Composition comprising heterophasic propylene copolymer
11603453 · 2023-03-14
Assignee
Inventors
Cpc classification
C08L2205/14
CHEMISTRY; METALLURGY
C08L23/0815
CHEMISTRY; METALLURGY
C08L2205/035
CHEMISTRY; METALLURGY
C08L23/16
CHEMISTRY; METALLURGY
C08L23/16
CHEMISTRY; METALLURGY
C08L2205/03
CHEMISTRY; METALLURGY
B29C45/0001
PERFORMING OPERATIONS; TRANSPORTING
C08L23/0815
CHEMISTRY; METALLURGY
C08L2205/025
CHEMISTRY; METALLURGY
International classification
B29B7/90
PERFORMING OPERATIONS; TRANSPORTING
Abstract
The invention relates to a composition comprising a heterophasic propylene copolymer (A), glass fibers (B) and an ethylene-α-olefin copolymer (C), wherein the α-olefin is chosen from the group of α-olefins having 3 to 12 carbon atoms. The heterophasic propylene copolymer (A) consists of (a) a propylene-based matrix, consisting of a propylene homopolymer and/or a propylene-α-olefin copolymer consisting of at least 85 wt % of propylene and at most 15 wt % of α-olefin, and (b) a dispersed ethylene-α-olefin copolymer, wherein the heterophasic propylene copolymer has a flexural modulus of less than 1000 MPa, wherein the dispersed ethylene α-olefin copolymer (b) has an average rubber particle size d.sub.50 of at most 1.15 μm as determined by scanning electron microscopy, and wherein the total amount of (b) the dispersed ethylene-α-olefin copolymer in the heterophasic propylene copolymer (A) and the ethylene-α-olefin copolymer (C) is 30 to 60 wt % based on the total composition.
Claims
1. A composition comprising: a heterophasic propylene copolymer (A), 10 to 40 wt % glass fibers (B) based on the total weight of the composition, and 20 to 30 wt % an ethylene-octene copolymer (C) based on the total weight of the composition, wherein the heterophasic propylene copolymer (A) consists of (a) a propylene-based matrix, wherein the propylene-based matrix consists of a propylene homopolymer; and wherein the propylene-based matrix is present in an amount of 55 to 75 wt % based on the total heterophasic propylene copolymer, and (b) a dispersed ethylene-α-olefin copolymer, wherein the dispersed ethylene-α-olefin copolymer is present in an amount of 45 to 25 wt % based on the total heterophasic propylene copolymer, and wherein the sum of the total amount of propylene-based matrix and total amount of the dispersed ethylene-α-olefin copolymer in the heterophasic propylene copolymer is 100 wt % based on the heterophasic propylene copolymer, wherein the heterophasic propylene copolymer (A) consists of one type of heterophasic propylene copolymer wherein the heterophasic propylene copolymer has a flexural modulus of less than 1000 MPa as determined at 23° C. in the parallel direction according to ASTM D790 Procedure B on a sample of 65×12.7×3.2 mm, wherein the dispersed ethylene α-olefin copolymer (b) has an average rubber particle size d.sub.50 of 0.3 to 1.15 μm as determined by scanning electron microscopy, and wherein a total rubber content in the composition is the sum of 1. (b) the dispersed ethylene-α-olefin copolymer in the heterophasic propylene copolymer (A) and 2. the ethylene-a octene copolymer (C) is 30 to 60 wt % based on the total weight of the composition.
2. The composition according to claim 1, wherein the composition has a melt flow index as determined according to ISO1133 at 230° C. and 2.16 kg in the range of 8.0 to 20.0 dg/min.
3. The composition according to claim 1, wherein the composition has a melt flow index as determined according to ISO1133 at 230° C. and 2.16 kg in the range of 8.5 to 20 dg/min, wherein the average rubber particle size of the dispersed ethylene α-olefin copolymer (b) as determined by scanning electron microscopy is at least 0.5 μm to 1.15 μm, wherein (b) the dispersed ethylene-α-olefin copolymer is present in an amount of 28 to 40 wt % based on the heterophasic propylene copolymer (A), wherein the amount of ethylene in (b) the ethylene-α-olefin copolymer in the heterophasic propylene copolymer (A) is in the range of 40 to 55 wt %, based on (b) the ethylene-α-olefin copolymer in the heterophasic propylene copolymer (A).
