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European Polymer Journal 44 (2008) 755–768
JOURNAL
www.elsevier.com/locate/europolj
Received 24 August 2007; received in revised form 12 December 2007; accepted 13 December 2007
Available online 8 January 2008
Abstract
In this work, poly(vinyl butyral) (PVB) film originated from the mechanical separation of windshields was tested as an
impact modifier of Polyamide-6 (PA-6). The changes undergone by PVB film during the recycling process and the blend
manufacturing were evaluated by thermal analyses, infrared spectroscopy and loss on ignition. Blends of PA-6/original
PVB film and PA-6/recovered PVB film were obtained in concentrations ranging from 90/10 to 60/40. The mechanical
properties of the blends were investigated and explained in light of the blends morphologies, which in turns were correlated
to the changes undergone by the PVB film during the recycling process. The original film presented a plasticizer content of
33 wt.%, which decreased to as low as 20 wt.% after the recycling and blend preparation processes. The PA-6/PVB film
blends presented lower values of tensile strength and Young’s modulus than Polyamide-6, but all blends presented a dra-
matic increase in their toughness, with a special feature for the 40 wt.% blend, which resulted in a super toughened material
(impact strength exceeding 500 J/m). Similar results were obtained with recovered PVB film and super tough blends were
also obtained. The use of recovered PVB resulted in a smaller improvement of the impact strength due to the loss of plas-
ticizer undergone during the recycling process. The morphological observations showed that if the interparticle distance is
smaller than around 0.2 lm (critical value), the notched Izod impact strength values increase considerably and the fracture
surface of blends exhibit characteristics of tough failure.
Ó 2007 Elsevier Ltd. All rights reserved.
0014-3057/$ - see front matter Ó 2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.eurpolymj.2007.12.012
756 T.S. Valera, N.R. Demarquette / European Polymer Journal 44 (2008) 755–768
presence of plasticizer, PVB film possesses similar where s is the interparticle distance between the sur-
properties to rubber [4]. In spite of the high price faces of two nearest neighboring particles, d is the
of PVB film (about US$15/m2) and the large quan- particle diameter and / is the rubber volume
tity of windshields that are annually discarded in fraction.
landfields (100 thousand tons per year of which The critical interparticle distance is independent
7% consist of PVB film, in the USA alone [5]) very of rubber volume fraction and particle size and is
little work has been conducted on finding alterna- characteristic of a given matrix. This parameter
tives to disposal of laminated glass residues to land- alone can explain the effects of rubber volume frac-
fields. Cha et al. [4,6,7] showed that it was possible tion, particle size, polydispersity, coalescence of
to use uncontaminated scrapped PVB film collected rubbery phase and morphology on toughness [22].
from windshield production as an impact modifier Since Wu proposed the interparticle distance model,
of Polyamide-6 (Nylon-6). Polyamides are pseudo- many authors worked on the subject [27–34,36,37]
ductile polymers often blended to rubbers [8] to and it was found that the critical interparticle dis-
enhance their low notched impact strength [9]. The tance can be affected by different parameters, such
PVB film used by Cha et al. [4,6,7] was very similar as temperature and speed of impact tests, notch
to virgin PVB film as it corresponded to the indus- radius of samples for impact test, interfacial tension
trial residues that could not be used in the wind- between blend components and other properties of
shields. However, during the production of the rubbery and matrix phases [29,30,32,33,36,37].
windshields and the recycling process, the properties In the present work, PVB film originated from the
of PVB film may change: the plasticizer may be mechanical separation of windshields, either from
eliminated and the PVB may suffer degradation industrial fabrication waste or from post-consump-
[2,3,10]. It is therefore of interest to study the tion products was tested as an impact modifier for
changes undergone by PVB film during the manu- Polyamide-6 (PA-6). The changes undergone by the
facturing of the windshields and recycling process PVB film during windshield manufacture and recy-
and the possibility of using the PVB film residue cling process were evaluated. Blends of PA-6/origi-
as impact modifier. nal PVB film/ and PA-6/recovered PVB film were
Polymer toughening has drawn a lot of attention obtained. Their mechanical properties were com-
from academics and plastic industry [4,6,7,9,11–37] pared and explained in light of blend morphology
as impact strength is one of the most important and of the changes undergone by the PVB film during
mechanical properties of plastics. It is well known the blend manufacturing and the recycling process.
