Reclaimed material-containing polypropylene composition with excellent coating adhesion

Abstract

A polypropylene composition (PC), the polypropylene composition (PC) being a hybrid plastic polypropylene blend wherein the polypropylene composition (PC) has: a) an MFR2 of from 1.0 to 30.0 g / 10 min; b) the layering area of the silver paint is 0.0 to 20.0 mm < 2 >; c) the layered area of the black paint is 0.0 to 20.0 mm < 2 >; d) a flexural modulus of from 1000 to 2000 MPa; e) a limonene content in the range of from 0.10 to 25.0 ppm; and f) an inorganic filler (F) content of 5.0 to 20.0 wt%, the inorganic filler (F) having a DL / DS value of 1.5 to 4.5; the polymer portion of the polypropylene composition (PC) has a content of a CRYSTEX QC soluble fraction (SF) of from 20.0 to 30.0 wt%, the soluble fraction (SF) having an intrinsic viscosity of from 2.40 to 3.50 dL / g, and a content of a CRYSTEX QC crystal fraction (CF) of from 70.0 to 80.0 wt%, the crystal fraction (CF) having an ethylene content of from 6.0 to 10.0 wt%.

Description

Technical Field

[0001] The present invention relates to a polypropylene composition (PC) and an article comprising the polypropylene composition (PC). The polypropylene composition (PC) is a mixed plastic polypropylene blend containing recycled materials. Background Art

[0002] Polyolefins, particularly polyethylene and polypropylene, are consumed in increasing quantities in a wide range of applications including packaging for food and other goods, fibers, automotive parts, and various manufactured articles.

[0003] Polypropylene-based materials have significant potential for mechanical recycling, as these materials are widely used in packaging. Considering the huge amount of waste collected (compared to the amount of waste recycled back into the stream), there is still great potential for the intelligent reuse of plastic waste streams and the mechanical recycling of plastic waste.

[0004] The development of polyolefins and polyolefin blends is generally focused on the goal of continuously improving the balance of mechanical properties, while also striving to more efficiently handle waste streams for economic and environmental reasons. It is generally believed that the use of recycled materials in polymer blends often leads to a deterioration in mechanical properties because the mechanical properties of virgin polymers are easy to adjust through polymerization conditions, while controlling the properties of recycled materials is inherently more difficult, resulting in inferior performance of such compositions.

[0005] For exterior applications in the automotive industry, materials are required to have good flow, coatability, surface appearance, and balanced mechanical properties in terms of stiffness and toughness. Recently, market demand has expanded towards the use of recycled polyolefins in virgin polymer blends to meet specific requirements.

[0006] However, there is an urgent need to enable the disposal and reuse of post-consumer polyolefin regrind in final products without posing health and safety risks.

[0007] Due to the poor homogeneity of recycled material blends, it is often observed that such recycled material blends have significantly lower performance than comparable virgin polymers in properties required for automotive exterior parts, such as paint adhesion.

[0008] Therefore, there is still a need to develop blends containing recycled materials with good surface properties to enable the use of recycled materials in applications requiring coating adhesion. Summary of the Invention

[0009] The present invention is based on the discovery that specific recycled material blends can be blended with two or more heterophasic propylene-ethylene copolymers, an ethylene-octene elastomer, fillers and various additives to form polypropylene compositions having a balanced profile of mechanical properties and excellent coating adhesion.

[0010] Alternatively, the polypropylene composition of the present invention may be described by its compositional properties rather than by the components used in the blend.

[0011] Therefore, in a first aspect, the present invention relates in the broadest sense to a polypropylene composition (PC), said polypropylene composition (PC) being a mixed plastic polypropylene blend, wherein said polypropylene composition (PC) has:

[0012] a) a melt flow rate (MFR2) of 1.0 to 30.0 g / 10 min, measured at 230°C and 2.16 kg according to ISO 1133;

[0013] b) The area of ​​the silver paint delamination measured according to the method defined in the measurement method is 0.0 to 20.0 mm 2 ;

[0014] c) The black paint delamination area measured according to the method defined in the measurement method is 0.0 to 20.0 mm 2 ;

[0015] d) According to ISO 178, use 80×10×4 mm injection molded in accordance with ISO 19069-2 3 The flexural modulus measured on the test bars was 1000 to 2000 MPa;

[0016] e) a limonene content of 0.10 to 25.0 ppm as measured by solid phase microextraction (HS-SPME-GC-MS); and

[0017] f) an inorganic filler (F) in an amount of 5.0 to 20.0 wt% relative to the total weight of the polypropylene composition (PC), said inorganic filler (F) having a median diameter (d ) measured according to ISO 13320-1 (laser) of 50 ) and the median diameter (d 50 ) ratio D L / D S The value ranges from 1.5 to 4.5;

[0018] The polymer fraction of the polypropylene composition (PC) has a soluble fraction (SF) content of 20.0 to 30.0 wt% as measured by CRYSTEX QC analysis, the polymer fraction of the polypropylene composition (PC) has a crystalline fraction (CF) content of 70.0 to 80.0 wt% as measured by CRYSTEX QC analysis, both contents are expressed as wt% with respect to the total weight of the polymer fraction of the polypropylene composition (PC), the inherent viscosity (iV(SF)) of the soluble fraction (SF) as measured by CRYSTEX QC analysis is 2.40 to 3.50 dL / g, the ethylene content (C2(CF)) of the crystalline fraction (CF) as measured by CRYSTEX QC analysis is 4.0 to 10.0 wt%.

[0019] Preferably, the polypropylene composition (PC) is obtainable by blending at least the following components a) to f):

[0020] a) 30.0 to 50.0 wt% of a first heterophasic propylene-ethylene copolymer (HECO1) with respect to the total weight of the polypropylene composition (PC), the first heterophasic propylene-ethylene copolymer (HECO1) has an ethylene content (C2(total)) of 8.1 to 20.0 wt% as measured by CRYSTEX QC analysis;

[0021] b) 5.0 to 15.0 wt% of a second heterophasic propylene-ethylene copolymer (HECO2) with respect to the total weight of the polypropylene composition (PC), the second heterophasic propylene-ethylene copolymer (HECO2) has an ethylene content (C2(total)) of 3.0 to 8.0 wt% as measured by CRYSTEX QC analysis;

[0022] c) 20.0 to 30.0 wt% of a mixed plastic polypropylene blend (B) with respect to the total weight of the polypropylene composition (PC), the mixed plastic polypropylene blend (B) has a melt flow rate (MFR2) of 10 to 50 g / 10 min as measured according to ISO 1133 at 230 °C and 2.16 kg;

[0023] d) 2.0 to 10.0 wt% of an ethylene-octene elastomer (EC);

[0024] e) 5.0 to 20.0 wt% of an inorganic filler (F);

[0025] f) 0.2 to 5.0 wt% of further additives (A);

[0026] The total content of components a) to f) with respect to the total weight of the polypropylene composition (PC) amounts to at least 95 wt%, more preferably to at least 98 wt%, most preferably to 100 wt%.

[0027] In a second aspect, the present application relates to a polypropylene composition (PC) having a melt flow rate (MFR2) measured according to ISO 1133 at 230 °C and 2.16 kg in the range of 1.0 to 30.0 g / 10 min, and obtainable by blending at least the following components a) to f):

[0028] a) 30.0 to 50.0 wt%, relative to the total weight of the polypropylene composition (PC), of a first heterophasic propylene-ethylene copolymer (HECO1) having an ethylene content (C2(total)) measured according to CRYSTEX QC analysis in the range of 8.1 to 20.0 wt%;

[0029] b) 5.0 to 15.0 wt%, relative to the total weight of the polypropylene composition (PC), of a second heterophasic propylene-ethylene copolymer (HECO2) having an ethylene content (C2(total)) measured according to CRYSTEX QC analysis in the range of 3.0 to 8.0 wt%;

[0030] c) 20.0 to 30.0 wt%, relative to the total weight of the polypropylene composition (PC), of a mixed plastic polypropylene blend (B) having a melt flow rate (MFR2) measured according to ISO 1133 at 230 °C and 2.16 kg in the range of 10 to 50 g / 10 min;

[0031] d) 2.0 to 10.0 wt% of an ethylene-octene elastomer (EC);

[0032] e) 5.0 to 20.0 wt% of an inorganic filler (F);

[0033] f) 0.2 to 5.0 wt% of further additives (A);

[0034] The total content of components a) to f) amounts to at least 95 wt%, more preferably at least 98 wt%, most preferably 100 wt%, relative to the total weight of the polypropylene composition (PC).

[0035] In another aspect, the present application relates to an article, preferably an injection molded article, comprising at least 95 wt%, more preferably at least 98 wt%, most preferably at least 99 wt%, of the polypropylene composition (PC) of the first or second aspect.

[0036] Definitions

[0037] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as those commonly understood by one of ordinary skill in the art to which this application belongs. Although methods and materials similar or equivalent to those described herein can be used in the practice and testing of the present application, the preferred methods and materials are described herein. In describing and claiming the present application, the following terminology will be used in accordance with the following definitions.

[0038] The use of the terms "a" and "an" and "the" and "at least one" are used generically herein, and are intended to mean one or more unless specifically stated otherwise.

[0039] Hereinafter, amounts are given in weight percent (wt%) unless otherwise stated.

[0040] A polypropylene homopolymer is a polymer consisting essentially of propylene monomer units. Due to impurities, especially during the commercial polymerization process, the polypropylene homopolymer can contain up to 0.1 mol% of comonomer units, preferably up to 0.05 mol% of comonomer units, most preferably up to 0.01 mol% of comonomer units.

[0041] A polypropylene copolymer is a copolymer of propylene monomer units and comonomer units, the comonomer units being preferably selected from ethylene and C4-C8a-olefins. A polypropylene random copolymer is a propylene copolymer in which the comonomer units are randomly distributed along the polymer chain, whereas a polypropylene block copolymer comprises blocks of propylene monomer units and blocks of comonomer units. A polypropylene random copolymer can comprise comonomer units from more than one comonomer differing in the amount of carbon atoms.

[0042] Typically, the heterophasic propylene copolymer comprises:

[0043] a) a crystalline propylene homopolymer or copolymer matrix (M); and

[0044] b) an elastomeric rubber, preferably a propylene-ethylene copolymer (E);

[0045] In the case of a random heterophasic propylene copolymer, the crystalline matrix phase is a random copolymer of propylene and at least one a-olefin comonomer.

[0046] The elastomeric phase can be a propylene copolymer with a high content of comonomers which are not randomly distributed in the polymer chain, but are distributed in block structures rich in comonomer and block structures rich in propylene. The heterophasic polypropylene is generally distinguished from the homophasic propylene copolymer in that it shows two distinct glass transition temperatures Tg g .

[0047] For the purposes of the present specification and the following claims, the term "recycled scrap" is used to mean materials recovered from post-consumer scrap and industrial scrap, as opposed to virgin polymers. Post-consumer scrap refers to items that have completed at least a first use cycle (or life cycle), i.e., items that have fulfilled their original purpose; while industrial scrap refers to manufacturing waste that typically does not reach the consumer.

[0048] The term "virgin" refers to newly produced materials and / or items prior to first use, and not recycled.

[0049] For example, the term "recycled material" as used herein refers to a material that has been reprocessed from "recycled scrap".

[0050] A polymer blend is a mixture of two or more polymer components. Typically, the blend can be prepared by mixing two or more polymer components. Suitable mixing processes known in the art are post-polymerization blending.

[0051] Post-polymerization blending can be dry blending of polymer components (e.g., polymer powders and / or compounded polymer pellets), or can be melt blending achieved by melt mixing the polymer components.