4. The composition according to claim 1, wherein the heterophasic propylene copolymer (A) is made by I) polymerizing monomers to obtain an intermediate heterophasic propylene copolymer having an intermediate melt flow index, and II) visbreaking said intermediate heterophasic propylene copolymer, to obtain the final heterophasic propylene copolymer (A) having a melt flow index that is higher than the melt flow index of the intermediate heterophasic propylene copolymer.
5. The composition according to claim 4, wherein the final heterophasic propylene copolymer (A) has a melt flow index as determined according to ISO1133 at 230° C. and 2.16 kg in the range of 18 to 60 dg/min.
6. The composition according to claim 3, wherein the heterophasic propylene copolymer (A) is made by I) polymerizing monomers to obtain an intermediate heterophasic propylene copolymer having an intermediate melt flow index, and II) visbreaking said intermediate heterophasic propylene copolymer, during extrusion directly after step I), to obtain the final heterophasic propylene copolymer (A) having a melt flow index that is higher than the melt flow index of the intermediate heterophasic propylene copolymer, wherein the final heterophasic propylene copolymer (A) has a melt flow index as determined according to ISO1133 at 230° C. and 2.16 kg in the range of 20 to 60 dg/min.
7. The composition according to claim 1, wherein (b) the dispersed ethylene-α-olefin copolymer is present in an amount of 28 to 35 wt % based on the heterophasic propylene copolymer (A).
8. The composition according to claim 1, and wherein the amount of ethylene in (b) the ethylene-α-olefin copolymer in the heterophasic propylene copolymer (A) is in the range of 35 to 65 wt %, based on (b) the ethylene-α-olefin copolymer in the heterophasic propylene copolymer (A).
9. The composition according to claim 1, wherein the composition comprises 10 to 30 wt % of the glass fibers (B).
10. The composition according to claim 1, wherein the composition further comprises a silicone particle having the formula (I)
R.sub.xSiO.sub.2-(x/2) (I) wherein x is a positive number greater than or equal to 1, and each R is independently an aliphatic hydrocarbon group, an aromatic hydrocarbon, or an unsaturated group.
11. A process for the preparation of the composition according to claim 1, comprising melt mixing (A), (B), (C) and optional components.
12. An article comprising the composition of claim 1.
13. The article according to claim 12, wherein the article is an injection moulded part.
14. A composition comprising: a heterophasic propylene copolymer (A), 20 to 30 wt % glass fibers (B) based on the total weight of the composition, and 20 to 30 wt % an ethylene-octene copolymer (C) based on the total weight of the composition, 0.5 to 5 wt % of a silicone particle having the formula R.sub.xSiO.sub.2-(x/2), wherein x is a positive number greater than or equal to 1, and each R is independently an aliphatic hydrocarbon group, an aromatic hydrocarbon, or an unsaturated group; 0.1 to 5 wt % of a modified polypropylene; 0.1 to 1 wt % of oleamide and/or erucamide; 0.2 to 5 wt % of a processing aide; wherein the heterophasic propylene copolymer (A) consists of (a) 55 to 75 wt % a propylene-based matrix, wherein the propylene-based matrix consists of a propylene homopolymer; and (b) 25 to 45 wt % of a dispersed ethylene-α-olefin copolymer based on the heterophasic propylene copolymer (A), wherein the amount of ethylene in (b) the ethylene-α-olefin copolymer in the heterophasic propylene copolymer (A) is in the range of 35 to 65 wt %, based on (b) the ethylene-α-olefin copolymer in the heterophasic propylene copolymer (A), and wherein the sum of the total amount of propylene-based matrix and total amount of the dispersed ethylene-α-olefin copolymer in the heterophasic propylene copolymer is 100 wt % based on the heterophasic propylene copolymer, wherein the heterophasic propylene copolymer (A) consists of one type of heterophasic propylene copolymer wherein the heterophasic propylene copolymer has a flexural modulus of less than 1000 MPa as determined at 23° C. in the parallel direction according to ASTM D790 Procedure B on a sample of 65×12.7×3.2 mm, wherein the dispersed ethylene α-olefin copolymer (b) has an average rubber particle size d.sub.50 of 0.5 to 1.15 μm as determined by scanning electron microscopy, and wherein a total rubber content in the composition is the sum of 1. (b) the dispersed ethylene-α-olefin copolymer in the heterophasic propylene copolymer (A) and 2. the ethylene-octene copolymer (C) is 30 to 60 wt % based on the total weight of the composition.
