THE EFFECT OF PHTHALOCYANINE PIGMENT ON THE MICROSTRUCTURAL AND MECHANICAL PERFORMANCE OF PROPYLENE- ETHYLENE BLOCK COPOLYMER

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1 THE EFFECT OF PHTHALOCYANINE PIGMENT ON THE MICROSTRUCTURAL AND MECHANICAL PERFORMANCE OF PROPYLENE- ETHYLENE BLOCK COPOLYMER Major, I.F.M and McNally, G.M. Polymer Processing Research Centre, Queen s University Belfast, Ashby Building, Stranmillis Road, Belfast, BT9 5AH, N. Ireland Abstract Injection moulded samples of a commercial propylene-ethylene block copolymer containing % - 8% phthalocyanine blue pigment were prepared using a range of mould temperatures (4ºC - 8ºC). Mechanical and thermal analysis showed progressive increase in tensile modulus, storage modulus (E ) and glass transition temperature (T g ) with increase in pigment loading. However, impact strength of the pigmented copolymer decreased progressively with increase in pigment loading and mould temperature. Thermal analysis of the samples shows that changes in crystalline melting phase H, and activation energies E a for phase relaxations (DMTA) may account for the overall decrease in impact performance of the pigmented copolymer. Introduction Propylene-ethylene block copolymers are gaining importance because of their improved impact performance and improved clarity over conventional isotactic polypropylene copolymers. Commercial propylene-ethylene block copolymer is formed by the addition of ethylene monomer to isotactic homopolymer polypropylene or propylene-ethylene random copolymer. The comonomer levels in block copolymers range from 5-25% and the composition of propylene-ethylene block copolymer is considered in reality to be more complicated than the long chains of homopolymer followed by long chains of comonomer structure suggested by the theory.(1) It has been shown that propylene-ethylene block copolymer is made up of a wide variety of molecular species: ranging from crystallizable oligimers of polypropylene and polypropylene, propylene-ethylene block copolymer to amorphous ethylene-propylene rubbers (EPR).(2) Some commercial propylene-ethylene block copolymer have been shown to contain only 28% block copolymer with the rest being composed of 52% polypropylene homopolymer, 15% EPR and 5% random copolymer.(2) DMTA analysis has also shown the presence of an EPR phase in the propylene-ethylene block copolymer and this acts as a discrete phase which is present in a twophase system that also comprises a continuous polypropylene homopolymer matrix.(3) It is the presence of this EPR phase that gives the propylene-ethylene block copolymer its exceptional impact properties. The ethylene comonomer, which is added to the polypropylene monomer to form the propylene-ethylene block copolymer, provides a regularly distributed amorphous elastomeric phase throughout the polypropylene crystalline matrix. This elastomeric phase adds impact resistance by absorbing energy causing local deformation instead of allowing crack propagation in the material. (1&2) The ethylene comonomers have been shown to lead to the formation of γ crystal modification, with the amount increasing with ethylene content. (2-4) The formation of the γ crystal modification is due to the disruption of the isotactic polypropylene homopolymer chain by the ethylene comonomer. It has been suggested that the ethylene chain sequences within the propylene-ethylene block copolymer may be long enough to crystallise. (2) Kinetically the α crystal modification is favoured by isotactic polypropylene homopolymer, but this is less true with increasing ethylene comonomer content. (4) However, it has been shown that there is very little difference in the crystallisation behaviour of isotactic polypropylene homopolymer and propylene-ethylene block copolymer with similar melting points (T m1 ), solidification temperatures (T c ), and H m values. (5) Nucleating agents, such as phthalocyanine blue pigment, have been shown to cause part shrinkage and changes to morphology in polypropylene, which affect mechanical, and thermal properties (6). These nucleating agents also initiate γ crystal modification. They also tend to enhance the amount of γ crystal modification formed due to the presence of ethylene in propylene-ethylene block copolymers, this is due to crystallisation being able to take place at higher temperatures. (2) The objective of this work is to investigate the effect of phthalocyanine blue pigment on the structure and mechanical performance of propylene-ethylene block copolymer, injection moulded at three different mould temperatures. Experimental (a) Materials - The polymer used in this investigation was a commercial propylene-ethylene block copolymer with an MFI of 7g/1min. The pigment used was a phthalocyanine based blue supplied in masterbatch (25% 68 / ANTEC 23