that pseudo-ductile matrixes, such as Polyamides
toughened with rubber material, present higher duc- 2. Experimental
tility, crack resistance and mainly greater impact
strength, when compared to the one of the pure 2.1. Materials
matrix [23]. Various theories have been proposed
to explain toughening mechanism, including stress The properties of the polymers used in this work
relief by cavitation of rubber particles, matrix craz- are listed in Table 1. Three types of PVB were used
ing and shear yielding. More details can be found in in this work: original PVB film corresponding to
different monographs on the subject [8,9,22,23,25– the material used in the production of windshields
28]. (Solutia, Saflex RB41), recovered PVB film origi-
Wu [22,26] proposed that interparticle distance nated from the grinding of windshields rejected in
(between the nodules of the dispersed phase) is the the production line or post-consumption, and pure
most important parameter that controls the brit- PVB without plasticizer to quantify the loss of plas-
tle-to-tough transition of rubber/polymer blends. ticizer from the PVB film during the recycling pro-
If the interparticle distance, given by Eq. (1) is smal- cess. Two types of recovered PVB film were used:
ler than a critical value (called critical interparticle one was originated from an industrial recycling com-
distance) the blend will be tough, otherwise, the pany (R2) and the other (R1) was ground using a
blend will be brittle: modified blade grinder, in our laboratories. The
ground material, originated from both the industrial
" 13 #
p and lab-scale process, was sieved (ASTM #10, sieve
s¼d 1 ð1Þ opening 2 mm) and the passing material was blended
6/
to Polyamide-6 by extrusion. The PVB plasticizer
T.S. Valera, N.R. Demarquette / European Polymer Journal 44 (2008) 755–768 757
12
2.3. Characterization 0
0 10 20 30 40 50
A Nicolet 560 IR – Magna infrared spectrometer Fig. 1. Calibration curve used to determine the plasticizer
was used to access the possible degradation of PVB content.
758 T.S. Valera, N.R. Demarquette / European Polymer Journal 44 (2008) 755–768
a c
Intensity (a.u.)
Intensity (a.u.)
8
8
7 7
6
5
6
4 5
3
4
2 3
2
1 1
b d
Intensity (a.u.)
Intensity (a.u.)
6
5
8 4
7
6 3
5 2
4
3
2 1
1
3200 3150 3100 3050 3000 2950 2900 2850 2800 2750 2700 2000 1500
Wavenumber (cm-1) Wavenumber (cm-1)
Fig. 2. Infrared spectra of the PVB films. 1 = original PVB film; 2 = R2 recovered PVB film; 3 = R1 recovered PVB film; 4 = original
PVB film (1 extrusion step); 5 = original PVB film (2 extrusion steps); 6 = R1 recovered PVB film (1 extrusion step); 7 = R2 recovered
PVB film (2 extrusion steps); 8 = R2 recovered PVB film (1 extrusion step). (a) The band at 3489 cm1, corresponding to –OH group; (b)
together with the band relative to C–H stretching at 2970 cm1; (c) the band at 1140 cm1 relative to C–C(@O)–O stretching of vinyl
acetate units; and (d) the band at 1730 cm1 of C@O group.