15. The composition of claim 1, wherein the dispersed ethylene α-olefin copolymer (b) has an average rubber particle size d.sub.50 of 0.5 to 1.15 μm as determined by scanning electron microscopy.
Description
EXAMPLES
(1) The volume average size of the rubber particles of the dispersed ethylene α-olefin copolymer, represented by the d.sub.50 parameter, is obtained by digital image analysis of scanning electron micrographs. Scanning electron microscopy (SEM) is performed on injection molded plaques. Samples of the injection molded plaques are trimmed from surface to bulk at −120° C. The trimmed blocks are stained for 24 hours in RuO.sub.4 solution. After staining, sections with a thickness of 70 nm are obtained. The remaining blocks are fixed into a SEM sample holder and coated with a conductive Ir layer. Imaging is done in a FEI Versa 3D FEGSEM at an acceleration voltage of 5 kV. The resulting micrographs are digitally analyzed using Olympus stream software using the assumptions and mathematical relations as described in D. Sahagian, A. Proussevitch: “3D particle size distributions from 2D observations: stereology for natural applications.” Journal of Volcanology and geothermal Research, 84 (1998) 173-196, to characterize the dispersed rubber phase in terms of its d.sub.10, d.sub.50, d.sub.90 and distribution width. Outside the area where the sample shows particles, reference material is present which has a certain color (C.sub.ref). The part for the particles that was taken into account for the measurements was determined by measuring the actual color of the particle pixel (C.sub.particle) and subtracting from this value C.sub.ref. A pixel lies within the particle, when the C.sub.particle is larger than C.sub.ref*1.05. In this way noise which may be present in the reference material is filtered out and not taken into account in determining the particle size. The particle size is the sum of all pixels which have a C.sub.particle>C.sub.ref*1.05.
(2) The melt flow index (MFI) was determined according to the International Organization for Standardization (ISO) test standards ISO 1133 at 230° C. under a load of 2.16 kilogram (kg).
(3) The total rubber content is the sum of the internal rubber (b) in the heterophasic propylene copolymer (A) and the external rubber (C) in wt % based on the total composition.
(4) The ash content was determined according to ISO 3451 measured after 15 minutes (min) at 525° C.
(5) Notched Izod impact parallel measurements were determined at 23° C. according to ISO180/1A and at −20° C. according to ISO180/1A.
(6) The flexural modulus and the flexural strength were determined at 23° C. according to the ASTM D790 Procedure B. ASTM D790 parallel and perpendicular measurements were done on 65×12.7×3.2 mm cut samples.
(7) Tensile properties were measured according to ISO 527/1A at 23° C.
(8) Gloss measurements were determined according to ISO 2813 at 23° C.
(9) Shrinkage measurements were determined according to ISO 294-4 (Apr. 23, 1990). The sample size used was 65×65×3.2 mm with measurements taken 24 h at 23° C. after moulding and after 1 h at 90° C. Parallel shrinkage indicated is parallel to the flow direction, perpendicular is the shrinkage in cross flow direction. Shrinkage was measured on 5 samples and averaged.
(10) Warpage measurements were determined by the ratio of shrinkage in the parallel and perpendicular directions. The tests were performed on samples which were kept at 23° C. at 24 hours before measuring.
