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The Effect of Compatibilisation for Blends of Nylon 6 or Polybutylene Terephthalate (PBT) with Metallocene Linear Low-Density Polyethylenes.

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Dev. Chem. Eng. Mineral Process. 12(1/2), pp. 77-90, 2004.
The Effect of Compatibilisation for Blends
of Nylon 6 or Polybutylene Terephthalate
(PBT) with Metallocene Linear Low-Density
Polyethylenes
F. Gribben, G.M. McNally, A.H. Clarke, W.R. Murphy
and T. McNally
Polymer Processing Research Centre, Queen 's University of Belfast,
Stranmillis Road, Beljast BT9 5AH, Northern Ireland, UK
Polymer blends of polyamides and polyethylenes are immiscible and highly
incompatible. These blends are characterised by high interfacial tension, a two-phase
morphology and poor physical characteristics due to reduced interaction across the
phase boundaries. PBT like many other polymers is a brittle material with a high
modulus value and is not suitable for certain applications. Blending and
compatibilising with an incompatible polyethylene phase may improve these
properties. The compatibilising agent, maleic anhydride-grafted-LLDPE, is
physically miscible with the polyethylene phase and has a chemical functionality with
the polyamide phase and the carboxylic and hydroxyl end groups of the PBTphase.
The use of a new generation mLLDPE (ENGAGE TM by Dupont) was also studied to
investigate its suitability as a modifier for the polyamide and polyester grades. The
influence of the percentage composition of the mLLDPE and the efect of the addition
of the compatibiliser were both investigated for their effect on the mechanical
properties. They were both shown to significantly improve the modulus and
elongation with only a slight reduction in the impact properties of the final product.
77
F. Gribben, G.M.McNaIly, A.H. Clarke, K R . Murphy and T. McNuI&
Introduction
Due to their superior mechanical performance, low wear, abrasion properties and
excellent chemical resistance, nylons are one of the most attractive classes of
thermoplastics and are used in a wide variety of engineering applications. The
disadvantages associated with the use of nylons are high moisture absorption, acid
intolerance, poor dimensional stability and brittleness. In order to overcome some of
these disadvantages, modification of the performance of the nylons may be achieved
by blending with suitably low modulus materials. Recently, there have been several
reports on the development of toughened nylons by blending with materials such as
natural rubbers or synthetic alternatives such as EPR-g-MA (maleated ethylene
propylene rubber) or EPDM-g-MA (maleated ethylene propylene diene rubber) [11.
Polybutylene terephthalate (PBT) is now being widely used as an engineering
polymer due to its high tensile and impact performance and excellent dimensional
stability, particularly in contact with water, coupled with its high rigidity and good
impact strength, even at low temperatures. Thermoplastic elastomers based on PBT
are now finding uses in automotive interior applications and have also become widely
accepted as engineering elastomers in applications such as seals, hosing and beltings.
These elastomeric properties have been imparted to PBT by blending the polymer
with modified rubbers such as EPR and EPDM [I] and ethylene rubbers [2]. The
carboxylic or hydroxyl end groups of the PBT react with the modified rubbers to
produce a grafted molecule that compatibilises the blend.
The use of polyolefins as an alternative to these hctionalised rubbers has been
limited because of the polar nature of the PBT and non-polar nature of the polyolefm,
which inhibits miscibility. A more recent alternative to these additives is an ethyleneoctene copolymer (EOC) based elastomer, tradename of ENGAGE. These materials
have been developed by DupontDow from elastomers using metallocene
polymerization catalysts. Results from recent work using these materials as impact
modifiers and tougheners for brittle materials such as polypropylene have shown
improvements in impact performance similar to blends of PPEPDM [2, 31. However,
unlike conventional elastomers, these pelletised copoIymers typically exhibit faster
mixing, better handling and better dispersion during extrusion blending due to their
pelletised form.
Recent studies have also shown that blending a maleated derivative of EOC with
nylon 6 gave a significant increase in notched izod impact strength [4,51. However,
there has been little work published to suggest that unmodified EOC has been used as
an impact modifier for nylon 6. Recent studies have also shown that a substantial
increase in notched izod impact strength of PBT had been achieved by blending with
a maleated derivative of EOC [ 5 ] . This increase in toughness was attributed to a
reduction in particle size caused by the increased EOC and graft content in the blend.
