molecular parameters as well as morphology
directly inuence the interactions between components
and thus may induce a modication in compatibility
[17].

3.3. Degradation eects on the rheological properties

The rheological properties of multiple recycled
polymers, particularly of the polypropylene have been
extensively studied. Gonzalez-Gonzalez et al. [19] have
made a multiple recycling (19 cycles) of a commercial
polypropylene (Mw, 3.6!105 and MFI, 3.48 dg/min)
in a single screw extruder at two temperature conditions;
one ranging from 195 to 240 (C and the other from 195
to 270 (C The Mw of this polymer fell to 2.1!105 and
1.3!105 for the low and high temperature range tested,
respectively. The decrease in molecular weight was
associated with a mechanism involving chain scissions
promoted by thermo-mechanical eects. The nal
polymers (after the 19th cycle) showed melt ow indexes
of 14.6 and 33.4 dg/min for the low and high
temperature processing conditions, respectively. This
remarkable increase in MFI corroborated the abrupt
decrease observed in the molecular weight of PP. The
recycling of PP by using a single screw extruder was also
studied by Incarnato et al. [3]. These authors reported
an interesting empirical correlation between rheological
properties and molecular parameters that can be useful
to evaluate the degradation induced by the processing
cycles. Also, a mechanical analysis of recycled PP

indicated a decrease in elongation at break as a function

of the number of cycles ( from 1 to 7) and a dependence
between molecular weight, MWD and morphology
(orientation and crystallinity) was established. In
general, the mechanical analysis showed that it is
possible to blend major amounts of recycled PP (up to
70%) with virgin PP without a signicant detriment in
properties. In the present work, the MFI of PP-EP/EVA
blends of dierent EVA content was determined after
each processing cycle (Fig. 5). It should be pointed out
that in general the MFI is superior for those blends
containing high concentrations of EVA and this is
simply due to the high initial MFI value of this
copolymer. On the other hand, the increase on the
number of processing cycles provoked in general
a monotonic increase in the MFI value, being more
remarkable for the PP-EP copolymer. This result is in
agreement with changes in molecular weight observed in
Fig. 4, where the decrease in Mw became less important
as the EVA concentration increased. The abrupt increase in MFI in the last cycles could be attributed to
degradation of the EVA copolymer due to the relatively
high temperature (230 (C) used in the MFI measurements. It should be mentioned that PP-EP/EVA blends
degrade from one cycle to another under multiple
reprocessing and that in the last cycles blends become
more susceptible to the thermo-degradation in such
a way that a high degradation rate would be expected in
the last cycles.
In order to get information that could be extrapolated to real processing conditions, capillary rheometry
measurements were carried out at shear rates close to
those normally used in extrusion and injection moulding. The viscosity of recycled PP-EP/EVA blends as
a function of shear rate is shown in Figs. 6 and 7 for the
1st and the 9th cycle, respectively. It can be seen that
blends subjected to nine processing cycles show less
dierences in viscosity between blends. This behaviour
may be attributed in part to changes in molecular weight
produced basically in the PP-EP copolymer, although
other variables like morphological parameters may also

16

Melt flow index (dg/min)

Mw x 10-5

100/0
80/20
60/40
40/60

12

0
0

10

Cycles
Fig. 5. Melt ow index (MFI) of PP-EP/EVA blends as a function of
the number of reprocessing cycles.

Log melt viscosity (poises)

E. Ramrez-Vargas et al. / Polymer Degradation and Stability 86 (2004) 301e307

305

4
100/0
80/20
60/40
40/60

1
2

2.5

3.5

4.5

Log shear rate (1/s)

Fig. 6. Melt viscosity as function of shear rate for PP-EP/EVA blends
subjected to one reprocessing cycle.

Log melt viscosity (poises)

aect the viscosity of the blends. In the rst processing

cycle important dierences in viscosity were observed at
low shear rates (close to the MFI conditions). As the
shear rate increases dierences become less important
up to an intersection point. Then at the highest shear
rates the curves are inverted. For blends subjected to
nine processing cycles smaller dierences in viscosity
were observed at low shear rates. Similarly, at high shear
rates an intersection point and inversion in the viscosity
values were observed. This behaviour seems to be
related to the combination of rheological properties of
pure components (Fig. 2). However, other authors have
made a wider explanation based on the analysis of
similar curves. This is the case of Gupta et al. [25] who
reported similar results for PP/EVA (12% of VA) blends
containing 10, 20, 30 and 40 wt.% of EVA. They have
attributed the convergence of curves to an eect produced by the shear rate on the dispersed particles.
According to these authors at low shear rates the
particles are spherical in shape and tend to be deformed
or elongated when the shear rate increases. However, at
high enough shear rates the particles break down and
become smaller in such a way that the melt viscosity is
less aected. At this point blends at all compositions may
have almost the same melt viscosity. This behaviour has
also been observed by Wu [27] and Min et al. [28].
In order to explore the eect of the number of cycles
on the processing characteristics, a viscosity versus
shear rate plot was built by using capillary rheometry

Fig. 8. Melt viscosity as function of shear rate of the PP-EP/EVA,

80/20 blend subjected to dierent number of reprocessing cycles.