(11) Falling dart impact (VEM) at −10° C. after 7 days was determined according to ISO 6603-B2.
(12) Soft-touch performance was determined by a panel of 5 experts in soft touch properties. Specifically, the experts felt the surface of an injection molded plaque of the respective compositions and assigned it a haptic rating + to ++, where a haptic rating of ++ is considered as better performing.
(13) Tiger-stripe performance: Samples of the compositions were injection moulded into two types of ruler-shaped test specimens. Two types of moulds were used, a so-called fan gate mould and a so-called pin-point gate mould. The molten polyolefin composition was extruded through a nozzle having an upper end having a diameter of 4 mm and a lower end having a diameter of 7 mm. The lower end of the nozzle merges with a rectangular channel of the mould.
(14) Along the length of the fan gate mould, the width changes from about 6.5 mm to 30 mm and the thickness changes from about 3 mm to 2 mm. After the fan shaped part, an elongated part follows having a width of 30 mm and a thickness of 3 mm. The rectangular part is about 34 mm in length. The fan shaped part of the mould is about 225 mm in length.
(15) The pin-point gate mould is identical to the fan gate except that the rectangular part comprises a portion having a width of 1.2 mm over a length of about 6 mm.
(16) The melt temperature during the injection moulding is set at 200° C., 230° C., or 260° C., respectively, and the mould is kept at room temperature. Three different screw speeds are used according to the conditions in Table 1.
(17) TABLE-US-00001 TABLE 1 Screw speed Condition injection [mm/s] Flow rate [cm.sup.3/s] Injection time [s] Low speed 20 14.1 2.49-2.51 Medium speed 50 35.3 0.99-1.0 High speed 160 113.1 0.38-0.39
(18) Specimens having a smooth side and a textured side were manufactured. After moulding each of the specimens is visually observed for occurrence of tiger stripes on its textured side. The quality of the surface was evaluated on a scale of 1 to 10, 10 being the best performance, as described in Table 2.
(19) The average tiger stripe rating is defined as the numerical average of the individual tiger stripe ratings for each of the test specimens manufactured at low, medium and high speed, manufactured with the pin-gate and the fan-gate and measured on the smooth and on the textured surface. Hence, the average tiger stripe rating as defined herein is the average of 12 individual tiger stripe measurements.
(20) TABLE-US-00002 TABLE 2 1 very sharp transition between glossy and dull sections visible seen from any angle 2 sharp transitions between glossy and dull sections seen from any angle 3 very visible transitions between glossy and dull sections seen from any angle 4 visible transitions between glossy and dull sections seen from any angle 5 less visible transitions between glossy and dull sections seen from any angle 6 visible transitions between glossy and dull sections seen from a specific angle only 7 less visible transitions between glossy and dull sections seen from a specific angle only 8 no transitions between glossy and dull sections visible and surface appearance inhomogeneous 9 no transitions between glossy and dull sections visible and surface appearance homogeneous 10 no transitions between glossy and dull sections visible and surface is perfect
(21) The materials used in the Examples are described in
(22) TABLE-US-00003 TABLE 3 Component Description PP1 A heterophasic polymer comprising 18.5 wt % of ethylene- propylene copolymer dispersed in a polypropylene homopolymer, wherein the amount of ethylene in the ethylene-propylene copolymer is 53 wt %. MFI of the heterophasic polymer is 33 dg/min measured at 230° C. under a load of 2.16 kg according to ISO 1133. The flexural modulus at 23° C. in the parallel direction is 1530 MPa. The volume average size of the rubber particles, represented by the d.sub.50 parameter, is 1.29 μm. PP2 A heterophasic polymer comprising 24 wt % of ethylene-propylene copolymer dispersed in a polypropylene homopolymer, wherein the amount of ethylene in the ethylene-propylene copolymer is 56.5 wt %. MFI of the heterophasic polymer is 14 dg/min measured at 