[0052] Mixed plastic polypropylene blends mean that the blend comprises predominantly polypropylene, but there is still a small amount of other plastics. Recycle blends, especially post-consumer recycle blends, are almost always mixed plastic blends, which reflects the efficiency of the sorting in the prior art recycling processes.

[0053] The present application will now be described in more detail. DETAILED DESCRIPTION

[0054] Polypropylene composition (PC) of the first aspect

[0055] In the first aspect, the present application relates to a polypropylene composition (PC) which is a mixed plastic polypropylene blend.

[0056] The polypropylene composition (PC) has a melt flow rate (MFR2) measured according to ISO 1133 at 230 °C and 2.16 kg of 1.0 to 30.0 g / 10 min, more preferably of 3.0 to 20.0 g / 10 min, most preferably of 5.0 to 15.0 g / 10 min.

[0057] The polypropylene composition (PC) has a silver paint delamination area of 0.0 to 20.0 mm 2 , more preferably of 0.0 to 10.0 mm 2 , most preferably of 0.0 to 5.0 mm 2 .

[0058] The polypropylene composition (PC) has a black paint delamination area of 0.0 to 20.0 mm2 more preferably 0.0 to 10.0 mm 2 most preferably 0.0 to 5.0 mm 2 .

[0059] The polypropylene composition (PC) has a limonene content of 0.10 to 25.0 ppm as determined according to solid phase microextraction (HS-SPME-GC-MS).

[0060] The limonene content indicates that the polypropylene composition (PC) contains at least one component derived from post-consumer waste. Therefore, it is also preferred that the polypropylene composition (PC) comprises a recycled material, i.e. comprises recycled content. It is particularly preferred that the polypropylene composition (PC) is at least partially derived from post-consumer waste.

[0061] The polypropylene composition (PC) has a flexural modulus of 1000 to 2000 MPa, more preferably 1200 to 1800 MPa, most preferably 1400 to 1600 MPa, as determined on a 80 x 10 x 4 mm 3 test bar according to ISO 178 using injection moulding according to ISO 19069-2.

[0062] The polypropylene composition (PC) has a Charpy notched impact strength at 23 °C of 40 to 100 kJ / m 3 as determined on a 80 x 10 x 4 mm 2 test bar according to ISO 179 using injection moulding according to ISO 19069-2. 2 more preferably 45 to 90 kJ / m 2 .

[0063] The polypropylene composition (PC) has a Charpy notched impact strength at -20 °C of 3.0 to 15 kJ / m 3 as determined on a 80 x 10 x 4 mm 2 test bar according to ISO 179 using injection moulding according to ISO 19069-2. 2 more preferably 4.0 to 12.0 kJ / m 2 .

[0064] The polypropylene composition (PC) has a longitudinal coefficient of linear thermal expansion (CLTE) of 0 to 100 x 10 -6 / K, more preferably 50 to 95 x 10 -6 / K, most preferably 70 to 90 x 10 -6 / K as determined according to ISO 11359-2.

[0065] The content of the inorganic filler (F) of the polypropylene composition (PC) is from 5.0 to 20.0 wt%, more preferably from 9.0 to 18.0 wt%, most preferably from 13.0 to 17.0 wt%.

[0066] The D L / D S value (i.e. the ratio of the median diameter (d 50 measured according to ISO 13320-1 (laser) to the median diameter (d 50 measured according to ISO 13317-3 (sedigraph)) is from 1.5 to 4.5, more preferably from 1.8 to 4.0, most preferably from 2.0 to 3.5.

[0067] The D L / D S value serves as an indicator for the aspect ratio of the inorganic filler, wherein a higher D L / D S value indicates a higher aspect ratio.

[0068] The median diameter (d 50 ) of the inorganic filler (F) measured according to ISO 13320-1 (laser) is preferably from 3.0 to 10.0 pm, more preferably from 4.0 to 8.5 pm, most preferably from 4.5 to 7.0 pm.

[0069] The top cut diameter (d 95 ) of the inorganic filler (F) measured according to ISO 13320-1 (laser) is preferably from 8.0 to 30.0 pm, more preferably from 9.0 to 25.0 pm, most preferably from 10.0 to 20.0 pm.

[0070] The median diameter (d 50 ) of the inorganic filler (F) measured according to ISO 13317-3 (sedigraph) is preferably from 1.0 to 3.0 pm, more preferably from 1.3 to 2.5 pm, most preferably from 1.5 to 2.0 pm.

[0071] The top cut diameter (d 95 ) of the inorganic filler (F) measured according to ISO 13317-3 (sedigraph) is preferably from 4.0 to 10.0 pm, more preferably from 4.5 to 9.0 pm, most preferably from 5.0 to 8.0 pm.

[0072] Preferably, the inorganic filler is selected from talc, calcium carbonate, barium sulfate, mica and mixtures thereof.

[0073] Most preferably, the inorganic filler (F) is talc.

[0074] The polymer fraction of the polypropylene composition (PC) can be characterized by the CRYSTEX QC method employing trichlorobenzene (TCB) as solvent. This method is described in the following determination methods section. The crystalline fraction (CF) comprises predominantly the matrix phase and only a small fraction of the elastomeric phase, and the soluble fraction (SF) comprises predominantly the elastomeric phase and only a small fraction of the matrix phase. In certain cases this method can provide more useful data, as the crystalline fraction (CF) and the soluble fraction (SF) more accurately correspond to the matrix phase and the elastomeric phase, respectively. Due to the differences in the separation methods of the xylene extraction and the CRYSTEX QC method, the properties of the XCS / XCI fractions and the crystalline / soluble (CF / SF) fractions are not exactly the same on the other hand, which means that the content and properties of the matrix phase and the elastomeric phase can differ.

[0075] The polymer fraction of the polypropylene composition (PC) has an ethylene content (C2(total)) measured according to CRYSTEX QC analysis of preferably 10.0 to 30.0 wt%, more preferably 13.0 to 25.0 wt%, most preferably 15.0 to 20.0 wt%.

[0076] The polymer fraction of the polypropylene composition (PC) has an intrinsic viscosity (iV(total)) measured according to CRYSTEX QC analysis of preferably 1.50 to 3.00 dL / g, more preferably 1.60 to 2.60 dL / g, most preferably 1.70 to 2.20 dL / g.

[0077] The polymer fraction of the polypropylene composition (PC) has a soluble fraction (SF) content of 20.0 to 30.0 wt%, more preferably 23.0 to 30.0 wt%, most preferably 25.0 to 30.0 wt% measured according to CRYSTEX QC analysis.

[0078] The soluble fraction (SF) has an ethylene content (C2(SF)) measured according to CRYSTEX QC analysis of preferably 30.0 to 60.0 wt%, more preferably 35.0 to 55.0 wt%, most preferably 40.0 to 50.0 wt%.

[0079] The soluble fraction (SF) has an intrinsic viscosity (iV(SF)) of 2.40 to 3.50 dL / g, more preferably 2.45 to 3.20 dL / g, most preferably 2.50 to 2.90 dL / g measured according to CRYSTEX QC analysis.

[0080] The polymer fraction of the polypropylene composition (PC) has a crystalline fraction (CF) content of 70.0 to 80.0 wt%, more preferably 70.0 to 77.0 wt%, most preferably 70.0 to 75.0 wt% measured according to CRYSTEX QC analysis.

[0081] The crystalline fraction (CF) has an ethylene content (C2(CF)) of 4.0 to 10.0 wt.-%, more preferably of 4.0 to 8.0 wt.-%, most preferably of 4.0 to 6.0 wt.-%, determined according to CRYSTEX QC analysis.

[0082] The crystalline fraction (CF) has an intrinsic viscosity (iV(CF)) of 1.00 to 2.50 dL / g, more preferably of 1.20 to 2.20 dL / g, most preferably of 1.40 to 1.90 dL / g, determined according to CRYSTEX QC analysis.

[0083] It is further preferred that the ratio of the intrinsic viscosities of the soluble fraction and the crystalline fraction (iV(SF) / iV(CF)), determined according to CRYSTEX QC analysis, is 1.00 to 3.00, more preferably 1.30 to 2.50, most preferably 1.50 to 2.00.

[0084] It is further preferred that the ratio of the ethylene contents of the soluble fraction and the crystalline fraction (C2(SF) / C2(CF)), determined according to CRYSTEX QC analysis, is 6.0 to 12.0, more preferably 7.0 to 11.0, most preferably 8.0 to 10.0.

[0085] Preferably, the polypropylene composition (PC) is obtainable by blending at least the following components a) to f):

[0086] a) 30.0 to 50.0 wt.-%, relative to the total weight of the polypropylene composition (PC), of a first heterophasic propylene-ethylene copolymer (HECO1);

[0087] b) 5.0 to 15.0 wt.-%, relative to the total weight of the polypropylene composition (PC), of a second heterophasic propylene-ethylene copolymer (HECO2);

[0088] c) 20.0 to 30.0 wt.-%, relative to the total weight of the polypropylene composition (PC), of a mixed plastic polypropylene blend (B);

[0089] d) 2.0 to 10.0 wt.-% of an ethylene-octene elastomer (EC);

[0090] e) 5.0 to 20.0 wt.-% of an inorganic filler (F);

[0091] f) 0.2 to 5.0 wt.-% of further additives (A).

[0092] The total content of components a) to f) amounts to at least 95 wt.-%, more preferably to at least 98 wt.-%, most preferably to 100 wt.-%, relative to the total weight of the polypropylene composition (PC).

[0093] More preferably, the polypropylene composition (PC) is obtainable by blending at least the following components a) to f):

[0094] a) 35.0 to 45.0 wt% of a first heterophasic propylene-ethylene copolymer (HECO1) with respect to the total weight of the polypropylene composition (PC);

[0095] b) 6.0 to 13.0 wt% of a second heterophasic propylene-ethylene copolymer (HECO2) with respect to the total weight of the polypropylene composition (PC);

[0096] c) 22.0 to 28.0 wt% of a mixed plastic polypropylene blend (B) with respect to the total weight of the polypropylene composition (PC);

[0097] d) 5.0 to 10.0 wt% of an ethylene-octene elastomer (EC);

[0098] e) 9.0 to 18.0 wt% of an inorganic filler (F);

[0099] f) 0.2 to 5.0 wt% of further additives (A).

[0100] Most preferably, the polypropylene composition (PC) is obtainable by blending at least the following components a) to f):

[0101] a) 37.0 to 41.0 wt% of a first heterophasic propylene-ethylene copolymer (HECO1) with respect to the total weight of the polypropylene composition (PC);

[0102] b) 8.0 to 11.0 wt% of a second heterophasic propylene-ethylene copolymer (HECO2) with respect to the total weight of the polypropylene composition (PC);

[0103] c) 23.0 to 27.0 wt% of a mixed plastic polypropylene blend (B) with respect to the total weight of the polypropylene composition (PC);

[0104] d) 8.0 to 10.0 wt% of an ethylene-octene elastomer (EC);

[0105] e) 13.0 to 17.0 wt% of an inorganic filler (F);

[0106] f) 0.2 to 5.0 wt% of further additives (A).

[0107] The blending of the polypropylene composition (PC) can be performed in a process comprising the following steps:

[0108] a) providing a first heterophasic propylene-ethylene copolymer (HECO1), optionally a second heterophasic propylene-ethylene copolymer (HECO2), a mixed plastic polypropylene blend (B), an ethylene-octene elastomer (EC), an inorganic filler (F) and further additives (A);

[0109] b) blending and extruding the first heterophasic propylene-ethylene copolymer (HECO1), optionally the second heterophasic propylene-ethylene copolymer (HECO2), the mixed plastic polypropylene blend (B), the ethylene-octene elastomer (EC), the inorganic filler (F) and the further additives (A) in an extruder, preferably a twin-screw extruder, at a temperature of 120 to 250 °C, thereby generating a polypropylene composition (PC), preferably in the form of pellets.