2 w/w) form. The pigment was tumble mixed with the polypropylene in various portions prior to injection moulding. The range of pigment/polymer blends comprised pigment masterbatch concentrations of %, 2%, 4%, 6% & 8%. (b) Preparation of Samples - Impact and tensile specimens were manufactured from the pigmented block copolymer using an Arburg 32S Allrounder 5-35 injection molding machine with a clamping force of 5kN (5 tons). This machine had a general-purpose screw of diameter 45mm and L/D ratio of 18. The barrel temperature profile from the feed section to the nozzle was maintained at 195 C, 215 C, 22 C, 225 o C and 23 C during the manufacture of the various samples. A test mould manufactured from tool steel with both a tensile and impact impression, was used to manufacture the samples. The samples were produced using mould cooling temperatures of 4 C, 6 C and 8 C. (c) Tensile Analysis - The tensile properties of the various pigmented samples were tested according to ASTM These tests were performed using an Instron 4411 Universal Tester with a load cell of 5kN and a constant crosshead speed of 5mm/min. The tensile modulus, break strength and elongation at break were recorded and averaged for at least 1 specimens. (d) Impact Analysis - The impact performance of the samples was determined using a CEAST automatic fractovis free falling dart impact tester, fitted with a data acquisition system. The peak force (N), peak energy (J), total energy (J) and impact strength (J/mm) was also recorded. (e) Crystallinity - The effect of mould cooling and increasing pigment loading on the crystallinity of the various injection moulded samples was investigated using a Perkin Elmer DSC 6 Modular Thermal Analyzer. A 5-1mg representative sample of each specimen was heated over a temperature range of 4 C to 23 C at 1 C/min. The enthalpy ( H m1 ) values and the melting temperature (T m1 ) was recorded for each of the samples. Controlled cooling studies were also performed in situ using the DSC at cooling rates of 1, 2 and 3 C/min and the solidification temperatures (T c ) and heat of solidification ( H c ) were recorded for all the samples. These samples were then reheated at 1 C/min in order to determine the effect of cooling rate and pigment concentration on the crystallinity developed. (f) DMTA Analysis - Dynamic mechanical thermal analysis of the samples was performed using a Polymer Lab MARK II dynamic mechanical thermal analyser. The samples of dimensions 46x13x3 mm were mounted in the DMTA in the dual cantilever mode. The samples were scanned over the temperature range 6 C to 6 C at a scan rate of 2 C per minute and at frequencies of.3, 1, 3, 1 and 3Hz. Results and Discussion Tensile Analysis - The effect of increasing pigment loading and mould temperature on the tensile properties of propylene-ethylene block copolymer are shown in Figs 1-3. The results in Fig 1 show a significant increase in tensile modulus with a progressive increase in pigment loading. Increasing mould temperature had little affect on tensile modulus. The results in Fig 2 show only a small increase in break strength with increase in pigment loading and increase mould temperature. The results in Fig 3 shows a decrease in elongation with increase in pigment loading and mould temperature with the lowest elongations being recorded for 8% pigment loading at 8ºC mould temperature. In general, increasing mould temperature has limited affect on the tensile properties of propylene-ethylene block copolymer. Impact Properties - The effects of increasing pigment loading and mould temperature on the impact strength of the various samples are shown in Fig 4. These results show that the impact strength of propyleneethylene block copolymer decreased progressively with increase in pigment loading. The results also show that there was only a slight decrease in impact strength with increasing mould temperature for all the samples. The results in Fig 5 show that the cold impact strength of propylene-ethylene