230° C. under a load of 2.16 kg according to ISO 1133. The flexural modulus at 23° C. in the parallel direction is 1500 MPa. The volume average size of the rubber particles, represented by the d.sub.50 parameter, is 1.23 μm. PP3 A heterophasic polymer comprising 33.5 wt % of ethylene- propylene copolymer dispersed in a polypropylene homopolymer, wherein the amount of ethylene in the ethylene-propylene copolymer is 51.5 wt %. MFI of the heterophasic polymer is 17 dg/min measured at 230° C. under a load of 2.16 kg according to ISO 1133. The flexural modulus at 23° C. in the parallel direction is 735 MPa. The volume average size of the rubber particles, represented by the d.sub.50 parameter, is 1.25 μm. PP4 A heterophasic polymer comprising 30.1 wt % of ethylene- propylene copolymer dispersed in a polypropylene homopolymer, wherein the amount of ethylene in the ethylene-propylene copolymer is 43.9 wt %. MFI of the final heterophasic polymer is 20.5 dg/min measured at 230° C. under a load of 2.16 kg according to ISO 1133. The flexural modulus at 23° C. in the parallel direction is 786 MPa. The volume average size of the rubber particles, represented by the d.sub.50 parameter, is 1.12 μm. PP5 A heterophasic polymer comprising 30.1 wt % of ethylene- propylene copolymer dispersed in a polypropylene homopolymer, wherein the amount of ethylene in the ethylene-propylene copolymer is 43.9 wt %. MFI of the final heterophasic polymer is 41.2 dg/min measured at 230° C. under a load of 2.16 kg according to ISO 1133. The flexural modulus at 23° C. in the parallel direction is 743 MPa. The volume average size of the rubber particles, represented by the d.sub.50 parameter, is 0.97 μm. PP6 A heterophasic polymer comprising 31.1 wt % of ethylene- propylene copolymer dispersed in a polypropylene homopolymer, wherein the amount of ethylene in the ethylene-propylene copolymer is 43.7 wt %. MFI of the final heterophasic polymer is 20.4 dg/min measured at 230° C. under a load of 2.16 kg according to ISO 1133. The flexural modulus at 23° C. in the parallel direction is 810 MPa. The volume average size of the rubber particles, represented by the d.sub.50 parameter, is 1.03 μm. PP7 A heterophasic polymer comprising 31.1 wt % of ethylene- propylene copolymer dispersed in a polypropylene homopolymer, wherein the amount of ethylene in the ethylene-propylene copolymer is 43.7 wt %. MFI of the final heterophasic polymer is 40.6 dg/min measured at 230° C. under a load of 2.16 kg according to ISO 1133. The flexural modulus at 23° C. in the parallel direction is 756 MPa. The volume average size of the rubber particles, represented by the d.sub.50 parameter, is 0.93 μm. Alpha-olefin Ethylene-octene copolymer having a MFI of 5.0 decigrams per minute (dg/min) measured at 190° C. under a load of 2.16 kg according to ASTM D 1238 Talc Talc Filler, d50 is 1.4 μm, d98 is 7.0 μm as measured on Sedigraph 5120. GF Glass fibers, 10 micrometer diameter, 4-5 mm long Coupling Maleic anhydride (MAh) functionalized homopolypropylene Agent produced by reactive extrusion. MAh level 0.5 to 1 wt %, MFI 100-120 [g/10 min] at 190° C./1.2 kg Tospearl Silicone Particles (methylsilsequioxane), average diameter (d.sub.50) is 2000B 6.0 μm PDMS 50% of an ultrahigh molecular weight polydimethylsiloxane polymer master batch dispersed in a polypropylene homopolymer Stabilizer A package of classical antioxidant & processing stabilizers package Slip agent Fatty acid amide Colorant Carbon black or pigments master batch
Catalyst A
(23) Catalyst A is prepared according to the method described in U.S. Pat. No. 5,093,415 of Dow, hereby incorporated by reference. This patent discloses an improved process to prepare a catalyst including a reaction between titanium tetrachloride, diisobutyl phthalate, and magnesium diethoxide to obtain a solid material. This solid material is then slurried with titanium tetrachloride in a solvent and phthaloyl chloride is added. The reaction mixture is heated to obtain a solid material which is reslurried in a solvent with titanium tetrachloride. Again this was heated and a solid collected. Once again the solid was reslurried once again in a solution of titanium tetrachloride to obtain a catalyst.