Table 3 Table 4
Glass transition temperature (Tg) of PVB copolymer and PVB Thermogravimetric analyses of PA-6, PVB copolymer, PVB
films, and the melting temperatures of blends films, and blends
Samples Glass Melt Samples Weight
temperature temperature loss (%)
(°C) (°C) Original PVB film 4.1
PVB copolymer 71 R1 recovered PVB film 2.8
Original PVB film 4 R2 recovered PVB film 2.1
R1 recovered PVB film 11 PA-6 0.7
R2 recovered PVB film 13 PA-6/original PVB film (90/10) – single extrusion 2.5
PA-6 222 PA-6/original PVB film (80/20) – single extrusion 3.3
PA-6/original PVB film (90/10) – 222 PA-6/original PVB film (70/30) – single extrusion 3.5
single extrusion PA-6/original PVB film (60/40) – single extrusion 3.8
PA-6/original PVB film (80/20) – 222 PA-6/original PVB film (80/20) – double extrusion 2.6
single extrusion PA-6/R1 PVB film (80/20) – single extrusion 2.0
PA-6/original PVB film (70/30) – 222 PA-6/R2 PVB film (80/20) – single extrusion 1.5
single extrusion PA-6/R2 PVB film (80/20) – double extrusion 1.2
PA-6/original PVB film (60/40) – 221 PA-6/original PVB film (60/40) – double extrusion 2.7
single extrusion PA-6/R1 PVB film (60/40) – single extrusion 2.2
PA-6/original PVB film (80/20) – 220 PA-6/R2 PVB film (60/40) – single extrusion 2.0
double extrusion PA-6/R2 PVB film (60/40) – double extrusion 1.6
PA-6/R1 PVB film (80/20) – 219
single extrusion
PA-6/R2 PVB film (80/20) – 220 film maintains the thermal properties of the matrix,
single extrusion
PA-6/R2 PVB film (80/20) – 220
one of requirements for an efficient toughness agent,
double extrusion besides the improvement in impact properties [8]. It
PA-6/original PVB film (60/40) – 220 can also be noticed in Table 4 that the blends with
double extrusion higher PVB film content present the greatest weight
PA-6/R1 PVB film (60/40) – 221 losses. These results are in good agreement with the
single extrusion
PA-6/R2 PVB film (60/40) – 220
ones presented in Table 2 since the PVB film weight
single extrusion loss is attributed to loss of plasticizer, the loss is
PA-6/R2 PVB film (60/40) – 220 greater for the blends containing higher plasticizer
double extrusion concentrations in the films.
10
1000 10000
Table 5
Dispersed phase/matrix viscosity ratio for all studied binary systems at a shear rate that corresponds to the injection molding shear rate
(10,000 s1)
Sample Viscosity ratio Weight fraction of plasticizer (%)
Original PVB film (single extrusion)/PA-6 (single extrusion) 0.36 28
Original PVB film (double extrusion)/PA-6 (double extrusion) 0.56 24
R1 recovered PVB film (single extrusion)/PA-6 (single extrusion) 0.51 21
R2 recovered PVB film (single extrusion)/PA-6 (single extrusion) 0.53 20
R2 recovered PVB film (double extrusion)/PA-6 (double extrusion) 0.58 19
For comparison purposes, the plasticizer content of PVB films presented in Table 4 is shown again.
3.4. Blend morphology PVB film (2E) blend. These results can be explained
in light of viscosity ratio that increases during the
Fig. 4 presents typical morphologies of the recycling process or after the second extrusion.
blends studied here. Fig. 4a and b shows PA-6/ori- These results are in good agreement with the results
ginal PVB film (60/40) blend, submitted to, respec- of Wu [40] who suggested that the finest morphol-
tively, one and two extrusion steps, Fig. 4c and d ogy is reached when the viscosity ratio is close to
shows PA-6/R2 recovered PVB film (60/40), after one.
one and two step extrusions, respectively. Table 6
summarizes the quantitative experimental results 3.5. Mechanical properties of the blends
of morphological observations. For comparison
purposes, the notched Izod impact strength values 3.5.1. Original PVB film/PA-6 blends
obtained for the blends are also presented. It can Figs. 5 and 6 present the tensile strength and
be seen that all blends studied present particle sizes Young’s modulus of the blends as a function of
greater than 0.1 lm and below 1 lm, and exhibit the original PVB film content (wt.%), respectively.