[0110] In particular, it is preferred to use conventional compounding or blending equipment, such as a Banbury mixer, a two-roll rubber mill, a Buss co-kneader or a twin-screw extruder. More preferably, the mixing is done in a co-rotating twin-screw extruder. The polymer material withdrawn from the extruder is typically in the form of pellets.

[0111] The polypropylene composition (PC) of the second aspect

[0112] The polypropylene composition (PC) of the second aspect can be obtained by blending at least the following components a) to f):

[0113] a) 30.0 to 50.0 wt% of a first heterophasic propylene-ethylene copolymer (HECO1) relative to the total weight of the polypropylene composition (PC);

[0114] b) 5.0 to 15.0 wt% of a second heterophasic propylene-ethylene copolymer (HECO2) relative to the total weight of the polypropylene composition (PC);

[0115] c) 20.0 to 30.0 wt% of a mixed plastic polypropylene blend (B) relative to the total weight of the polypropylene composition (PC);

[0116] d) 2.0 to 10.0 wt% of an ethylene-octene elastomer (EC);

[0117] e) 5.0 to 20.0 wt% of an inorganic filler (F);

[0118] f) 0.2 to 5.0 wt% of further additives (A).

[0119] The total content of components a) to f) amounts to at least 95 wt%, more preferably to at least 98 wt% and most preferably to 100 wt% relative to the total weight of the polypropylene composition (PC).

[0120] More preferably, the polypropylene composition (PC) is obtainable by blending at least the following components a) to f):

[0121] a) 35.0 to 45.0 wt% of a first heterophasic propylene-ethylene copolymer (HECO1) with respect to the total weight of the polypropylene composition (PC);

[0122] b) 6.0 to 13.0 wt% of a second heterophasic propylene-ethylene copolymer (HECO2) with respect to the total weight of the polypropylene composition (PC);

[0123] c) 22.0 to 28.0 wt% of a mixed plastic polypropylene blend (B) with respect to the total weight of the polypropylene composition (PC);

[0124] d) 5.0 to 10.0 wt% of an ethylene-octene elastomer (EC);

[0125] e) 9.0 to 18.0 wt% of an inorganic filler (F);

[0126] f) 0.2 to 5.0 wt% of further additives (A).

[0127] Most preferably, the polypropylene composition (PC) is obtainable by blending at least the following components a) to f):

[0128] a) 37.0 to 41.0 wt% of a first heterophasic propylene-ethylene copolymer (HECO1) with respect to the total weight of the polypropylene composition (PC);

[0129] b) 8.0 to 11.0 wt% of a second heterophasic propylene-ethylene copolymer (HECO2) with respect to the total weight of the polypropylene composition (PC);

[0130] c) 23.0 to 27.0 wt% of a mixed plastic polypropylene blend (B) with respect to the total weight of the polypropylene composition (PC);

[0131] d) 8.0 to 10.0 wt% of an ethylene-octene elastomer (EC);

[0132] e) 13.0 to 17.0 wt% of an inorganic filler (F);

[0133] f) 0.2 to 5.0 wt% of further additives (A).

[0134] The blending of the polypropylene composition (PC) can be performed in a process comprising the following steps:

[0135] a) providing a first heterophasic propylene-ethylene copolymer (HECO1), optionally a second heterophasic propylene-ethylene copolymer (HECO2), a mixed plastic polypropylene blend (B), an ethylene-octene elastomer (EC), an inorganic filler (F) and further additives (A);

[0136] b) blending and extruding the first heterophasic propylene-ethylene copolymer (HECO1), optionally the second heterophasic propylene-ethylene copolymer (HECO2), the mixed plastic polypropylene blend (B), the ethylene-octene elastomer (EC), the inorganic filler (F) and the further additives (A) in an extruder, preferably a twin-screw extruder, at a temperature of 120 to 250 °C, thereby generating a polypropylene composition (PC), preferably in the form of a pellet.

[0137] In particular, it is preferred to use conventional compounding or blending equipment, such as a Banbury mixer, a two-roll rubber mill, a Buss Ko-kneader or a twin-screw extruder. More preferably, the mixing is done in a co-rotating twin-screw extruder. The polymer material withdrawn from the extruder is typically in the form of pellets.

[0138] The polypropylene composition (PC) has a melt flow rate (MFR2) measured according to ISO 1133 at 230 °C and 2.16 kg of 1.0 to 30.0 g / 10 min, more preferably of 3.0 to 20.0 g / 10 min, most preferably of 5.0 to 15.0 g / 10 min.

[0139] The polypropylene composition (PC) has a silver paint delamination area of preferably 0.0 to 20.0 mm 2 , more preferably of 0.0 to 10.0 mm 2 , most preferably of 0.0 to 5.0 mm 2 .

[0140] The polypropylene composition (PC) has a black paint delamination area of preferably 0.0 to 20.0 mm 2 , more preferably of 0.0 to 10.0 mm 2 , most preferably of 0.0 to 5.0 mm 2 .

[0141] The polypropylene composition (PC) has a limonene content of 0.10 to 25.0 ppm, measured according to solid phase microextraction (HS-SPME-GC-MS).

[0142] The limonene content indicates that the polypropylene composition (PC) contains at least one component derived from post-consumer waste. Therefore, it is also preferred that the polypropylene composition (PC) comprises a recycled material, i.e. comprises recycled content. It is particularly preferred that the polypropylene composition (PC) is at least partially derived from post-consumer waste.

[0143] Polypropylene composition (PC) was prepared according to ISO 178 using an 80×10×4 mm2 injection molded plastic according to ISO 19069-2. 3 The flexural modulus measured on the test strips is preferably from 1000 to 2000 MPa, more preferably from 1200 to 1800 MPa, most preferably from 1400 to 1600 MPa.

[0144] Polypropylene composition (PC) was prepared according to ISO 179 using an 80×10×4 mm2 injection molded plastic according to ISO 19069-2. 3 The Charpy notched impact strength at 23°C measured on a test strip is preferably 40 to 100 kJ / m 2 , more preferably 45 to 90 kJ / m 2 , most preferably 50 to 80 kJ / m 2 .

[0145] Polypropylene composition (PC) was prepared according to ISO 179 using an 80×10×4 mm2 injection molded plastic according to ISO 19069-2. 3 The Charpy notched impact strength at -20°C measured on a test bar is preferably 3.0 to 15.0 kJ / m 2 , more preferably 4.0 to 12.0 kJ / m 2 , most preferably 5.0 to 9.0 kJ / m 2 .

[0146] The coefficient of longitudinal linear thermal expansion (CLTE) of the polypropylene composition (PC) measured according to ISO 11359-2 is preferably 0 to 100×10 -6 / K, more preferably 50 to 95×10 -6 / K, most preferably 70 to 90×10 -6 / K.

[0147] The polymer part of the polypropylene composition (PC) preferably has an ethylene content (C2(total)) as determined according to CRYSTEX QC analysis of 10.0 to 30.0 wt-%, more preferably 13.0 to 25.0 wt-%, most preferably 15.0 to 20.0 wt-%.

[0148] The polymer part of the polypropylene composition (PC) preferably has an intrinsic viscosity (iV(total)) as measured according to CRYSTEX QC analysis of 1.50 to 3.00 dL / g, more preferably 1.60 to 2.60 dL / g, most preferably 1.70 to 2.20 dL / g.

[0149] The polymer fraction of the polypropylene composition (PC) has a soluble fraction (SF) content measured according to CRYSTEX QC analysis preferably in the range of 20.0 to 30.0 wt.-%, more preferably in the range of 23.0 to 30.0 wt.-%, most preferably in the range of 25.0 to 30.0 wt.-%.

[0150] The soluble fraction (SF) has an ethylene content (C2(SF)) measured according to CRYSTEX QC analysis preferably in the range of 30.0 to 60.0 wt.-%, more preferably in the range of 35.0 to 55.0 wt.-%, most preferably in the range of 40.0 to 50.0 wt.-%.

[0151] The soluble fraction (SF) has an intrinsic viscosity (iV(SF)) measured according to CRYSTEX QC analysis preferably in the range of 2.40 to 3.50 dL / g, more preferably in the range of 2.45 to 3.20 dL / g, most preferably in the range of 2.50 to 2.90 dL / g.

[0152] The polymer fraction of the polypropylene composition (PC) has a crystalline fraction (CF) content measured according to CRYSTEX QC analysis preferably in the range of 70.0 to 80.0 wt.-%, more preferably in the range of 70.0 to 77.0 wt.-%, most preferably in the range of 70.0 to 75.0 wt.-%.

[0153] The crystalline fraction (CF) has an ethylene content (C2(CF)) measured according to CRYSTEX QC analysis preferably in the range of 4.0 to 10.0 wt.-%, more preferably in the range of 4.0 to 8.0 wt.-%, most preferably in the range of 4.0 to 6.0 wt.-%.

[0154] The crystalline fraction (CF) has an intrinsic viscosity (iV(CF)) measured according to CRYSTEX QC analysis preferably in the range of 1.00 to 2.50 dL / g, more preferably in the range of 1.20 to 2.20 dL / g, most preferably in the range of 1.40 to 1.90 dL / g.

[0155] It is further preferred that the ratio of the intrinsic viscosities of the soluble fraction and the crystalline fraction (iV(SF) / iV(CF)) measured according to CRYSTEX QC analysis is in the range of 1.00 to 3.00, more preferably in the range of 1.30 to 2.50, most preferably in the range of 1.50 to 2.00.

[0156] It is further preferred that the ratio of the ethylene contents of the soluble fraction and the crystalline fraction (C2(SF) / C2(CF)) measured according to CRYSTEX QC analysis is in the range of 6.0 to 12.0, more preferably in the range of 7.0 to 11.0, most preferably in the range of 8.0 to 10.0.

[0157] The following sections will now detail the properties of the individual components (for both the first and the second aspect).

[0158] first heterophasic propylene-ethylene copolymer (HECO1)

[0159] The amount of the provided first heterophasic propylene-ethylene copolymer (HECO1) is 30.0 to 50.0 wt.-%, more preferably 35.0 to 45.0 wt.-%, most preferably 37.0 to 41.0 wt.-%, relative to the total weight of the polypropylene composition (PC).

[0160] The first heterophasic propylene-ethylene copolymer (HECO1) has a melt flow rate (MFR2) measured according to ISO 1133 at 230 °C and 2.16 kg of preferably 1.0 to 50 g / 10 min, more preferably 3.0 to 30 g / 10 min, most preferably 5.0 to 20 g / 10 min.

[0161] The first heterophasic propylene-ethylene copolymer (HECO1) has an ethylene content (C2(total)) measured according to CRYSTEX QC analysis of 8.1 to 20.0 wt.-%, more preferably 10.0 to 18.0 wt.-%, most preferably 13.0 to 17.0 wt.-%.

[0162] The first heterophasic propylene-ethylene copolymer (HECO1) has a soluble fraction (SF) content measured according to CRYSTEX QC analysis of preferably 20.0 to 40.0 wt.-%, more preferably 25.0 to 37.0 wt.-%, most preferably 29.0 to 35.0 wt.-%.