block copolymers decreased more rapidly with progressive pigment loading than at room temperature. The drop in impact strength was approximately 5J/mm for each 2% increase in pigment loading. Crystallinity DSC analysis was performed on all the samples in order to determine the effect of pigment loading and mould temperature on the overall crystallinity and crystalline development. Typical melting endotherms in Fig 6 show the effect of mould temperature on the crystallinity of unpigmented and 8% pigmented propylene-ethylene block copolymer. These thermograms show melting endotherms occurring over the temperature range C. There was also a slight reduction in the melting temperature recorded for the samples containing 8% phthalocyanine blue. Very little change in the melting temperature was recorded for increasing mould temperature. The H m1 values for all the samples were recorded and these values are shown in Table 1. These results show an increase in H m1 values for samples with increasing mould temperature. Much lower H m1 values were recorded for the pigmented samples, with further small increases being recorded for progressive increase in pigment loading. The initial decrease in H m1 for the small pigment loadings would tend to indicate that a different crystalline modification had been formed as a result of addition of phthalocyanine blue to this propylene-ethylene block copolymer. In order to investigate this effect in greater detail controlled heating and cooling experiments were performed using the DSC. The various samples were heated to 23 C at 1 C/min. After holding at this ANTEC 23 / 681

3 temperature for three minutes; the samples were cooled at 1, 2 and 3 C/min to 4 C and then reheated to 23 C at 1 C/min. The first heat H m1, the controlled cooling H c and the second heat H m2 are shown in table 2. The solidification temperatures at different cooling rates for all the samples are shown in Fig 7. These results show a significant increase in solidification temperatures of the propylene-ethylene block copolymer by up to 6 deg C on the addition of even small amounts of pigment i.e. 2% pigment loading. Further increase in pigment loading showed only slight increases in solidification temperature, especially at the higher cooling rates. These results confirm the nucleating effect of this pigment on the propylene-ethylene block copolymer. The H values recorded for the controlled heating and cooling experiments are shown in Table 2. Once again the results show a decrease in H m2 for all the pigmented samples. The H m2 values were also shown to decrease with increasing cooling rate over the range 1 C/min to 3 C/min for all the pigmented samples. These results once again indicate the formation of a different crystal modification as a result of the pigment. DMTA - The effect of pigment loading on damping tan δ and storage modulus (E ) is shown in Figs 8&9. These thermograms clearly show a significant shift in phase transition temperatures from 22 C to 55 C with addition of pigment. It has been reported (7) that the dominant relaxation, shown to occur for the unpigmented samples, is generally taken to be the glass transition temperature (T g ) of the amorphous regions associated with isotactic polypropylene homopolymer. The larger tan δ peak occurring at around 5 C, shown for the pigmented sample, has been reported to be associated with the α crystal modification relaxation of isotactic polypropylene homopolymer. Therefore these results would tend to show a significant change in crystal modification had occurred as a result of the pigment. Recently, Feng et al (7) reported on the dynamic mechanical behaviour of polypropylene copolymers and showed the loss modulus (E ) to be related to the impact energy, with higher impact energies values being recorded for copolymers with higher loss modulii (E ). The results in Fig 1 show the effect of pigment loading on the loss modulus of propylene-ethylene block copolymer. These results clearly show a decrease in loss modulus for the pigmented sample. This decrease in E would account for the rapid decrease in impact strength for pigmented propylene-ethylene block copolymer. Conclusion This work investigated on the effect of phthalocyanine blue pigment and mould temperatures on the mechanical properties and crystalline development of an injection moulding grade propylene-ethylene block copolymer. The tensile