low polydispersity (dv/dn < 2), which are favorable The results show that both the tensile strength and
conditions for a successful rubber toughening modulus decreased when the PVB content
[8,23]. It can be also seen from Table 6 that dn increased. A reduction in those two mechanical
increases with increasing PVB film concentration properties is a common observation in rubber
due to dispersed phase coalescence. It can be also toughened polymers because of the lower strength
seen from Table 6 that dn of PA-6/original PVB film and modulus of the dispersed phase [9,22–28].
(1E) blend is larger than the one of PA-6/R1 recov- Fig. 7 presents the notched Izod impact strength
ered PVB film (1E) and PA-6/R2 recovered PVB of the blends using original PVB films. It can be seen
film (1E) blends, and that dn of PA-6/original PVB from Fig. 7 that the notched Izod impact strength
film (1E) blend is larger than dn of PA-6/original increases when the PVB film content increases,
762 T.S. Valera, N.R. Demarquette / European Polymer Journal 44 (2008) 755–768
Fig. 4. Typical morphologies of the blends. 1E = one extrusion step and 2E = two extrusion steps. (a) PA-6/original PVB film (60/40), 1E,
after ethanol etching. (b) PA-6/original PVB film (60/40), 2E, after ethanol etching. (c) PA-6/recovered PVB film (60/40), 1E, after ethanol
etching. (d) PA-6/recovered PVB film (60/40), 2E, after ethanol etching.
Table 6
Quantitative results of the morphology of studied blends: dv = volume average diameter and dn = number average diameter
Sample dn dv Polydispersity (dv/dn) Notched Izod impact strength (kJ/m2)
PA-6/original PVB (90:10), 1E 0.53 1.04 1.9 166 ± 12
PA-6/original PVB (80:20), 1E 0.68 1.06 1.6 233 ± 48
PA-6/original PVB (70:30), 1E 0.86 1.40 1.6 326 ± 49
PA-6/original PVB (60:40), 1E 1.05 1.79 1.7 1590 ± 39
PA-6/original PVB (80:20), 2E 0.53 0.97 1.8 215 ± 23
PA-6/original PVB (60:40), 2E 0.60 0.86 1.4 1279 ± 69
PA-6/R1 recovered PVB – (80:20), 1E 0.44 0.71 1.6 202 ± 18
PA-6/R2 recovered PVB – (80:20), 1E 0.48 0.91 1.9 202 ± 26
PA-6/R2 recovered PVB – (80:20), 2E 0.57 1.02 1.8 196 ± 26
PA-6/R1 recovered PVB – (60:40), 1E 0.61 0.99 1.6 1289 ± 46
PA-6/R2 recovered PVB – (60:40), 1E 0.51 0.97 1.9 1239 ± 72
PA-6/R2 recovered PVB – (60:40), 2E 0.59 0.92 1.6 1108 ± 40
1E = one extrusion step and 2E = two extrusion steps. For comparison purposes, the notched Izod impact strength values of the blends
are also presented here.
and that the PA-6/original PVB film blends can be et al. [4], who used scrapped PVB films, very similar
considered tough (for PVB film concentrations up to original PVB film, as an impact modifier for Poly-
to 30%) and super tough (for PVB film concentra- amide-6. The greatest difference between the values
tion of 40%) [8]. The results obtained in this work reported by the authors and the results obtained
partially corroborate the results reported by Cha in this work is in the impact strength values of the
T.S. Valera, N.R. Demarquette / European Polymer Journal 44 (2008) 755–768 763
70 2000
60
40 1200
30
800
20
400
10
0
0 10 20 30 40 0
PVB Film content (wt.%) 0 10 20 30 40
PVB Film content (wt.%)
Fig. 5. Tensile strength versus original PVB film content (wt.%).