measurements (Fig. 8). Because all blends have shown

a similar behaviour only the curves corresponding to the
PP-EP/EVA 80/20 are presented. In this gure only
small variations in viscosity as a function of processing
cycles were observed. This result indicates that the
extruders or injection moulding machines used for the
processing of virgin PP-EP/EVA blends will not require
signicant changes in operation conditions for the
processing of recycled blends, as those here studied.
3.4. Degradation eects on the mechanical properties
The impact strength of PP-EP and PP-EP/EVA
blends subjected to multiple reprocessing is shown in
Fig. 9. It can be noticed that for the PP-EP copolymer
this property increases slightly in the rst reprocessing
cycles, then it remains almost constant as the number of
recycling processes increases. However, the case of PPEP/EVA blends is a little bit dierent showing a monotonic increase from one cycle to the other, particularly
for those blends with high EVA contents. It should be
emphasized that in the twin screw extruder the blend is
subjected to high shear rates that may produce the
breaking of particles ( particularly the big ones), leading
to a reduction of both the size and size distribution of
the dispersed phase and to a more homogeneity. All
these morphological changes favour the interfacial

4
100/0
80/20
60/40
40/60

1
2

2.5

3. 5

4.5

Log shear rate (1/s)

Fig. 7. Melt viscosity as function of shear rate for PP-EP/EVA blends
subjected to nine reprocessing cycles.

Fig. 9. Impact strength as a function of the number of reprocessing

cycles for PP-EP/EVA blends.

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E. Ramrez-Vargas et al. / Polymer Degradation and Stability 86 (2004) 301e307

interaction between the PP-EP and EVA copolymers

[17], and this in turn is reected in an slight improvement of the impact strength. There are few reports of an
improvement of the impact strength with recycling. One
of the them is the recycling of compatibilized LDPE/PP
blends reported by Bertin and Robin [21]. In just one
step of recycling in a twin screw extruder these authors
observed an interesting improvement in the impact
strength as well as in other mechanical properties.
Gupta et al. [13] have measured the impact strength of
PP/EVA blends at compositions ranging from 0 to 40
wt.% of EVA copolymer and they have observed an
increase in this property as a function of both, the EVA
content and test temperature. This behaviour was also
observed by Dutra et al. [29]. On the other hand, the
elongation at the yield point for PP-EP and PP-EP/EVA
blends as a function reprocessing is shown in Fig. 10. All
blends showed a slight and continuous increase in
elongation, except for the PP-EP/EVA 60/40, which
showed a quite remarkable increase for all recycling
steps. Also, the PP-EP/EVA 40/60 and 60/40 showed
a pronounced increase above the seventh cycle. In
previous studies on PP-EP/EVA blends [16,17] we have
demonstrated that these blends show a compatibility
window at compositions between 40 and 60 wt.% of
EVA. A this composition, EVA particles coalesce to
form interconnected elongated droplets improving the
elongation of blends. For recycled blends the elongation
is also improved by the homogeneity achieved during
mixing, as reported by Varghese et al. [30] for
reprocessed NBR/EVA blends and Bertin and Robin
for recycled LDPE/PP blends [21]. Both, the interconnection of the EVA phase and the homogeneity in the
distribution of EVA particles produces a favourable
eect in elongation.
On the other hand, Fig. 11 shows the tensile strength
as a function of the number of reprocessing cycles for
PP-EP/EVA blends. It can be seen that this property is
highly dependent on composition and only slightly
dependent on reprocessing. For the PP-EP the main
decrease in tensile strength occurs is the rst three cycles,
then it becomes practically constant up to the ninth

Fig. 10. Elongation at the yield point as a function of the number of

reprocessing cycles for PP-EP/EVA blends.

Fig. 11. Tensile strength as a function of the number of reprocessing

cycles for PP-EP/EVA blends.

cycle. This result is in concordance with the initial

changes observed in molecular weight as a function of
recycling. However, for blends there is no clear tendency
(particularly for those of high EVA content) due to the
combined morphological [30] and molecular eects [24].
The results obtained here can be compared with those
of similar blends using industrial polymers. A close
example is that of the EVA/HDPE blend reported by
Zattera et al. [31] which was prepared with residual EVA
from industry aiming to get economical benets. The
knowledge of the molecular characteristics as well as the
rheological and mechanical properties of recycled
blends, as those here studied, gave us a good indication
on how long (maximum recycling) it is possible to blend
recycled polymers with crude polymers to accomplish
with the quality levels of materials required for a specic
application.

4. Conclusion
A series of PP-EP/EVA blends of dierent composition were subjected to nine reprocessing cycles in a twin
screw extruder. It has been observed that the molecular
weight of the blends decreases in the rst three reprocessing cycles, then remains almost constant. According to the changes observed for dierent blends, the
decrease in molecular weight could be attributed
basically to chain scissions occurring almost exclusively
in the PP-EP copolymer. The melt viscosity of blends
decreased from one cycle to the other, although, it is
important to point out that in general only minor
changes were observed in this property, even after the
ninth processing cycle. On the other hand, the impact
strength as well as the elongation have shown in general
a slight improvement with recycling, except for PP-EP/
EVA blends with high EVA content (40 and 60 wt.%),
which showed a remarkable increase in elongation. In
contrast, the tensile strength has shown in general
a slight decrease, but without a clear tendency. Variations in mechanical properties were attributed either to

E. Ramrez-Vargas et al. / Polymer Degradation and Stability 86 (2004) 301e307

the decrease in molecular weight or to changes in

morphology, like those related to the formation of
elongated particles and/or to the improvement in
homogeneity normally achieved during mixing. According to previous reports, these changes in morphology
seems to improve the compatibility of blends. Finally, it
can be concluded that recycled PP-EP/EVA blends can
be blended with virgin ones without a signicant
detriment in the rheological and mechanical properties.

Acknowledgements
The authors wish to thank the Mexican National
Council of Science and Technology (CONACYT) for
the grant 28554-U.

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