A major challenge in blending these materials with polyolefins has been the
difference in polarity of the polar nylon 6 or PBT and the non-polar polyolefin [ 6 ] .
To overcome this problem, a compatibilisation method for the system was
required. There are many alternatives to maleated derivatives that enable
compatibilisation of such polymer blends, including chemical hnctionalisation or the
introduction of an additional component with a similar chemical structure to both
components. Usually this is a block or graft copolymer. For th~sstudy a maIeic
78
Compatibilisationfor Blends of Nylon 6 or PBT with Metallocene LLDPEs
anhydride-grafted-LLDPE was used. This compatibiliser should be physically
miscible with the PE phase, and have a chemical functionality with the polyamide and
the carboxylic or hydroxyl groups of the PBT. The aim of t h s work was to investigate
the influence of blend composition and the addition of a compatibiliser on the
mechanical properties and phase morphology of nylon 6/EOC and PBT/EOC blends.
Experimental Details
(a) Materials. The materials used in this investigation were nylon 6 (N6), Grilon
R47HW, supplied by EMS Chemie; polybutylene terephthalate (PBT), Grilpet
B24HNZ, from EMS-Chemie; and ethylene-octene copolymer (EOC), ENGAGE
8150, supplied by Dupont-Dow Elastomers. The compatibilser used in this work was
a linear low-density polyethylene-grafted-maleic anhydride (LLDPE-g-MAH)
copolymer, Polybond 3 109, supplied by Uniroyal Chemicals.
(6) Compounding. All the materials were supplied in pellet form and dried according
to the manufacturers specifications prior to compounding. A range of samples of
nylon 6 blended with ethylene-octene copolymer (EOC) were prepared, with a
composition range of 0, 5, 10, 25, 50, 75 and lOOwt% EOC. Another set of samples
was prepared which included an additional 5% of the LLDPE-g-MAH compatibiliser.
Similar blends were also made using PBT as the base material. The compounding
extrusion was carried out using a 38 mm Davis Standard Killion extruder fitted with a
barrier screw. The compounding temperatures were 225°C at the feed section to
240°C at the adapter and die, for both the nylon 6 and PBT systems. The samples
were dned and stored for injection moulding.
(c) Injection Moulding. Tensile, flexural and impact test specimens were produced
using a 50 tonne Arburg 320s Allrounder 500-350 injection molding machme with a
general purpose screw. All the samples were conditioned at ambient conditions for a
minimum of 48 hours prior to testing. An average of 10 samples was used for all of
the following test procedures.
(d) Mechanical Anabsis. The tensile and flexural property analysis was performed
using an Instron 41 1 Universal tensile tester, fitted with a 5 kN load cell. The tensile
tests were carried out according to ASTM D638M standard, using a cross-head speed
of 200 d m i n . The flexural tests were carried out according to ASTM 690M, using
a cross-head speed of 5.1 mrdmin.
(e) Diflerential Scanning Calorimety (DSC). Crystallinity of the samples was
determined using a Perkin Elmer DSC 6 Modular Thermal Analyser with liquid
nitrogen attachment for sub-ambient temperatures. A 5-10 mg sample was heated
over a temperature range from -50°C to +275"C at 10"C/min. The crystallinity was
determined from the latent heat of fusion (AH) values of the melt endothem, and
using the AH values of 190 J/g for 100% crystalline nylon 6 [lo] and 142 J/g for
100% crystalline PBT [ 111.
79
F. Gribben, G.M. McNally, A.H. Clarke, K R . Murphy and T. McNally
v ) Impact Analysis. The impact properties of the samples were determined using a
CEAST Falling Weight Instrumented Impact Tester, with data acquisition system,
using an impact height of 1 meter and a mass of 28.3 kg. The software recorded the
peak energy required to fracture the samples.
(g) Dynamic Mechanical Thermal Analysis (DMTA). Changes in viscoelastic
characteristics of the materials, i.e. glass transition temperature (T& and storage
modulus (E'), were measured using DMTA (Polymer Laboratories Mark 11).