Fig. 7. Notched Izod impact strength (J/m) as a function of
dispersed phase content (wt.%).
2300
Original PVB film (1E)
2100 Original PVB film (2E) Interparticle distance
Average particle diameter
1900 1800
Young's Modulus (MPa)
1200
1300
1000
1100
800
900
600
700 70/30 Blend 70/30 Blend
400
80/20 Blends
500 200
0 5 10 15 20 25 30 35 40 45 80/20 Blends
90/10 Blends
PVB Film Content (wt.%) 0
0.01 0.1 1 10
Fig. 6. Young’s modulus versus original PVB film content Interparticle distance (μm) or Average particle diameter (μm)
(wt.%). 1E = material extruded once, 2E = material extruded
twice. Fig. 8. Notched Izod impact strength versus interparticle dis-
tance and average particle size.
Fig. 9. Micrograph of the notched Izod impact fracture of (a) PA-6, (b) PA-6/original PVB film (80/20) blend, (c) PA-6/original PVB film
(60/40) blend, (d) a magnification of 60/40 blend micrograph, after etching.
20 wt.% present an interparticle distance greater surfaces show the presence of two different regions
than the critical. The interparticle distance of all in the PA-6 and 80/20 blend specimens (Fig. 9a
blends seem to be dependent only on their PVB con- and b). The inside region of the circles presented
tent, regardless the kind of PVB film used (original in Fig. 9a and b features a mirror zone, which is
or recovered), or the number of extrusion steps (sin- commonly observed in samples for which fracture
gle or double). is preceded by craze formation. The outside circle
Fig. 9 shows typical fracture surfaces of notched region, called hackle region [41], presents rough sur-
Izod impact strength specimens of PA-6 and PA-6/ faces, with divergent lines pointing towards the
PVB film (80/20 and 60/40) blends. The fracture crack propagation directions. The 60/40 blends pre-
T.S. Valera, N.R. Demarquette / European Polymer Journal 44 (2008) 755–768 765
70
50
Tensile Strength (MPa)
40
62
60
30
44
43
42
42
41
41
20
37
36
36
24
10
0
PA-6 (1 and 2E) PVB O (1E) PVB O (2E) PVB R2 (1E) PVB R2 (2E) PVB R1 (1E)
Fig. 10. Tensile strength versus recovered and original PVB film content. The specimens were extruded once or twice. 1E = material
extruded once, 2E = material extruded twice, R1 = recovered film using lab-scale grinder; R2 = recovered film using an industrial grinder;
O = original film.
2500
PA-6/PVB film (80/20)
PA-6/PVB film (60/40)
2000
Young’s Modulus (MPa)
1500
2093
2075
1000
1695
1698
1596
1600
1259
1136
1139
1100
1091
500
793
0
PA-6 (1 and 2E) PVB O (1E) PVB O (2E) PVB R2 (1E) PVBR2(2E) PVB R1 (1E)
Fig. 11. Young’s modulus of the blends with recovered and virgin PVB film. 1E = material extruded once; 2E = material extruded twice;
R1 = recovered film using lab-scale grinder; R2 = recovered film using an industrial grinder; O = original film.
sented in Fig. 9c show an extensive matrix yielding, present greater fracture energy than 80/20
characteristic deformation of tough failure. The blends. These observations are in good agreement
tough fracture proceeds entirely within the PA-6 with the interparticle distance parameter since the
matrix, without exposing the PVB film particles (see 60/40 blends exhibit values of interparticle distance
Fig. 9d). Since the shear yielding of the matrix is smaller than the critical value (around 0.2 lm),
more effective to improve the impact strength whereas 80/20 blends presented values above the
than crazing, it is expected that the 60/40 blends critical.