[0163] The first heterophasic propylene-ethylene copolymer (HECO1) has an ethylene content (C2(SF)) of the soluble fraction measured according to CRYSTEX QC analysis of preferably 25.0 to 45.0 wt.-%, more preferably 30.0 to 42.0 wt.-%, most preferably 35.0 to 40.0 wt.-%.

[0164] The first heterophasic propylene-ethylene copolymer (HECO1) has an intrinsic viscosity (iV(SF)) of the soluble fraction measured according to CRYSTEX QC analysis of 2.00 to 4.00 dL / g, more preferably 2.60 to 3.80 dL / g, most preferably 3.20 to 3.60 dL / g.

[0165] The first heterophasic propylene-ethylene copolymer (HECO1) has a crystalline fraction (CF) content measured according to CRYSTEX QC analysis of preferably 60.0 to 80.0 wt.-%, more preferably 63.0 to 75.0 wt.-%, most preferably 65.0 to 71.0 wt.-%.

[0166] The first heterophasic propylene ethylene copolymer (HECO1) has an ethylene content of the crystalline fraction (C2(CF)) measured according to CRYSTEX QC analysis of 1.0 to 8.0 wt.-%, more preferably of 2.0 to 7.0 wt.-%, most preferably of 4.0 to 6.0 wt.-%.

[0167] The first heterophasic propylene ethylene copolymer (HECO1) has an intrinsic viscosity of the crystalline fraction (iV(CF)) measured according to CRYSTEX QC analysis of 1.10 to 2.00 dL / g, more preferably of 1.20 to 1.80 dL / g, most preferably of 1.30 to 1.60 dL / g.

[0168] It is also preferred that the ratio of the intrinsic viscosities of the soluble fraction and the crystalline fraction (iV(SF) / iV(CF)) measured according to CRYSTEX QC analysis is 1.20 to 4.00, more preferably 1.50 to 3.00, most preferably 2.00 to 2.50.

[0169] The second heterophasic propylene-ethylene copolymer (HECO2)

[0170] The amount of the second heterophasic propylene-ethylene copolymer (HECO2) provided is 6.0 to 13.0 wt.-%, more preferably 5.0 to 15.0 wt.-%, most preferably 8.0 to 11.0 wt.-%, relative to the total weight of the polypropylene composition (PC).

[0171] The second heterophasic propylene-ethylene copolymer (HECO2) has a melt flow rate (MFR2) measured according to ISO 1133 at 230 °C and 2.16 kg of 1.0 to 15 g / 10 min, more preferably of 3.0 to 10.0 g / 10 min, most preferably of 5.0 to 8.0 g / 10 min.

[0172] The second heterophasic propylene ethylene copolymer (HECO2) has an ethylene content (C2(total)) measured according to CRYSTEX QC analysis of 3.0 to 8.0 wt.-%, more preferably of 4.0 to 8.0 wt.-%, most preferably of 5.0 to 8.0 wt.-%.

[0173] The second heterophasic propylene ethylene copolymer (HECO2) has a soluble fraction (SF) content measured according to CRYSTEX QC analysis of 10.0 to 30.0 wt.-%, more preferably of 14.0 to 27.0 wt.-%, most preferably of 18.0 to 24.0 wt.-%.

[0174] The second heterophasic propylene ethylene copolymer (HECO2) has an ethylene content of the soluble fraction (C2(SF)) measured according to CRYSTEX QC analysis preferably in the range of 10.0 to 30.0 wt%, more preferably in the range of 15.0 to 27.0 wt%, most preferably in the range of 20.0 to 25.0 wt%.

[0175] The second heterophasic propylene ethylene copolymer (HECO2) has an intrinsic viscosity of the soluble fraction (iV(SF)) measured according to CRYSTEX QC analysis in the range of 3.00 to 7.00 dL / g, more preferably in the range of 4.00 to 6.00 dL / g, most preferably in the range of 4.50 to 5.50 dL / g.

[0176] The second heterophasic propylene ethylene copolymer (HECO2) has a crystalline fraction (CF) content measured according to CRYSTEX QC analysis preferably in the range of 70.0 to 90.0 wt%, more preferably in the range of 73.0 to 86.0 wt%, most preferably in the range of 76.0 to 82.0 wt%.

[0177] The second heterophasic propylene ethylene copolymer (HECO2) has an ethylene content of the crystalline fraction (C2(CF)) measured according to CRYSTEX QC analysis preferably in the range of 0.0 to 5.0 wt%, more preferably in the range of 0.5 to 4.0 wt%, most preferably in the range of 1.0 to 3.0 wt%.

[0178] The second heterophasic propylene ethylene copolymer (HECO2) has an intrinsic viscosity of the crystalline fraction (iV(CF)) measured according to CRYSTEX QC analysis in the range of 1.40 to 2.70 dL / g, more preferably in the range of 1.60 to 2.40 dL / g, most preferably in the range of 1.80 to 2.10 dL / g.

[0179] It is further preferred that the ratio of the intrinsic viscosities of the soluble fraction and the crystalline fraction (iV(SF) / iV(CF)) measured according to CRYSTEX QC analysis is in the range of 2.00 to 5.00, more preferably in the range of 2.30 to 4.00, most preferably in the range of 2.50 to 3.00.

[0180] Mixed plastic polypropylene blend (B)

[0181] The amount of the mixed plastic polypropylene blend (B) provided is in the range of 20.0 to 30.0 wt%, more preferably in the range of 22.0 to 28.0 wt%, most preferably in the range of 23.0 to 27.0 wt% relative to the total weight of the polypropylene composition (PC).

[0182] The mixed plastic polypropylene blend (B) is a polypropylene-rich recycled material, meaning that its polypropylene content is significantly higher than that of polyethylene. Polypropylene-rich recycled waste streams are available, for example, from the automotive industry, especially since some automotive parts (e.g., bumpers) are a source of fairly pure polypropylene material in the recycling stream.

[0183] Preferably, the polypropylene-rich recycled material is obtained from recycled waste by plastic recycling processes known in the art. Such recycled materials can be obtained from commercial sources, such as Corepla (Italian packaging plastic waste collection, recycling and recovery consortium), Resource Plastics (Brampton, Ontario), Kruschitz GmbH, Plastics and Recycling (AT), Vogt Plastik GmbH (Germany), Mtm ​​Plastics GmbH (Germany), etc. Non-exhaustive examples of polypropylene-rich recycled materials include: PP (Mtm Plastics GmbH), Polypropylene pellets (Axion Ltd) and polypropylene copolymer (BSP Compounds) were recycled.

[0184] During recycling, any reasonable measures are typically taken to reduce / remove any components other than polyethylene and polypropylene where the end application or use dictates such measures; however, other components are often present in small amounts.

[0185] Other such components include polystyrene (PS), polyamide (PA), polyethylene terephthalate (PET), all of which are present in as low an amount as possible, preferably below the detection limit.

[0186] The mixed plastic polypropylene blend (B) has a melt flow rate (MFR2) measured according to ISO 1133 at 230°C and 2.16 kg of 10.0 to 50 g / 10 min, more preferably 15 to 40 g / 10 min, most preferably 20 to 30 g / 10 min.

[0187] The mixed plastic polypropylene blend (B) preferably has an ethylene content (C2(total)) as determined by CRYSTEX QC analysis of 2.5 to 10.0 wt%, more preferably 3.0 to 9.0 wt%, most preferably 4.0 to 8.0 wt%.

[0188] The mixed plastic polypropylene blend (B) preferably has a soluble fraction (SF) content as measured by CRYSTEX QC analysis of 4.0 to 15.0 wt%, more preferably 6.0 to 14.0 wt%, most preferably 8.0 to 13.0 wt%.

[0189] The content of the crystalline fraction (CF) of the mixed plastic polypropylene blend (B) as determined according to CRYSTEX QC analysis is preferably in the range of 85.0 to 96.0 wt.-%, more preferably in the range of 86.0 to 94.0 wt.-%, most preferably in the range of 87.0 to 92.0 wt.-%.

[0190] The ethylene content of the soluble fraction (C2(SF)) of the mixed plastic polypropylene blend (B) as determined according to CRYSTEX QC analysis is preferably in the range of 20.0 to 50.0 wt.-%, more preferably in the range of 22.0 to 40.0 wt.-%, most preferably in the range of 24.0 to 35.0 wt.-%.

[0191] The ethylene content of the crystalline fraction (C2(CF)) of the mixed plastic polypropylene blend (B) as determined according to CRYSTEX QC analysis is preferably in the range of 1.0 to 8.0 wt.-%, more preferably in the range of 1.5 to 6.0 wt.-%, most preferably in the range of 2.0 to 4.0 wt.-%.

[0192] The intrinsic viscosity of the soluble fraction (iV(SF)) of the mixed plastic polypropylene blend (B) as determined according to CRYSTEX QC analysis is preferably in the range of 1.00 to 2.20 dL / g, more preferably in the range of 1.30 to 2.00 dL / g, most preferably in the range of 1.60 to 1.90 dL / g.

[0193] The intrinsic viscosity of the crystalline fraction (iV(CF)) of the mixed plastic polypropylene blend (B) as determined according to CRYSTEX QC analysis is preferably in the range of 1.00 to 2.20 dL / g, more preferably in the range of 1.20 to 2.00 dL / g, most preferably in the range of 1.40 to 1.70 dL / g.

[0194] The inorganic residue content of the mixed plastic polypropylene blend (B) as determined by calcination analysis according to DIN ISO 1172:1996 is preferably in the range of 0.05 to 5.0 wt.-%, more preferably in the range of 0.10 to 3.0 wt.-%, most preferably in the range of 0.50 to 2.0 wt.-%.

[0195] The mixed plastic polypropylene blend (B) is preferably derived from post-industrial waste or post-consumer waste, most preferably from post-consumer waste.

[0196] The limonene content of the mixed plastic polypropylene blend (B) as determined according to solid phase microextraction (HS-SPME-GC-MS) is preferably in the range of 0.10 to 25.0 ppm.

[0197] The presence of limonene indicates that the mixed plastic polypropylene blend (B) is derived from post-consumer waste.

[0198] Further characterisation of the recycling properties of the mixed plastic polypropylene blend (B) includes the presence of other polymers, such as polystyrene and polyamide-6, and the presence of fatty acids.

[0199] Accordingly, it is further preferred that the mixed plastic polypropylene blend (B) comprises one or more of polystyrene, polyamide-6 and fatty acids, preferably comprises each of polystyrene, polyamide-6 and fatty acids.

[0200] The mixed plastic polypropylene blend (B) has a density of 890 to 950 kg / m3, more preferably 900 to 940 kg / m3, most preferably 910 to 930 kg / m3, as measured according to ISO 1183-187. 3 The Charpy notched impact strength at 23 °C measured on the test bar is preferably 1.0 to 20.0 kJ / m2, more preferably 2.0 to 15.0 kJ / m2, most preferably 3.0 to 10.0 kJ / m2. 2 The Charpy notched impact strength at 23 °C measured on the test bar is preferably 1.0 to 20.0 kJ / m2, more preferably 2.0 to 15.0 kJ / m2, most preferably 3.0 to 10.0 kJ / m2. 2 The Charpy notched impact strength at 23 °C measured on the test bar is preferably 1.0 to 20.0 kJ / m2, more preferably 2.0 to 15.0 kJ / m2, most preferably 3.0 to 10.0 kJ / m2. 2 .

[0201] The mixed plastic polypropylene blend (B) has a flexural modulus of 1000 to 1600 MPa, more preferably 1100 to 1500 MPa, most preferably 1200 to 1400 MPa, as measured according to ISO 178 using ISO 19069-2 injection moulded 80 x 10 x 4 mm test bars. 3 The flexural modulus measured on the test bar is preferably 1000 to 1600 MPa, more preferably 1100 to 1500 MPa, most preferably 1200 to 1400 MPa.