Specimens of dimensions 34 x 13 x 3 mm for DMTA analysis were cut fiom the
tensile test specimens, and the analysis was carried out in dual cantilever mode over
the temperature range from -60°C to +60°C, using a frequency of 1 Hz. Glass
transition temperatures (TJ were recorded as being the temperature at which the
Tan 6 maximum occurred.
(I) Phase Morphology. The structural morphology of the blends was investigated
using a Joel Scanning Electron Microscope (SEM). The samples were cryogenically
fractured in liquid nitrogen and etched with n-heptane at 5OoC to remove the EOC
phase. They were finally splutter coated with gold prior to SEM analysis.
Results and Discussion
(I) Mechanical Anulysis, The effect of EOC and compatibiliser on the tensile
strength is shown in Figures land 2. The results for the nylon blends in Figure 1 gave
an overall decrease in tensile strength with increasing EOC content, except for the
blends containing 10% EOC content which had a slight increase in tensile strength.
In general, those blends with compatibiliser had increased strength over the
uncompatibilised blends. The effect of EOC and compatibiliser on the tensile strength
for the PBT blends is shown in Figure 2. There was an overall decrease in tensile
strength with increasing EOC content, except for the blends containing 5% and 10%
EOC content which showed a slight increase in tensile strength. In general, those
blends with compatibiliser had a slight increase in tensile strength over the
uncompatibilised blends.
1;
t 40
1
15
0
(a)
5
10
u
K EOC
50
1s
iw
0
(b)
5
10
25
50
75
100
Y Ern
Figure 1. The effect of EOC content on the tensile strength of compatibilised and
uncompatibilised (a) nylon 6/EOC blends and (b) PBT/EOC blends.
80
Compatibilisationfor Blends of Nylon 6 or PBT with Metallocene LLDPEs
25
10
I
0
60
I5
1W
K EOC
fa)
10
5
0
23
K EOC
6)
75
50
1w
Figure 2. The effect of EOC content on the % elongation of compatibilised and
uncompatibilised (a) nylon 61EOC blends and (b) PBT/ EOC blends.
The results in Figure 2 show the effect of EOC and compatibiliser on the
elongation of the various samples of the nylon and PBT blends. The nylon blends
showed an elongation increase for up to 10% EOC content, and then a reduction in
elongation up to 50% EOC content, with another increase in values for the hrgher
percentage EOC blends. These results may suggest that there is an optimum EOC
content for these blends between 10-25%. There was evidence that the compatibiliser
had brought some stability to the system as the pattern was again apparent for the
compatibilised blends but to a lesser extent. The increase in elongation for the higher
% EOC content may be explained by a change in phase morphology of the blends as
the EOC became the dominant phase and the properties of the blends became more
like the pure elastomer.
The results for the PBT blends had an overall increase in elongation with
increasing EOC content, with a substantial increase in elongation for those blends
containing more than 25% EOC. This elongation increase for the hrgher EOC content
may also be due to changes in phase morphology of the blends as the EOC became
the more dominant phase, and the properties of the blends tend towards those of EOC.
Figures 3 and 4 show a decrease in tensile and flexural moduli with increasing
EOC content for both the nylon and PBT blends. This was expected for incorporation
of a low modulus component into a blend with a stiff matrix material such as nylon or
PBT.
0
fa)
6
10
23
K EM:
50
75
1w
"
fb)
.
.
0
5
.
10
.
26
K EOC
.
5a
75
1cQ
Figure 3. The effect of EOC content on the (a) tensile modulus and (b) flexural
modulus of compatibilised and uncompatibilised nylon 6/EOC blends.
81
F, Gribben. G.M. McNally. A.H. Clarke, W.R. Murphy and T. McNally
Figure 4. The efect of EOC content on the (a) tensile modulus and (b) flexural
modulus of compatibilised and uncompatibilised PBT/ EOC blends.