(24) PP1-PP7 were prepared using a two-step process as described here below:
(25) Step I)
(26) Five intermediate heterophasic propylene copolymers (A, B, C, D and E) were produced by co-polymerization of propylene and ethylene using two reactors in series. In the first reactor (temperature 60-85° C., pressure 2.2.10.sup.1-3.0 10.sup.1 bar), the propylene homopolymer matrix phase was prepared. After polymerization, the powder was transported from the first to the second reactor (temperature 60-85° C., pressure 2.2.10.sup.1-3.0 10.sup.1 bar) where the polymerization of the rubber phase consisting of an ethylene-propylene copolymer was done. Materials were prepared using the catalyst system composed of catalyst A and di(iso-propyl) dimethoxysilane (DiPDMS). Table 4 provides an overview of reactor powders A-E that were prepared in this manner.
(27) MFR R1 represents the melt flow rate of the propylene homopolymer manufactured in the first reactor. MFR R2 represents the melt flow rate of the intermediate heterophasic propylene copolymer powder obtained after the polymerization of the rubber phase in the second reactor.
(28) RC represents the amount of rubber phase (ethylene-propylene copolymer) based on the total weight of the heterophasic propylene copolymer and is measured using .sup.13C-NMR. RCC2 is the ethylene weight percentage of the ethylene-propylene copolymer phase and is also measured by .sup.13C-NMR.
(29) CXS and CXI represent, respectively, the amount of soluble and insoluble fractions in p-xylene at 25° C. based on the total weight of the heterophasic propylene copolymer. IV-CXS and IV-CXI represent the intrinsic viscosities of the p-xylene soluble and p-xylene insoluble fractions, respectively, measured in decaline at 135° C. according to DIN EN ISO 1628-1 and -3. The IV ratio is defined as the ratio of IV-CXS to IV-CXI.
(30) TABLE-US-00004 TABLE 4 Properties of intermediate heterophasic propylene copolymers MFR R1 MFR R2 RC RCC2 CXS IV-CXS CXI IV-CXI IV ratio Exp # dg/min dg/min wt. % wt. % wt. % dl/g wt. % dl/g — A 68 33 18.5 53 16.7 2.3 83.3 1.15 2.0 B 4.7 1.5 24 56.5 21.9 4.7 78.1 2.0 2.35 C 4.5 1.1 33.5 51.5 30.9 4.4 69.1 2.0 2.20 D 21.7 4.6 30.1 43.9 28.5 3.0 71.5 1.65 1.82 E 30.2 3.7 31.1 43.7 29.1 4.3 70.9 1.65 2.61
Step II)
(31) For achieving higher flow propylene heterophasic copolymers, reactor powders B, C, D and E (the intermediate heterophasic propylene copolymer powders) were peroxide shifted (i.e. visbreaking) to higher melt flow rates to obtain the final heterophasic propylene copolymers (PP2, PP3, PP4, PP5, PP6 and PP7). This was done by feeding the powder to an extruder and adding Luperco 802PP40 as a peroxide (1,4-bis(2-tert-butylperoxypropan-2-yl)benzene, CAS Registry Number: 2781-00-2) in different concentrations to achieve for each reactor powders different final melt flow rates. Table 5 lists details of the visbreaking experiments for the different reactor powders including starting MFR (intermediate MFR), target MFR (final MFR) and the amount of peroxide in weight percentage. Besides the peroxide, some additives common in the art were also added (0.25 weight percentage based on the total weight of the final heterophasic propylene copolymer). The additive package was the same for all experiments. PP1 was not visbroken, but was also extruded a second time with no peroxide to have the same processing history than other examples. The final heterophasic propylene copolymers have the same amount of rubber phase (RC) and the same amount of ethylene in the rubber phase (RCC2) than the intermediate heterophasic propylene copolymers (Table 3).