[0202] The mixed plastic polypropylene blend (B) has a density of 890 to 950 kg / m3, more preferably 900 to 940 kg / m3, most preferably 910 to 930 kg / m3, as measured according to ISO 1183-187. 3 The flexural modulus measured on the test bar is preferably 1000 to 1600 MPa, more preferably 1100 to 1500 MPa, most preferably 1200 to 1400 MPa. 3 The flexural modulus measured on the test bar is preferably 1000 to 1600 MPa, more preferably 1100 to 1500 MPa, most preferably 1200 to 1400 MPa. 3 .

[0203] Ethylene-octene elastomer (EC)

[0204] The ethylene-octene elastomer (EC) is an elastomeric copolymer containing ethylene monomers and 1-octene comonomers.

[0205] The amount of ethylene-octene elastomer (EC) provided is 2.0 to 10.0 wt%, more preferably 5.0 to 10.0 wt%, most preferably 8.0 to 10.0 wt%, relative to the total weight of the polypropylene composition (PC).

[0206] The ethylene-octene elastomer (EC) has a melt flow rate (MFR2) of 2.0 to 20 g / 10 min, more preferably 5.0 to 15 g / 10 min, most preferably 7.0 to 13 g / 10 min, as measured according to ISO 1133 at 190 °C and 2.16 kg.

[0207] The density of the ethylene octene elastomer (EC) measured according to ISO 1183-187 is preferably from 870 to 900 kg / m 3 , more preferably 875 to 894 kg / m 3 , most preferably 880 to 888 kg / m 3 .

[0208] Inorganic filler (F)

[0209] The inorganic filler (F) is provided in an amount of 5.0 to 20.0 wt%, more preferably 9.0 to 18.0 wt%, most preferably 13.0 to 17.0 wt%, relative to the total weight of the polypropylene composition (PC).

[0210] D of inorganic filler L / D S The median diameter (d 50 ) and the median diameter (d 50 ) is from 1.5 to 4.5, more preferably from 1.8 to 4.0, most preferably from 2.0 to 3.5.

[0211] The median diameter (d) of the inorganic filler (F) was measured according to ISO 13320-1 (laser). 50 ) is preferably 3.0 to 10.0 μm, more preferably 4.0 to 8.5 μm, most preferably 4.5 to 7.0 μm.

[0212] Inorganic filler (F) top cut diameter (d 95 ) is preferably 8.0 to 30.0 μm, more preferably 9.0 to 25.0 μm, most preferably 10.0 to 20.0 μm.

[0213] The median diameter (d) of the inorganic filler (F) is measured according to ISO 13317-3 (sedimentation diagram). 50 ) is preferably 1.0 to 3.0 μm, more preferably 1.3 to 2.5 μm, most preferably 1.5 to 2.0 μm.

[0214] The top cut diameter (d) of the inorganic filler (F) is measured according to ISO 13317-3 (sedimentation diagram). 95 ) is preferably 4.0 to 10.0 μm, more preferably 4.5 to 9.0 μm, most preferably 5.0 to 8.0 μm.

[0215] Preferably, the inorganic filler is selected from talc, calcium carbonate, barium sulfate, mica and mixtures thereof.

[0216] Most preferably, the inorganic filler (F) is talc.

[0217] additives

[0218] The amount of the other additives (A) provided is 0.2 to 5.0 wt.%. The skilled person is able to select suitable additives known in the art.

[0219] The additives (A) are preferably selected from pigments, antioxidants, UV stabilizers, anti- scratch agents, mold release agents, acid scavengers, lubricants, antistatic agents, and mixtures thereof.

[0220] It is understood that the content of additives (A) includes any carrier polymer, i.e. masterbatch carrier polymer, used to introduce the additives into the polypropylene composition (PC) relative to the total weight of the polypropylene composition (PC). One example of such a carrier polymer is a polypropylene homopolymer in powder form.

[0221] articles

[0222] In another aspect, the present application relates to an article, preferably an injection molded article, comprising the polypropylene composition of the first aspect in an amount of at least 95 wt.%, more preferably at least 98 wt.%, most preferably at least 99 wt.%.

[0223] Preferably, the article, more preferably the injection molded article, is an automotive exterior article, more preferably selected from the group consisting of a bumper, a side trim, a running board, a body panel, and a spoiler.

[0224] Examples

[0225] 1. Measurement methods

[0226] The following terms definitions and determination methods apply to the general description of the application, including the claims, and the following examples, unless otherwise defined.

[0227] Quantification of the microstructure by NMR spectroscopy

[0228] Quantitative nuclear magnetic resonance (NMR) spectroscopy is employed to quantify the comonomer and regio-defect content of the polymers.

[0229] Quantitative 1 H and 13 C in solution state 13 C{ 1 H} NMR spectroscopy. The following pulse sequences were used: 13C Optimum 10 mm extended temperature probe recorded all spectra at 125 °C, all pneumatic devices used nitrogen. Approximately 200 mg of material was dissolved in approximately 3 mL of 1,2-tetrachloroethane-d2 (TCE-d2) along with chromium (III) acetylacetonate (Cr(acac)3) to form a 65 mM relaxant solution in solvent {singh09}. To ensure solution homogeneity, after initial sample preparation in the heating block, the NMR tube was further heated in a rotating constant temperature oven for at least 1 hour. The tube was inserted into the magnet with a 10 Hz spin rate. This setting was chosen primarily for the high resolution and quantitation required for accurate ethylene content quantitation. Standard single pulse excitation with no NOE was employed using an optimized tip angle, 1 second recycle delay, and a two-step WALTZ16 decoupling scheme {zhou07, busico07}. A total of 6144 (6k) transients were acquired per spectrum.

[0230] Quantitation 13 C{ 1 H}NMR spectra were processed and integrated using a proprietary computer program, and the relevant quantitative properties were determined from the integrals. All chemical shifts were indirectly referenced to the center methylene of the ethylene block (EEE) at 30.00 ppm using the chemical shift of the solvent. This approach allowed for a comparable reference even though this structural unit was not present.

[0231] Characteristic signals corresponding to ethylene incorporation were observed {wang00, cheng84, randall89}.

[0232] The comonomer fractions were quantitated by integrating multiple signals across the spectral region in the 13 C{ 1 H} spectrum using the method of Wang et al. {wang00}. This approach was chosen for its robustness and ability to account for the presence of regional imperfections when necessary. Minor adjustments to the integration region were made to improve applicability across the range of comonomer contents encountered.

[0233] For systems where only isolated ethylene was observed in the PPEPP sequence, the method of Wang et al. was modified to reduce the influence of non-zero integrals for sites known to be absent. This approach reduced the overestimation of ethylene content in such systems by reducing the number of sites used to determine the absolute ethylene content. By using this set of sites, the corresponding integral equation becomes:

[0234] p S = I A + (0.5 * I B )

[0235] p T = I D + IF +I D

[0236] p = (p S +p T ) / 2

[0237] e = 0.5 * (I H +(0.5 * I B )) fE = e / (e+p)

[0238] The same notation as used in the article of Wang et al. {wang00} is used.

[0239] The mole percent of comonomer incorporation is calculated from the mole fraction:

[0240] E [mol%] = 100 * fE

[0241] The weight percent of comonomer incorporation is calculated from the mole fraction:

[0242] E [wt%] = 100 * (fE * 28.06) / ((fE * 28.06) + ((1 - fE) * 42.08))

[0243] Characteristic signals corresponding to regio defects were observed {resconi00, wang00}. The presence of two methyl sites at 17.7 and 17.2 ppm indicated the presence of isolated 2,1-erythro regio defects and was confirmed by other characteristic sites. The presence of two inequivalent Sαβ signals at 34.9 and 34.7 ppm and a Tγγ signal at 34.1 ppm indicated the presence of 2,1-erythro regio defects adjacent to ethylene units.

[0244] The isolated 2,1-erythro regio defects (P 21e孤立 ) were quantified using the average integral of two characteristic methyl sites at 17.7 (I e8 ) and 17.4 (I e6 ) ppm, respectively:

[0245] P 21e孤立 = (I e6 + I e8 ) / 2

[0246] The 2,1 regio defects adjacent to ethylene (P E21 ) were quantified using the methine site at 34.1 ppm (I Tγγ ):

[0247] P E21 = I Tγγ

[0248] The total propylene (P总 ) Quantified through the methyl region between 23.0 and 19.9 ppm (I CH3 ) and corrected for sites within this region that are not related to propylene insertion. Methyl Pppresulting from 2,1 regio defects adjacent to ethylene already exist in I CH3 :

[0249] P 总 = I CH3 + 2*P 21e孤立

[0250] Multiply isolated 2,1-erythro regio defects (P 21e孤立 ) by 2 to account for the two (2) propylene units in a 2,1-erythro regio defect.

[0251] Quantify the mole percent of isolated 2,1-erythro regio defects relative to all propylene:

[0252] [21e] mol% = 100*P 21e孤立 / P 总

[0253] Quantify the mole percent of 2,1 regio defects adjacent to ethylene relative to all propylene:

[0254] [E21] mol% = 100*P E21 / P 总

[0255] Quantify the total amount of 2.1 defects as:

[0256]

[21] mol% = [21e] + [E21]

[0257] Characteristic signals corresponding to other types of regio defects (2,1-threo, 3,1 insertion) were not observed {resconi00}.

[0258] zhou07 Zhou, Z., Kuemmerle, R., Qiu, X., Redwine, D., Cong, R., Taha, A., Baugh, D. Winniford, B., J. Mag. Reson. 187 (2007) 225

[0259] busico07 Busico, V., Carbonniere, P., Cipullo, R., Pellecchia, R., Severn, J., Talarico, G., Macromol. Rapid Commun. 2007, 28, 1128

[0260] resconi00 Resconi, L., Cavallo, L., Fait, A., Piemontesi, F., Chem. Rev. 2000, 100, 1253

[0261] wang00 Wang, W-J., Zhu, S., Macromolecules 33 (2000), 1157

[0262] cheng84 Cheng, H.N., Macromolecules 17 (1984), 1950

[0263] singh09 Singh, G., Kothari, A., Gupta, V., Polymer Testing 28 5 (2009), 475

[0264] randall89 Randall, J. Macromol. Sci., Rev. Macromol. Chem. Phys. 1989, C29, 201.

[0265] CRYSTEX QC analysis

[0266] Crystalline fraction and soluble fraction method

[0267] The crystalline fraction (CF) and soluble fraction (SF) of the polypropylene (PP) composition, as well as the comonomer content and intrinsic viscosity of each fraction, were analyzed using a CRYSTEX instrument from Polymer Char (Valencia, Spain). Detailed information on the technique and method can be found in the literature (Ljiljana Jeremic, Andreas Albrecht, Martina Sandholzer & Markus Gahleitner (2020) Rapid characterization of high-impact ethylene-propylene copolymer composition by crystallization extraction separation: comparability to standard separation methods, International Journal of Polymer Analysis and Characterization, 25:8, 581-596).

[0268] The crystallized and amorphous fractions were separated by temperature cycling: dissolution at 160°C, crystallization at 40°C, and redissolution in 1,2,4-trichlorobenzene at 160°C. SF and CF were quantified and the ethylene content (C2) was determined by an integrated infrared detector (IR4), while the intrinsic viscosity (IV) was determined using an online double capillary viscometer.