(ii) Difserential Scanning Calorimetry (DSC). Figures 5 and 6 present the DSC
thermograms for the uncompatibilised and compatibilised blends of various nylon 6
and PBT blends. The two discernable peaks recorded on Figure 5 show that nylon 6
and EOC are immiscible when blended together. The same occurred with PBT and
EOC as shown by the separate peaks in Figure 6. The thermograms in Figure 5
possessed two broad melting endotherms recorded over the temperature ranges of
180°C to 220°C and 30°C to 70°C, these represent the melting endothem of nylon 6
and EOC respectively. A narrow melting peak at 212°C for the nylon 6 and a broad
melting peak at 45°C for the EOC are also clearly shown in the thennograms. The
thermograms in Figure 6 have two broad melting endotherms recorded over the
temperature ranges of 210°C to 240°C and 30°C to 70°C, these represent the melting
endotherms of PBT and EOC respectively. The themograms clearly show a sharp
melting peak at 223°C for the PBT and a broad melting peak at 45°C for the EOC.
The latent heats of fusion (AH) for the nylon and PBT phases were calculated by
measuring the AH of the material melting endotherm, and then adjusting these values
b)
160
60
T.mp.r.l"r.
260
('CI
Figure 5. DSC thermograms for (a) uncornpatibilised and (b) compatibilised nylon
6/EOC blends.
82
Compatibilisationfor Blends of Nylon 6 or PBT with Metallocene LLDPEs
.
0
a)
SO
150
200
T r m p a r a l u r r ('C)
100
250
0
(bl
50
.
.
200
T a m p r r a l u r r ('C )
I00
150
.
250
Figure 6. DSC thermograms for (a) uncompatibilised and (b) compatibilised PBT/
EOC blends.
according to the weight fraction of the material in the blend. The crystallinities were
then calculated using the theoretical latent heat of fusion for 100% crystalline nylon
(190 J/g, [lo]) and the latent heat of fusion for 100% crystalline PBT (142 J/g, [ 111).
The effect of increasing EOC content on nylon crystallinity is given in Figure 7a.
There was very little change in the overall crystallinity with EOC content increasing
up to 25% for the uncompatibilised blends. The compatibilised blends had a
progressive decrease in crystallinity from 28% to 15% with increasing EOC content
from 0% to 25%, and an increase in crystallinity (20%) being recorded for 50% and
75% EOC blends. Further increase in EOC content to 50% in the uncompatibilised
blends showed a decrease in crystallinity to approximately 18%. There was very little
change in the crystallinity at higher EOC contents for both the compatibilised and the
uncompatibilised blends. The change in crystallinity with EOC content and
compatibilisation may account for the changes in the mechanical performance of
these blends, with lower moduli and higher elongations being recorded for the blends
with lower crystallinity.
The effect of increasing EOC content on crystallinity is presented in Figure 7b.
There was a general decrease in crystallinity with increasing EOC content for the
uncompatibilised and compatibilised blends. The uncompatibilised blends showed a
progressive decrease in crystallinity from 21% to 13% with an increasing EOC
content, and an increase in crystallinity (17.5%) being recorded for the 50% EOC
blend. The compatibilised blends had a progressive decrease in crystallinity from
21% to 15% with increasing EOC content and an increase in crystallinity (18%) being
recorded for the 10% EOC blend. The change in crystallinity with EOC content and
compatibilisation may again account for the changes in the mechanical performance
of these blends, with lower moduli and hgher elongations being recorded for the
blends with lower crystallinity.
83
F. Gribben, G.M. McNally, A.H. Clarke, W.R. Murphy and T. McNally
Figure 7. The efect of EOC content on (a) nylon 6 crystallinity in nylon 6/EOC
blends and (b) PBT clystallinity in PBT/EOC blends.
(iii) Impact Strength. The effect of EOC content and compatibilisation on the
impact strength of nylon 6/EOC and PBT/EOC blends is presented in Figure 8. There
was a progressive decrease in impact strength with increasing EOC content for both
the compatibilised and uncompatibilised nylon blends. The results also show a
significant reduction in impact strength for the compatibilised blends for the EOC
content range of 5% to 25%. The PBT blends exhibited a progressive decrease in
impact strength with increasing EOC content for both the compatibilised and
uncompatibilised blends, with a slight increase in values for the blends with EOC
content range of 10% to 25%. There was a significant reduction in impact strength
for the blends over the EOC content range of 25% to 50%.