(32) TABLE-US-00005 TABLE 5 MFR change Intermediate Intermediate MFR Final MFR Peroxide Exp # powder dg/min dg/min wt. % PP1 A 33 33 0 PP2 B 1.5 14 0.105 PP3 C 1.1 17 0.125 PP4 D 4.6 20.5 0.085 PP5 D 4.6 41.2 0.2 PP6 E 3.7 20.4 0.095 PP7 E 3.7 40.6 0.215 PP1 is not peroxide shifted, but extruded a second time to have the same processing history than other examples. PP2 is peroxide shifted heterophasic copolymer from experiment B, PP3 is peroxide shifted heterophasic copolymer from experiment C, PP4 and PP5 are peroxide shifted heterophasic copolymers from experiment D, PP6 and PP7 are peroxide shifted heterophasic copolymers from experiment E. intermediate MFR is the MFR of the intermediate heterophasic propylene copolymer Final MFR is the MFR of the final heterophasic propylene copolymer.
Examples CE1-E6
(33) The components as recited in Table 3 for CE1-E6 (Examples CE1-CE2 and E3-E6) were mixed together and injected molded using a standard machine equipped with a three-zone screw typically used for mineral filled polypropylene compounds at a temperature of 240° C. The compositions of Examples CE1-E6 are shown in Table. Amounts of components are in wt %, unless otherwise indicated. Some common in the art stabilizers were also added (0.5 wt %). The stabilizer package was the same for all experiments.
(34) The total rubber content is defined as summation of the amount of ethylene-propylene copolymer in the heterophasic propylene copolymer, proportional to the amount of base resin used in the compositions, and the amount of Alpha-olefin added during compounding step.
(35) TABLE-US-00006 TABLE 6 Compositions CE1 CE2 E3 E4 E5 E6 PP1 (wt %) 10 PP2 (wt %) 31.4 PP3 (wt %) 41.4 PP4 (wt %) 41.4 PP5 (wt %) 41.4 PP6 (wt %) 41.4 PP7 (wt %) 41.4 Alpha-olefin (wt %) 25 25 25 25 25 25 Talc (wt %) 0.5 0.5 0.5 0.5 0.5 0.5 GF (wt %) 25 25 25 25 25 25 Coupling agent (wt %) 2.5 2.5 2.5 2.5 2.5 2.5 Tospearl (wt %) 1 1 1 1 1 1 Stabilizers (wt %) 0.5 0.5 0.5 0.5 0.5 0.5 PDMS master batch (wt %) 1 1 1 1 1 1 Slip agent (wt %) 0.1 0.1 0.1 0.1 0.1 0.1 Colorant (wt %) 3 3 3 3 3 3 Total (wt %) 100 100 100 100 100 100 Total rubber content (wt %) 34.4 38.9 37.5 37.5 37.9 37.9
(36) The mechanical and aesthetic properties were determined and are shown in Table.