[0269] The IR4 detector is a multi-wavelength detector that measures two different wavelength bands (CH3 stretching vibration (centered at about 2960 cm -1 ) and CH stretching vibration (2700-3000cm -1 )) is used to determine the concentration and ethylene content of ethylene-propylene copolymers. The IR4 detector is calibrated with a series of 8 EP copolymers with known ethylene contents ranging from 2 to 69 wt% (given by 13 C-NMR determination), the concentration of each copolymer ranged from 2 to 13 mg / mL. In order to simultaneously correct for both concentration and ethylene content (for the various polymer concentrations that may occur in the Crystex analysis), the following calibration equation was applied:

[0270] Concentration = a + b * absorbance (CH) + c * (absorbance (CH)) 2 +d*absorbance(CH3)+e*(absorbance(CH3) 2 +f*

[0271] Absorbance (CH) * Absorbance (CH3) (Equation 1)

[0272] CH3 / 1000C=a+b*absorbance(CH3)+c*absorbance(CH3)+d*(absorbance(CH3) / absorbance(CH3))+e

[0273] *(Absorbance (CH3) / Absorbance (CH)) 2 (Equation 2)

[0274] Constants a to e of Equation 1 and constants a to f of Equation 2 were determined by least squares regression analysis.

[0275] Use the following relationship to convert CH3 / 1000C to ethylene content (in wt%):

[0276] wt% (ethylene in EP copolymer) = 100 - CH3 / 1000TC*0.3 (Equation 3)

[0277] The amount of soluble fraction (SF) and crystalline fraction (CF) is related to the amount of "xylene cold soluble" (XCS) fraction and the amount of "xylene cold insoluble" (XCI) fraction measured according to the standard gravimetric method of ISO 16152 by means of an XS calibration curve. The XS calibration curve is realized by testing various EP copolymers with XS contents in the range of 2 to 31 wt%. The determined XS calibration curve is linear:

[0278] wt% XS = 1,01 * wt% SF (equation 4)

[0279] The inherent viscosities (IV) of the parent EP copolymer and its soluble fraction and crystalline fraction are determined using an online double capillary viscometer and are related to the corresponding iV measured according to ISO 1628-3 by standard method in decalin. Calibration is done with various EP PP copolymers with IV = 2-4 dL / g. The determined calibration curve is linear:

[0280] IV (dL / g) = a * Vsp / c (equation 5)

[0281] The sample to be analyzed is weighed at a concentration of 10 to 20 mg / ml. To avoid injection of gels and / or polymers (e.g. PET and PA) that can not be soluble in TCB at 160°C, the weighed sample is loaded into a stainless steel mesh with MW 0.077 / D 0.05 mm.

[0282] After automatic filling of the vials with 1,2,4-TCB containing 250 mg / l 2,6-tert-butyl-4-methylphenol (BHT) as antioxidant, the sample is dissolved at 160°C until complete dissolution, usually for 60 minutes, with continuous stirring at 400 rpm. To avoid sample degradation, the polymer solution is covered with a N2 atmosphere during the dissolution process.

[0283] A defined volume of the sample solution is injected into a column filled with an inert carrier, where the sample crystallizes and separation of the soluble fraction from the crystalline part takes place. This procedure is repeated twice. During the first injection, the whole sample is measured at high temperature, the IV [dl / g] and C2 [wt%] of the PP composition are determined. During the second injection, the soluble fraction (low temperature) and the crystalline fraction (high temperature) of the crystallization cycle as well as the crystallization period (wt% SF, wt% C2, IV) are measured.

[0284] Melt flow rate

[0285] Melt flow rate (MFR) is determined according to ISO 1133 in g / 10 min. MFR characterizes the flowability of a polymer and thus its processability. The higher the melt flow rate, the lower the viscosity of the polymer. MFR2 of polypropylene is determined at a temperature of 230 °C under a load of 2.16 kg.

[0286] Density:

[0287] Density was determined according to ISO 1183-187. Sample preparation was done by compression moulding according to ISO 1872-2:2007.

[0288] Xylene soluble fraction at room temperature (XCS, wt%): The amount of xylene cold soluble fraction was determined according to ISO 16152 (5th edition; 1 July 2005) at 25 °C.

[0289] DSC analysis: melting temperature (T m ) and heat of fusion (H f ), crystallization temperature (T c ) and heat of crystallization (H c ):

[0290] Determination was performed using a TA Instrument Q200 differential scanning calorimeter (DSC) on 5 to 7 mg samples. DSC was run according to ISO 11357 / Part 3 / Method C2 in a heat / cool / heat cycle with a scan rate of 10 °C / min in the temperature range of -30 to +225 °C. Crystallization temperature (T c ) and heat of crystallization (H c ) were determined from the cooling step, while melting temperature (T m ) and heat of fusion (H m ) were determined from the second heating step.

[0291] Flexural modulus was determined according to ISO 178 method A (3 point bending test) on specimens of 80 mm x 10 mm x 4 mm. According to the standard a test speed of 2 mm / min and a span length of 16 times the thickness were used. The testing temperature was 23 ± 2 °C. Injection moulding was performed according to ISO 19069-2, all materials used a melt temperature of 230 °C, independent of the material melt flow rate.

[0292] Notched Charpy impact strength (NIS)

[0293] Charpy notched impact strength (NIS) was determined according to ISO 1791 eA at +23 °C or -20 °C on 80 x 10 x 4 mm 3 injection moulded test bar specimens, all materials used a melt temperature of 230 °C, independent of the material melt flow rate.

[0294] Average particle size (diameter) d 50 and top cut diameter d 95

[0295] Particle size definition is calculated from the particle size distribution [mass percentage] measured according to two different methods:

[0296] Laser diffraction method using a Laser Mastersizer according to ISO 13320-1.

[0297] Sedimentation method i.e. gravity liquid sedimentation method according to ISO 13317-3.

[0298] d 50 defined as the median diameter, whereas d 95 is the diameter observed at the 95th percentile point from the particle size distribution.

[0299] Inorganic residue

[0300] Inorganic residue was quantitatively analyzed according to DIN ISO 1172:1996 using a Perkin Elmer TGA 8000. About 10-20 mg of material was placed into a platinum pan. The temperature was equilibrated at 50 °C for 10 minutes and then raised to 950 °C at a heating rate of 20 °C / min under nitrogen. The ash content was evaluated as weight-% at 850 °C.

[0301] Limonene detection

[0302] The determination of limonene is based on a static headspace (HS) method. This analysis combines the use of a HS sampler, a gas chromatograph (GC) and a mass spectrometer (MS) for screening.

[0303] Samples were delivered to the laboratory in sealed aluminized polyethylene (PE) bags. Prior to analysis, samples were frozen ground, 2.000 ± 0.100 g of sample was weighed into a 20 mL HS vial and sealed. Two determinations were performed per sample.

[0304] HS / GC / MS parameters

[0305] • HS parameters (Agilent G1888 headspace sampler)

[0306] Vial equilibration time: 120 minutes (sample), 5 minutes (standard)

[0307] Thermostat temperature: 100 °C (sample), 200 °C (standard)

[0308] Loop temperature: 110 °C (sample), 205 °C (standard)

[0309] Transfer line temperature: 120 °C (sample), 210 °C (standard)

[0310] Low oscillation

[0311] • GC parameters (Agilent 7890A GC system)

[0312] Column: ZB-WAX 7HG-G007-22 (30 m x 250 pm x 1 pm)

[0313] Carrier gas: Helium 5.0

[0314] Flow rate: 2 mL / min

[0315] Split: 5:1

[0316] GC oven program: 35 °C for 0.1 min

[0317] 10 °C / min until 250 °C

[0318] 250 °C for 1 min

[0319] • MS parameters (Agilent 5975C Inert XL MSD)

[0320] Acquisition mode: Scan

[0321] Scan parameters:

[0322] Low mass: 20

[0323] High mass: 200

[0324] Threshold: 10

[0325] • Software / data evaluation

[0326] MSD ChemStation E.02.02.1431

[0327] MassHunter GC / MS Acquisition Software B.07.05.2479

[0328] AMDIS GC / MS Analysis Software Version 2.71

[0329] NIST / EPA / NIH Mass Spectral Library (2011 version)

[0330] NIST Mass Spectral Search Program Version 2.0g

[0331] • AMDIS Deconvolution parameters

[0332] Minimum match factor: 80

[0333] Threshold: Low

[0334] Scan direction: High to Low

[0335] Data file format: Agilent file

[0336] Instrument Type: Quadrupole

[0337] Component Width: 20

[0338] Adjacent Peak Subtraction: 2

[0339] Resolution: High

[0340] Sensitivity: Very High

[0341] Peak Shape Requirement: Medium

[0342] Solvent Delay: 91 m / z

[0343] Column Bleed: 207 m / z

[0344] Minimum Model Peak: 2

[0345] Minimum S / N: 10

[0346] Minimum Specific Peak: 0.5

[0347] • MSD ChemStation Integration Parameters

[0348] Integrator: ChemStation

[0349] Initial Area Elimination: 0

[0350] Initial Peak Width: 0.005

[0351] Shoulder Detection: Off

[0352] Initial Threshold: 10.5

[0353] In this study, the expression "below the limit of detection (< LOD)" describes the cases where the matching factor is below 80 (AMDIS) or the signal-to-noise ratio of the peak in the sample run (Pk-pk S / N = corrected signal / Pk-pk noise, MSD ChemStation signal-to-noise report) is below 3. The results are only relevant to the measured sample, the measurement time and the application parameters.

[0354] Standard solution

[0355] To accurately identify and compare with the (lowest) odor detection threshold (ODT), a limonene standard was used.

[0356] In the HS / GC / MS analysis, 5 μΐ of the respective standard was injected into a 20 mL HS bottle, sealed and detected.

[0357] Assuming complete vaporization of the standard, the limonene concentration c in the HS G The estimates are shown in the following table.

[0358] Table 1 : Calibration standards and ODT

[0359] Analyte Solvent c G / mg m -3 ]]> Target ions (m / z) (minimum) ODT / mg m -3 [1]]]> Limonene 2-butanol 75 68 0.21

[0360] Data evaluation

[0361] Concentration c of analyte in HS G By considering the mass m of the substance G and the available volume V of the HS G The concentration c of the analyte in the HS above the polymer sample is calculated (eq. 1).

[0362]

[0363] For the estimation of the concentration of the analyte in the HS above the polymer sample, a single-point calibrated response factor Rf is required (eq. 2). The peak area of the analyte is obtained by integration of the extracted ion chromatogram (EIC). The corresponding target ions are listed in Table 1.

[0364]

[0365] Concentration of analyte in HS above polymer sample The concentration of the analyte in the HS above the polymer sample is calculated by multiplying the response factor with the EIC peak area of the sample (eq. 3).

[0366]

[0367] Furthermore, the odor relevance of the analyte in the HS above the polymer sample can be estimated by the odor activity value (OAV). Therefore, the concentration of the analyte in the HS above the polymer sample is compared to the (lowest) odor detection threshold (ODT) found in the literature (eq. 4) [1]. A value greater than 1 indicates that the analyte is relevant to the odor at the given HS temperature.

[0368]

[0369] Considerations and limitations

[0370] It has to be considered that the ODT of certain substances is below the limit of detection (LOD) of this method. Therefore, components below the LOD can be missed, although they are still relevant to the overall odor.

[0371] The OAV is based on the assumption that the HS parameters can be correlated to the measurement conditions of the ODT determination to some extent. This is of course not completely applicable, as such experiments do not necessarily choose a temperature setting of 100 °C, which has limited practical value. Nevertheless, this approach can at least indicate the relevance of defined marker substances to the odor.