Figure 8. The effect of EOC content on the impact strength of uncompatibilised and
compatibilised (a) nylon 6/EOC blends and (3) PBT/EOC blends.
Dynamic Mechanical Thermal Analysis (DMTA). The thermogram in Figure
9 shows the effect of EOC content on the phase transitions of uncompatibilised nylon
6EOC blends. There were two distinct peaks, which were typically associated with
the phase transitions in nylon 6 and EOC. The thermogram also had a gradual
(iv)
84
Compatibilisationfor Blends of Nylon 6 or PBT with Metallocene LLDPEs
decrease in the phase transition temperature (Tg) for all the blends, except for the
blend containing 50% EOC which showed an increase in Tg. Although not presented
here, a similar trend was recorded for compatibilised blends with the increase being
recorded for the 25% EOC blend. Ths suggests that the blend with a higher EOC
content was slightly more miscible. The increase in Tg at 50% may explain the
change in mechanical properties experienced at this EOC content.
I
I
I
0
Temperature ('C)
60
-60
Figure 9. DMTA thermograms for uncompatibilised nylonb/EOC blends of various
EOC compositions.
100%
/
75%
25%
0
E
$
1on
I
--
I
0
60
Temperature('C)
120
Figure 10. DMTA thermograms for compatibilised PBT/EOC blends of various EOC
compositions.
85
F.Gribben, G.M. McNally, A.H. Clarke, W.R. Murphy and T.McNally
50% EOC (Comp)
50% EOC (Uncomp)
z
-
. - Uncompatlblllaad
ComprUbllaad
(440
60
0
Tampmtun (‘CI
40
0
(b)
120
60
Tarnp.ratun (‘C)
Figure 11. The effect of compatibilisation on tan 6for (a) 50/.50 w/w nylon6/EOC
blends and (b) 50/50 w/w PBT/ EOC blends.
The thermogram in Figure 10 demonstarte the effect of EOC content on the phase
transitions of compatibilised PBTEOC blends. There are two distinct peaks, whch
were typically associated with the phase transitions in PBT and EOC. There was a
gradual decrease in the phase transition temperature (Tg) for all the blends. Although
not shown here, a similar trend was recorded for uncompatibilised blends. This
suggests that the blends with higher EOC content are slightly more miscible.
Figure 11 presents the effect of incorporation of a compatibiliser on the phase
transition temperature of 50/50 nylon 6/EOC blends. The results for the nylon show
that the blends were not completely miscible as indicated by two distinct peaks,
however the lower transition temperature recorded for the compatibilised blend would
tend to indicate better phase miscibility. The results for the PBT show that the blends
were again not completely miscible as there were two distinct peaks. However, the
shift to lower Tg values recorded for the 50% EOC blend would again tend to indicate
better phase miscibility. The results also highlight that there was no significant change
in peak temperature for the uncompatibilised and compatibilised blends. This suggests
that the compatibilisation strategy used has not been beneficiai to this system.
Table 1. The effect of EOCcontent on the storage modulus (Log E 7 at 25°C of
(a) nylon 6/EOC blends and (b) PBT/EOC blends.
0
5
10
25
50
75
loo
86
8.68
8.8
8.59
8.79
8.5
7.52
7.8
8.88
8.6
8.32
8.46
7.85
7.98
7.81
0
5
10
25
50
75
loo
9.01
8.89
8.71
8.61
8.19
7.19
7.8
9.01
8.74
8.59
8.64
8.15
7.74
78
Coinpatibilisationfor Blends of Nylon 6 or PBT with Metallocene LLDPEs
Table 1 shows the effect of EOC content on the storage modulus (E’) of the
various blends. The results for both the nylon and PBT exhibit a general decrease in
E’ with increasing EOC content for both the uncompatibilised and compatibilised
blends, except for a slight increase in E’ for the 25% blends. The nylon blends also
had lower E’ values, being recorded for the compatibilised blends. These changes in
recorded storage modulus with EOC content confirm the overall changes in
mechanical performance with EOC content discussed earlier. The results for the PBT
blends showed similar E’ values being recorded for the compatibilised and
uncompatibilised blends. These changes in recorded storage modulus with EOC
content confirm the overall changes in mechanical performance with EOC content
discussed earlier.