analysis shows an increase in tensile modulus and break strength with increasing pigment loading. This increase in tensile modulus is normally attributed to an increase in crystallinity. However, much lower crystallinities were recorded for the pigmented samples, even at the lower pigment loadings of 2%. The thermograms showed that there was a slight difference in the melting temperatures of the unpigmented and pigmented samples and much higher solidification temperatures were recorded for the pigmented samples. This would indicate that this pigment had a nucleating effect on the copolymer. DMTA analysis showed large differences in phase transition temperatures with the higher temperature transition (56 C) associated with α crystal modification being predominant in the thermogram for 6% pigmented sample. The loss modulus values were shown to be much lower for the pigmented sample. This decrease in E and predominance of the α crystal modification, would account for the rapid decrease in impact strength for pigmented propylene-ethylene block copolymer and confirms earlier work by Feng et al. (7) Since the EPR phase in the propylene-ethylene block copolymer provides impact resistance, it can be said that increasing pigment loading and mould temperature, interferes in the ability of EPR to effectively absorb energy. Therefore instead of local deformation occurring, which reduces impact failure, cracks propagate in the material, causing fracture. DMTA analysis has shown a significant reduction in the EPR phase formation (tan δ -2 C) and this has resulted in the much lower impact performance of the pigmented samples. References 1. Polypropylene - The Definitive User's Guide and Databook 1998 Morphology and Commercial Forms, Plastics Design Library, pp Y. Feng, et al, The Measurement of Compositional Heterogeneity in a Propylene Ethylene Block Copolymer Polymer, Vol. 39 (1998) pp Y. Feng, et al, Crystalline Structure of Propylene- Ethylene Copolymer Fractions, Journal of Applied Polymer Science Vol. 68 (1998), pp T. Foresta, et al, Competition between α and γ phases in isotactic polypropylene: effects of ethylene content and nucleating agents at different cooling rates, Polymer 42 (21), pp Cheng-Fang Ou, The Crystallization Characteristics of Polypropylene and Low Ethylene Content Polypropylene Copolymer with Copolyesters, European Polymer Journal Vol. 38 (22), pp P.R. Hanna, et al, The Effect of Pigment Type and Concentration on the Mechanical and Thermal Properties of Injection Molded Polypropylene, SPE, ANTEC 21, pp Y. Feng, et al, Dynamic Mechanical Behavior Analysis for Low Ethylene Content Polypropylene Copolymers, Journal of Applied Polymer Science Vol. 68 (1998), pp / ANTEC 23

4 8 % 2% 4% 6% 8% 4 % 2% 4% 6% 8% 4 % 2% 4% 6% 8% Tensile Modulus (MPa) Break Strength (MPa) Elongation (%) Fig 1 - The effect of mould the tensile modulus Fig 2 - The effect of mould the break strength Fig 3 - The effect of mould the % elongation 25 % 2% block 4% COPP6% 8% 2 % 2% 4% 6% 8% Impact Strength (J/mm) Impact Strength (J/mm) Fig 4 - The effect of mould the impact strength Fig 5 - The effect of mould the impact strength at -4ºC 13 Solidification Temperature (C) cooling rate 1 C/min cooling rate 2 C/min cooling rate 3 C/min % 2% 4% 6% 8% Pigment Loading Fig 7 - The effect of pigment loading and cooling rate on solidification temperature Fig 6 - The effect of mould temperature on DSC thermograms of unpigmented and 8% pigmented propylene-ethylene block copolymer ANTEC 23 / 683

5 9 Log E' (N-.75) (MPa) 5 Log E' (N-.75) Tan Tan Delta Fig 8 DMTA thermogram of unpigmented propyleneethylene block copolymer Log E' (N-.75) (MPa) 5 Log E' (N-.75) Tan δ Tan Delta.16 Fig 7 - The effect of pigment on DSC thermograms of unpigmented and 8% pigmented propylene-ethylene block copolymer Enthalpy (J/g) Pigment 4 C 6 C 8 C loading H H H % % % % % Table 1 - The effect of pigment loading and mould temperature on DSC H values Log E" (MPa) Fig 9 - DMTA thermogram of 6% pigmented propyleneethylene block copolymer % 6% Fig 1 - The effect of pigment on the loss modulus (E ).11 1 C/min 2 C/min 3 C/min pigment H (J/g) H (J/g) H (J/g) loading m1 m2 c m1 m2 c m1 m2 c % % % % % Table 2 - The effect of pigment loading and cooling rate on DSC H values for first heat enthalpy (m1), second heat enthalpy (m2) and solidification enthalpy (c). 684 / ANTEC 23

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