[0372] References

[0373] [1] Van Gemert L.J., Odour Thresholds: Compilations of odour threshold values in air, water and other media, Utrecht, Oliemans Punter & Partners BV, 2011.

[0374] CLTE

[0375] The coefficient of linear thermal expansion (CLTE) is determined according to ISO 11359-2:1999 on 10 mm cubes cut from the same injection moulded test specimen as used for the determination of the flexural modulus. The measurements are carried out in the machine direction at a temperature range of -30 to +80 °C (heating rate 1 °C / min) and 23 to +80 °C (heating rate 1 °C / min), respectively.

[0376] Coating delamination

[0377] The paint adhesion is characterized as the resistance of the decorative coating (e.g. paint) when washed by a high pressure washer under the following specific conditions. Injection moulded plaques (150 mm x 80 mm x 3 mm) are prepared at a melt temperature of 240 °C and a mould temperature of 50 °C. The flow front velocity is 100 mm / s. Before coating, the plaques are washed with Zeller Gmelin mm / s for 5 minutes. Subsequently, the surface is activated by a flame treatment, wherein a burner sprays a mixture of propane (9 L / min) and air (180 L / min) at a 1 :20 ratio at a speed of 670 mm / s on the polymer substrate. After that, three layers are applied on the polymer substrate, i.e. a primer, a base coat (black) and a clear coat. The flame treatment step is performed twice.

[0378] Black paint test conditions

[0379] The decorative coating is cut into the substrate with a cutting tool (9 mm cutting knife) to a total depth of about 500 pm (including the coating and the substrate) resulting in a cross with branches of 100 mm and inclined at an angle of 30° to the substrate. On each coated substrate, 3 strips corresponding to the scribe lines of the cross are cut by hand. The cut area is further exposed to steam of hot water at a temperature T for a time t at a distance d from the surface of the test panel at an angle a. The pressure of the water jet depends on the water flow rate and is determined by the type of nozzle mounted at the end of the water pipe.

[0380] The following parameters are used:

[0381] T (water) = 68°C; t = 60 s; d = 130 mm, a = 90°, water pressure 68 bar, nozzle type = Walter 13 / 32.

[0382] Silver paint test conditions

[0383] The decorative coating is cut into the substrate with a cutting tool (1 mm Sikkens knife) to a total depth of about 130 pm (including coating and substrate) resulting in a cross with branches of 100 mm and inclined at an angle of 90° to the substrate. On each coated substrate, 3 strips of scribe lines corresponding to the cross are cut using an automated device. The cut area is further exposed to steam of hot water at a temperature T for a time t, at a spray distance d, at an angle a to the surface of the test panel. The pressure of the water jet depends on the water flow rate and is determined by the type of nozzle mounted at the end of the water pipe.

[0384] The following parameters are used:

[0385] T (water) = 68°C; t = 60 s; d = 130 mm, a = 90°, water pressure 68 bar, nozzle type = Walter 13 / 32.

[0386] The adhesion is evaluated by quantifying the area of coating failure or delamination (in mm 2 ) on each test scribe line in both cases. For each example, 5 panels (150 mm x 80 mm x 3 mm) are tested. For this purpose, images of the test scribe lines before and after water jet exposure are taken. Subsequently, the delamination area is calculated using image processing software. The average failure area of 3 test scribe lines on 5 test specimens, i.e. the average of a total of 15 test points, is reported as the average failure area. SD is the standard deviation, calculated according to the following formula:

[0387]

[0388] wherein:

[0389] x is the observation;

[0390] is the mean of the observations;

[0391] n is the number of observations.

[0392] 2. Example

[0393] 2.1. Synthesis of the heterophasic propylene-ethylene copolymer (HECO)

[0394] Preparation of the catalyst of HECO1 and HECO2

[0395] First, in a reactor at atmospheric pressure, 0.1 mol MgCl2 × 3EtOH is suspended in 250 mL decane under inert conditions. The solution is cooled to -15 ° C and 300 mL cold TiCl4 is added while the temperature is maintained at the level. The temperature of the slurry is then slowly raised to 20 ° C. At this temperature, 0.02 mol dioctyl phthalate (DOP) is added to the slurry. After adding the phthalate, the temperature is raised to 135 ° C over 90 minutes and the slurry is left to stand for 60 minutes. Then, another 300 mL TiCl4 is added and the temperature is maintained at 135 ° C for 120 minutes. Afterwards, the catalyst is filtered out from the liquid and washed six times with 300 mL heptane at 80 ° C. Then, the solid catalyst component is filtered and dried. Catalysts and their preparation concepts have been generally described in, for example, patent disclosures EP 491566, EP 591224 and EP 586390. The catalyst was further modified (VCH modification of the catalyst). Under inert conditions at room temperature, 35 ml of mineral oil (Paraffinum Liquidum PL68) was added to a 125 mL stainless steel reactor, followed by 0.82 g of triethylaluminum (TEAL) and 0.33 g of dicyclopentyldimethoxysilane (donor D). After 10 minutes, 5.0 g of the catalyst prepared above (Ti content 1.4 wt%) was added, followed by 5.0 g of vinylcyclohexane (VCH) after a further 20 minutes. The temperature was raised to +60°C over a period of 30 minutes and maintained at this temperature for 20 hours. Finally, the temperature was lowered to +20°C, and the oil / catalyst mixture was analyzed for the concentration of unreacted VCH, which was 200 ppm by weight.

[0396] Catalyst of HECO3

[0397] The catalyst used in the polymerization process is commercial ZN180M from Basell, wherein triethylaluminum (TEA) is used as a co-catalyst and dicyclopentyldimethoxysilane (donor D) is used as a donor.

[0398] Preparation of the catalyst of HECO4 and polymerization

[0399] For the polymerization process of HECO4, the Ziegler-Natta type catalyst used in the invention example of WO2016 / 066446A1 was used, and vinylcyclohexane was prepolymerized to achieve poly(vinylcyclohexane) nucleation.

[0400] EP 290256 B1 and EP 2960279 B1 describe in detail the nucleation process using vinylcyclohexane prepolymerization.

[0401] The above catalyst system was used in combination with triethylaluminum (TEAL) as cocatalyst and bis(cyclopentyl)dimethoxysilane (donor D) as external donor.

[0402] The subsequent polymerization was carried out under the following conditions.

[0403] Table 1 : Polymerization conditions for HECO

[0404]

[0405] The heterophasic copolymers HECO1, HECO2, HECO3 and HECO4 were compounded in a co-rotating twin-screw extruder Coperion ZSK 47 at 220 °C, adding 0.15 wt% of antioxidant (Irganox B215FF from BASF AG, Germany; this is a 1 :2 mixture of pentaerythritol tetrakis(3-(3',5'-di-tert-butyl-4-hydroxyphenyl)propionate (CAS No. 6683-19-8) and tris(2,4-di-tert-butylphenyl) phosphite (CAS No. 31570-04-4) and 0.05 wt% of calcium stearate (CAS No. 1592-23-0, commercially available from Faci, Italy).

[0406] 2.2. Mixed plastic polypropylene blend (B1 )

[0407] The mixed plastic polypropylene blend (B1 ) was taken from a post-consumer plastic waste stream in Germany, complying with the DSD324 specification standard. The raw material was provided in bale form, which was processed by un-baling and fed into a vibrating screen, separating oversized (> 400 mm) and undersized (< 30 mm) fractions, followed by a multi-stage sorting step based on NIR and color in a cascade of 4 Tomra Autosort devices. The high quality fraction consisting of white PP material was then fed into a hot caustic soda (minimum 0.5 wt% NaOH at 80 °C) washing line based on the design of Krones Metapure W, followed by mechanical drying, thermal drying, air separation, sieving (separation of material with size < 2 mm), two-step flake sorting using a Tomra Autosort Flake device, followed by extrusion. The properties of the mixed plastic polypropylene blend (B1 ) are listed in Table 2.

[0408] Table 2: Properties of the mixed plastic polypropylene blend (B1 )

[0409]

[0410] The mixed plastic polypropylene blend (B1 ) further contained traces of polystyrene, polyamide-6 and fatty acids.

[0411] 2.3. Compounding of inventive and comparative compositions

[0412] The inventive and comparative compositions were prepared by compounding in a co-rotating twin-screw extruder Coperion ZSK 40 at 220 °C according to the formulations shown in Table 3.

[0413] In addition to the HECO and the mixed plastic polypropylene blend described above, the following commercially available components were used: EC1 elastomeric ethylene-octene copolymer, trade name Queo 8210, available from Borealis,

[0414] MFR2(190 °C) of 10 g / 10 min, density of 883 kg / m 3

[0415] EC2 elastomeric ethylene-butene copolymer, trade name Engage HM 7487, available from Dow Chemicals

[0416] MFR2(190 °C) of 0.27 g / 10 min, density of 860 kg / m 3 .

[0417] EC3 elastomeric ethylene-octene copolymer, trade name Engage 8842, available from Dow Chemicals (USA), MFR2(190 °C) of 1.0 g / 10 min, density of 857 kg / m

[0418] 3 .

[0419] h-PP commercially available propylene homopolymer HL712FB, available from Borealis (Austria), MFR2(230 °C) of 1200 g / 10 min, T

[0420] m .

[0421] F1 talc, trade name Steamic T1 CA, available from Imerys (France), median diameter d 50 of 1.8 pm, top cut diameter d 95 of 6.2 pm; median diameter d 50 of 6.0 pm, top cut diameter d 95 of 14.7 pm, D L / D S of 3.33.

[0422] F2 talc, trade name Jetfine 3CA, available from Imerys (France), median diameter d 50 ​​of 1.3 pm, top cut diameter d 95 of 3.9 pm; median diameter d 50 of 4.4 pm, top cut diameter d 95 of 9.9

[0423] pm, D L / D S of 3.38.

[0424] F3 talc, trade name Luzenac HAR T84, from Imerys (France), median diameter d 50 of 2.0 pm, top cut diameter d 95 of 11.3 pm;

[0425] median diameter d 50 of 10.5 pm, top cut diameter d 95 of 34.2 pm, D L / D S of 5.25.

[0426] Black MB polyethylene-based masterbatch CBMBLD-09A02 from Borealis Norge AS (Norway). Its pigment content

[0427] is 40 wt%.

[0428] MB carrier masterbatch carrier propylene homopolymer, trade name HC001 A, from Borealis AG (Austria).

[0429] SA1 slip agent, trade name Finawax-O, from Fine Organics (India).

[0430] SA2 oleamide slip agent, trade name Crodamide OR (CAS number: 301-02-0), from Croda Polymer Additives (UK).

[0431] Croda Polymer Additives (UK).

[0432] GMS glycerol monostearate, trade name GMS-90, from Sabo S.p.A (Italy). AO1 antioxidant, trade name Irganox 1010 (CAS number: 6683-19-8), from BASF

[0433] AG (Germany).

[0434] AO2 antioxidant, trade name Irganox 1076 (CAS No. 2082-79-3), available from BASF

[0435] AG (Germany).

[0436] UV1 UV stabilizer, trade name Chimasorb 119, available from BASF AG (Germany).

[0437] Properties of the inventive compositions and comparative compositions are listed in Table 4.

[0438] Table 3: Formulation of inventive examples and comparative examples

[0439]

[0440] CE1 and CE2 correspond to IE1 and IE2 of WO 2022 / 034127 A1, respectively, while CE3 to CE6 correspond to IE1 to IE4 of WO 2022 / 258578 A1, respectively.