(v) SEM. SEM analysis of various samples was performed in order to investigate
the effect of EOC content and compatibiliser on the phase morphology of nylon
6/EOC and PBTEOC blends. Figures 12 and 13 illustrate the effect of increasing
EOC content on the blend structural morphology. Photomicrographs illustrate the
distribution of the EOC phase (etched with n-heptane) within the nylon phase in
Figure 12 and the PBT phase in Figure 13. The increases in EOC content up to 25%
resulted in a greater EOC particle size dispersed within the blend. Further increases in
EOC content resulted in the morphology changing from one phase being dispersed in
another, to a two-phase interpenetrating network microstructure. This change in
morphology occurring above 25% EOC content may account for the change in
mechanical properties.
The photomicrographs shown in Figures 14 and 15 illustrate the effect of
compatibiliser and increased EOC content on the phase morphology of these blends.
The results for the nylon blends in Figure 14 show reduced particle size and increased
particle distribution for these blends, which may explain the change in properties and
change in mechanical performance of these blends. The photomicrographs of the
PBT/EOC in Figure 15 show no reduction in particle size and little change in particle
distribution for these blends, c o n f i i n g that the compatibiliser had little effect upon
the mechanical performance of these blends.
The effect of % EOC content on domain shape and size for
uncompatibilised nylon 6/EOC blends: (a) 10% EOC, (b) 25% EOC and (c) 50%
EOC (magnification x 3500).
Figure 12.
87
F. Gribben, G.M. McNally, A.H. Clarke, K R . Murphy and
T. McNalh
Figure 13. The effect of % EOC content on domain shape and size for
uncompatibilised PBT/EOC blends: (a) 5% EOC, (b) 10% EOC, (c) 25% EOC and
(d) 50% EOC (magnification x 3500).
Figure 14. The effect of the addition of 5% LLDPE-g-MAH on domain shape and
size of the dispersed EOC phase in various nylon 6/EOC blends: (a) 10% EOC,
(b) 25% EOC and (c) 50% EOC (magnification x 3500).
Figure 15. The effect of the addition of 5% LLDPE-g-MAH on domain shape and
size of the dispersed EOCphase in various PBT/EOC blends: (a) 5% EOC, (b) 10%
EOC, (c) 25% EOC and (d) 50% EOC (magnification x 3500).
88
Compatibilisationfor Blends of Nylon 6 or PBT with Metallocene LLDPEs
Summary and Conclusions
This work investigates the effect of EOC content on the mechanical performance,
crystallinity and phase morphology of nylon 6EOC and PBT/EOC blends. There was
a substantial decrease in tensile strength, tensile and flexural modulus, and impact
strength with increasing EOC content for both uncompatibilised and compatibilised
blends for both materials. DSC analysis highlighted a significant reduction in the
crystallinity of the nylon phase with an increasing EOC content, particularly for the
uncompatibilised blends. Also a significant reduction in the crystallinity of the PBT
phase with an increasing EOC content for both compatibilised and uncompatibilised
blends.
DMTA analysis for the nylon/EOC blends showed changes in the Tg of the
blends, which suggests some degree of miscibility in these blends. The addition of
the compatibiliser also had the effect of increasing the miscibility of those blends.
For the PBT/EOC blends, there was a slight reduction in Tg of the PBT component of
the blends with increasing EOC content, which suggests some degree of miscibility
for this blend at the higher EOC concentrations but the addition of the compatibiliser
had no effect on the phase transitions.
SEM analysis for the nylon/EOC blends showed a well dispersed EOC phase,
with smaller particle sizes being recorded for the compatibilised blends. The blends
with higher EOC content had a two-phase interpenetrating network structure. SEM
analysis for the PBT/EOC blend showed similar changes in the morphology with
increasing EOC content. However, there was no reduction in particle size and little
change in particle distribution with the addition of the compatibiliser for these blends.
These results correspond to the changes in mechanical and dynamic mechanical
properties reported earlier.
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