(37) TABLE-US-00007 TABLE 7 Examples CE1 CE2 E3 E4 E5 E6 Ash content (%) 27.4 27.0 27.0 27.8 26.9 26.4 MFI ISO 1133 @ 230° C. Melt flow index (g/10 min) 7.4 7.0 9.5 15 8.7 12.5 Melt volume index 8.1 7.6 10.4 16.4 8.6 14.0 (cc/10 min) Notched Izod impact at 23° C. Izod impact (kJ/m.sup.2) 37.5 40.2 46.7 42.7 44.9 42.6 Notched Izod impact at −20° C. Izod impact (kJ/m.sup.2) 20.3 24.6 28 23.5 24 21.8 VEM ISO 6603-B2 at −10° C. after 7 days Energy at 90% Fmax (J) 6.4 6.2 6.66 6.36 6.52 6.01 Break Force (Fmax) (N) 1983 1993 2100 1995 2089 2085 Flexural modulus at 23° C. Flexural modulus parallel 1799 1259 1369 1459 1526 1650 (N/mm.sup.2) Flexural modulus, 965 740 723 781 817 959 perpendicular (N/mm.sup.2) Tensile modulus at 23° C. Tensile modulus (N/mm.sup.2) 2717 1943 2007 2182 2293 2435 Tensile strength (N/mm.sup.2) 33 24.4 24 24 29 29 Yield strength (N/mm.sup.2) 31.8 24.4 23.7 23.8 28.6 28.7 Elongation at yield (%) 7 6 6.1 4.8 7.9 6.4 Elongation at break (%) 9 8.2 9 7 11 9 Stress at break (N/mm.sup.2) 29 21.6 17.8 20.3 24.1 24.5 Warpage Measurements Warpage after 24 h at 3.1 4.7 2.8 2.5 2.5 2.4 23° C. Gloss values at 23° C. 20° 17 13 14 15 15 16 60° 46 35.4 43 44 44 44 85° 78 67 76 77 77 77 Tiger-stripe performance At 200° C., high injection 7 6 8 7 7 7 speed, textured, fan gate At 200° C., high injection 7 5 8 7 7 7 speed, textured, pinpoint gate At 230° C., high injection 7 6 8 7 8 7 speed, textured, fan gate At 230° C., high injection 7 5 8 7 7 7 speed, textured, pinpoint gate At 260° C., high injection 8 5 7 6 7 7 speed, textured, fan gate At 260° C., high injection 7 5 7 6 7 7 speed, textured, pinpoint gate Soft-touch performance + ++ ++ ++ ++ ++
(38) Table shows that all of examples E3-E6 have higher melt flow index than the comparative example CE1, as a result of the higher melt flow of the heterophasic propylene copolymer (A) (PP4-PP7). This is even more pronounced for E4 and E6 with MFI values of 15 and 12.5 dg/min compared to MFI of 7.4 dg/min for CE1. The MFI of E3-E6 was higher than that of CE2.
(39) Izod impact at 23° C. and −20° C. of examples E3-E6 is increased compared to comparative example CE1. E3 and E5 show an improvement in impact vs. CE1, resulting from higher total rubber content. The Izod impact of E3-E6 is similar to that of CE2.
(40) Falling dart impact (VEM) at −10° C. is maintained at the same level or shows slight increase in E3-E6 compared to CE1 and CE2.
(41) Flexural modulus in parallel and perpendicular directions of examples E3-E6 shows some decrease due to higher rubber fraction of the base resins (also referred to herein as heterophasic propylene copolymer (A)) used in the compounds (final compositions) when compared to CE1. The flexural modulus of E3-E6 generally shows some increase as compared to CE2.
(42) Same conclusion as for flexural modulus can be drawn for tensile modulus.
(43) Table also shows that increasing the total rubber content of the base resin and/or its melt flow index results in a decrease in warpage of the final composition, where CE1 shows higher warpage values as compared to those of E3-E6. CE2 shows a notably higher warpage value than those of E3-E6.
(44) Results present in Table show a trend in slight decreased gloss levels of E3-E6 when compared to CE1. These excellent results are unexpected, as the increase in total rubber content commonly leads to higher gloss levels. The gloss of E3-E6 is higher than that of CE2.
(45) Table shows that the tiger-stripe performance of E3-E6 is maintained at the level of CE1, although their total rubber content is increased. This is positively surprising result for injection molded article, as generally the higher total rubber content leads to worsened tiger-stripe performance. The tiger-stripe performance of E3-E6 is much better than that of CE2.
(46) Although the haptic properties of the comparative sample CE1 was already very good (ranked +), by increasing the total rubber content the haptic properties of E3-E6 were even further improved (ranked ++). The haptic properties of CE2 were similar as those of E3-E6.
CONCLUSION
(47) Comparing CE1 and CE2 to E3-E6, the compositions of the invention have a higher flow in combination with a good soft touch performance. Also, the results show that the compositions of the invention maintain properties and may even improve impact, warpage, tensile strength, gloss and/or tiger stripe performance, which makes the compositions of the invention suitable for (injection) molding applications as mentioned herein.