766 T.S. Valera, N.R. Demarquette / European Polymer Journal 44 (2008) 755–768
3.5.2. Recovered PVB film/PA-6 blends (2) The notched Izod impact strength values of the
The PVB concentrations that resulted in best blends containing recovered films are higher
combination of impact strength and tensile proper- than the ones for pure PA-6. However, the
ties were found to be 20 and 40 wt.% of PVB film. blends containing recovered films show a lower
Adding 40 wt.% PVB film to PA-6 resulted in an impact strength value than the ones containing
increase of impact strength of about 1400% when the original PVB film, except in the case of the
compared to the one for pure PA-6, although pre- 60/40 original PVB blend extruded twice.
senting the smallest tensile strength and modulus. (3) Independently of the type of PVB film used,
Adding 20 wt.% PVB film to PA-6 resulted in a super tough blends were obtained when
reduction in the tensile strength values of at least 40 wt.% of PVB film is added to PA-6.
50% smaller than the ones for the 40 wt.% PVB film (4) The tensile strength and Young’s modulus of
blend, but the improvement in impact strength was the blends obtained using recovered PVB are
not as significant. Hence, the 80/20 and 60/40 com- of the same order of magnitude as the ones
positions were chosen for studying the substitution of the blends obtained using pure PVB films
of original PVB film from recovered PVB film. processed twice; the specimens with original
Figs. 10–12 present a comparison of the tensile PVB film as toughening agent, submitted to
strength, Young’s modulus and notched Izod only one extrusion presented the smallest ten-
impact strength of the blends obtained with original sile strength and modulus.
PVB and with recovered PVB (for both processes (5) The tensile strength of the 80/20 blends sub-
R1 and R2). All those mechanical properties were mitted to one or two extrusions are of the
determined for samples extruded once (1E) and same order of magnitude within experimental
twice (2E). The following observations can be done error. In the particular case of the 60/40 origi-
when analyzing those three figures. nal PVB blend, a large increase of tensile
strength was observed when the blend was
(1) Both recycling processes (industrial R2 or lab processed twice (see Fig. 10). The tensile
scale R1) result in blends with similar mechan- strength increased in about 83% when the
ical properties within experimental error. blend was reprocessed.
1200
1000
1590
800
1289
1279
1239
600
1108
400
200
233
215
202
202
196
104
95
0
PA-6 (1 and 2E) PVB O (1E) PVB O (2E) PVB R2 (1E) PVB R2 (2E) PVB R1 (1E)
Fig. 12. Notched Izod impact strength of the blends with original and recovered PVB film as impact modifier. 1E = material extruded
once; 2E = material extruded twice; R1 = recovered film using lab-scale grinder; R2 = recovered film using an industrial grinder;
O = original film.
T.S. Valera, N.R. Demarquette / European Polymer Journal 44 (2008) 755–768 767
1450
PA-6/PVB film (60/40)
conditioned to the quantification of the loss of plas-
1250
ticizer undergone during the windshield recycling
1050
process and blend preparation since the amount of
850 plasticizer controls the viscosity ratio of the dis-
650
persed and matrix phases, which in turns controls
the morphology of the blends and their properties.
450
The morphological observations showed that if the
250 interparticle distance is smaller than around
50 0.2 lm (critical value), the notched Izod impact
0 5 10 15 20 25 30
strength values increase considerably. Conse-
Plasticizer content (wt.%)
quently, the fracture surface of these blends exhib-
Fig. 13. Notched Izod impact strength of the blends as a function ited characteristics of tough failure.
of plasticizer content. 1E = material extruded once; 2E = mate-
rial extruded twice; R1 = recovered film using lab-scale grinder;
R2 = recovered film using an industrial grinder; O = original
Acknowledgments
film.
The authors would like to thank FAPESP,
CAPES and CNPq for financial support. Saint-
(6) When comparing the 80/20 and 60/40 blends it Gobain Sekurit, Celanese Chemical Europe and
can be seen, as expected, that the tensile Solutia do Brasil for providing the materials used
strength and Young’s modulus of the 80/20 in this study.
blends (for every kind of PVB film used) are
larger than the ones of 60/40 blends. An oppo-
site trend is observed for the notched impact References
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