[0441] Table 4: Properties of inventive compositions and comparative compositions

[0442]

[0443] *- n.m. = not measured

[0444] As can be seen from Table 4, the paint adhesion of inventive example IE1 (containing HECO1, HECO2, EC1, F1 and B1 as well as pigments / other additives) is significantly improved, with no delamination observed for either the black or silver paint. Moreover, the mechanical properties remain at a good level despite the lower content of elastomer component used in IE1, with the notched impact strength even slightly improved over CE1 to CE6.

Claims

1. A polypropylene composition (PC) which is a mixed plastic polypropylene blend, wherein, The polypropylene composition (PC) has: a) a melt flow rate (MFR2) of 1.0 to 30.0 g / 10 min measured according to ISO 1133 at 230 °C and 2.16 kg; b) a silver paint delamination area of 0.0 to 20.0 mm2measured according to the method defined in the test method 2 ; c) a black paint delamination area of 0.0 to 20.0 mm2measured according to the method defined in the test method 2 ; d) 80 x 10 x 4 mm injection moulded according to ISO 178 using ISO 19069-2 3 The flexural modulus measured on the test bar is 1000 to 2000 MPa; e) a limonene content of 0.10 to 25.0 ppm measured according to solid phase microextraction (HS-SPME-GC-MS); and f) the content of inorganic filler (F) is 5.0 to 20.0 wt.-%, relative to the total weight of the polypropylene composition (PC), the inorganic filler (F) having a ratio D 50 / D 50 value of 1.5 to 4.5, the ratio of the median diameter (d L ) measured according to ISO 13320-1 (laser) to the median diameter (d S ) measured according to ISO 13317-3 (sedigraph) of 1.5 to 4.5; The polymer fraction of the polypropylene composition (PC) has a soluble fraction (SF) content of 20.0 to 30.0 wt% measured according to CRYSTEX QC analysis, the polymer fraction of the polypropylene composition (PC) has a crystalline fraction (CF) content of 70.0 to 80.0 wt% measured according to CRYSTEX QC analysis, both contents are expressed as wt% relative to the total weight of the polymer fraction of the polypropylene composition (PC), the inherent viscosity of the soluble fraction (iV(SF)) measured according to CRYSTEX QC analysis is 2.40 to 3.50 dL / g, the ethylene content of the crystalline fraction (C2(CF)) measured according to CRYSTEX QC analysis is 4.0 to 10.0 wt%.

2. The polypropylene composition (PC) according to claim 1, wherein: the inherent viscosity of the crystalline fraction (iV(CF)) of the polymer fraction of the polypropylene composition (PC) measured according to CRYSTEX QC analysis is 1.00 to 2.50 dL / g; and / or the ratio of the inherent viscosities of the soluble fraction and the crystalline fraction (iV(SF) / iV(CF)) measured according to CRYSTEX QC analysis is 1.00 to 3.

00.

3. The polypropylene composition (PC) according to claim 1 or 2, wherein the ethylene content of the soluble fraction (C2(SF)) measured according to CRYSTEX QC analysis is 30.0 to 60.0 wt%, and / or the ratio of the ethylene contents of the soluble fraction and the crystalline fraction (C2(SF) / C2(CF)) measured according to CRYSTEX QC analysis is 6.0 to 12.

0.

4. The polypropylene composition (PC) according to any one of the preceding claims, wherein, the ethylene content (C2(total)) of the polypropylene composition (PC) measured according to CRYSTEX QC analysis is 10.0 to 30.0 wt%.

5. The polypropylene composition (PC) according to any one of the preceding claims, wherein, The polypropylene composition (PC) has one or more, preferably all, of the following properties: a) Charpy notched impact strength at 23°C of 40 to 100 kJ / m measured on 80 x 10 x 4 mm specimens injection moulded in accordance with ISO 19069-2 using ISO 179 3 a Charpy notched impact strength at 23°C of 40 to 100 kJ / m measured on 80 x 10 x 4 mm specimens injection moulded in accordance with ISO 19069-2 using ISO 179 2 ; b) Charpy notched impact strength at -20°C of 3.0 to 15 kJ / m measured on test bars according to ISO 179 using ISO 19069-2 compliant injection moulded 80x10x4 mm 3 Charpy notched impact strength at -20°C of 3.0 to 15 kJ / m measured on test bars according to ISO 179 using ISO 19069-2 compliant injection moulded 80x10x4 mm 2 ; and c) a coefficient of longitudinal linear thermal expansion (CLTE) of 0 to 100 x 10 -6 / K, measured according to ISO 11359-2.

6. The polypropylene composition (PC) according to any one of the preceding claims, wherein, The inorganic filler (F) is talc, more preferably having one or more, preferably all, of the following properties: a) a median diameter (d 50 ) of 3.0 to 10.0 pm measured according to ISO 13320-1 (laser); b) a top cut diameter (d 95 ) of 8.0 to 30.0 pm measured according to ISO 13320-1 (laser); c) a median diameter (d 50 ) of 1.0 to 3.0 pm measured according to ISO 13317-3 (sedigraph); and d) a top cut diameter (d 95 ) of 4.0 to 10.0 pm, measured according to ISO 13317-3 (sedigraph).

7. The polypropylene composition (PC) according to any one of the preceding claims, wherein, The polypropylene composition (PC) is obtainable by blending at least the following components a) to f): a) 30.0 to 50.0 wt% of a first heterophasic propylene-ethylene copolymer (HECO1) relative to the total weight of the polypropylene composition (PC), the first heterophasic propylene-ethylene copolymer (HECO1) has an ethylene content (C2(total)) of 8.1 to 20.0 wt% measured according to CRYSTEX QC analysis; b) 5.0 to 15.0 wt% of a second heterophasic propylene-ethylene copolymer (HECO2) having an ethylene content (C2(total)) of 3.0 to 8.0 wt% as determined by CRYSTEX QC analysis, relative to the total weight of the polypropylene composition (PC); c) 20.0 to 30.0 wt% of a mixed plastic polypropylene blend (B) having a melt flow rate (MFR2) of 10 to 50 g / 10 min as determined by ISO 1133 at 230 °C and 2.16 kg, relative to the total weight of the polypropylene composition (PC); d) 2.0 to 10.0 wt% of an ethylene-octene elastomer (EC); e) 5.0 to 20.0 wt% of an inorganic filler (F); f) 0.2 to 5.0 wt% of further additives (A); The total content of components a) to f) amounts to at least 95 wt%, more preferably at least 98 wt%, most preferably 100 wt%, relative to the total weight of the polypropylene composition (PC).

8. The polypropylene composition (PC) according to claim 7, wherein The first heterophasic propylene-ethylene copolymer (HECO1) has one or more, preferably all, of the following properties: a) a melt flow rate (MFR2) of 1.0 to 50 g / 10 min as determined by ISO 1133 at 230 °C and 2.16 kg; b) a soluble fraction (SF) content of 20.0 to 40.0 wt% as determined by CRYSTEX QC analysis and a crystalline fraction (CF) content of 60.0 to 80.0 wt% as determined by CRYSTEX QC analysis; c) an ethylene content of the soluble fraction (C2(SF)) of 25 to 45 wt% as determined by CRYSTEX QC analysis; d) an ethylene content of the crystalline fraction (C2(CF)) of 1.0 to 8.0 wt% as determined by CRYSTEX QC analysis; e) an intrinsic viscosity of the soluble fraction (iV(SF)) of 2.00 to 4.00 dL / g as determined by CRYSTEX QC analysis; f) an intrinsic viscosity of the crystalline fraction (iV(CF)) of 1.10 to 2.00 dL / g as determined by CRYSTEX QC analysis; and g) an intrinsic viscosity ratio (iV(SF) / iV(CF)) of 1.20 to 4.00 as determined by CRYSTEX QC analysis.

9. The polypropylene composition (PC) according to claim 7 or 8, wherein The second heterophasic propylene-ethylene copolymer (HECO2) has one or more, preferably all, of the following properties: a) a melt flow rate (MFR2) of 1.0 to 15.0 g / 10 min as determined by ISO 1133 at 230 °C and 2.16 kg; b) a soluble fraction (SF) content of 10.0 to 30.0 wt% as determined by CRYSTEX QC analysis and a crystalline fraction (CF) content of 70.0 to 90.0 wt% as determined by CRYSTEX QC analysis; c) the soluble fraction has an ethylene content (C2(SF)) of 10 to 30 wt% as determined by CRYSTEX QC analysis; d) the crystalline fraction has an ethylene content (C2(CF)) of 0.0 to 5.0 wt% as determined by CRYSTEX QC analysis; e) the soluble fraction has an intrinsic viscosity (iV(SF)) of 3.00 to 7.00 dL / g as determined by CRYSTEX QC analysis; f) the crystalline fraction has an intrinsic viscosity (iV(CF)) of 1.40 to 2.70 dL / g as determined by CRYSTEX QC analysis; and g) the intrinsic viscosity ratio (iV(SF) / iV(CF)) is 2.00 to 5.00 as determined by CRYSTEX QC analysis.

10. The polypropylene composition (PC) according to any one of claims 7 to 9, wherein The ethylene-octene elastomer (EC) has a melt flow rate (MFR2) measured according to ISO 1133 at 190 °C and 2.16 kg of 2.0 to 20 g / 10 min, and / or a density measured according to ISO 1183-187 of 870 to 900 kg / m3 3 .

11. The polypropylene composition (PC) according to any one of claims 7 to 10, wherein The mixed plastic polypropylene blend (B) has one or more, preferably all of the following properties: a) an ethylene content (C2(total)) of 2.5 to 10.0 wt% as determined by CRYSTEX QC analysis; b) a soluble fraction (SF) content of 4.0 to 15.0 wt% and a crystalline fraction (CF) of 85.0 to 96.0 wt%, both as determined by CRYSTEX QC analysis; c) the crystalline fraction has an ethylene content (C2(CF)) of 1.0 to 8.0 wt% as determined by CRYSTEX QC analysis; d) the soluble fraction has an ethylene content (C2(SF)) of 20 to 50 wt% as determined by CRYSTEX QC analysis; e) the crystalline fraction has an intrinsic viscosity (iV(CF)) of 1.00 to 2.20 dL / g as determined by CRYSTEX QC analysis; f) the soluble fraction has an intrinsic viscosity (iV(SF)) of 1.00 to 2.20 dL / g as determined by CRYSTEX QC analysis; g) an inorganic residue content of 0.05 to 5.0 wt% as determined by calcination analysis according to DIN ISO 1172:1996; h) a limonene content of 0.10 to 25.0 ppm as determined by solid phase microextraction (HS-SPME-GC-MS); and i) a density of 890 to 950 kg / m3measured according to ISO 1183-187 3 .

12. The polypropylene composition (PC) according to any one of claims 7 to 11, wherein The mixed plastic polypropylene blend (B) has: a) Charpy notched impact strength at 23 °C of 1.0 to 20.0 kJ / m2measured on a test bar of 80 x 10 x 4 mm injection moulded according to ISO 179 using ISO 19069-2 compliant 3 ; and / or 2 ; and / or b) 80 x 10 x 4 mm injection moulded according to ISO 19069-2 using ISO 178 3 The flexural modulus of the test bars was measured to be 1000 to 1600 MPa.

13. The polypropylene composition (PC) according to any one of claims 7 to 12, wherein The mixed plastic polypropylene blend (B) is derived from post-consumer waste.

14. The polypropylene composition (PC) according to any one of claims 7 to 13, wherein, The mixed plastic polypropylene blend (B) comprises one or more of polystyrene, polyamide-6 and fatty acids.

15. An article, preferably an injection molded article, comprising the polypropylene composition of any of the preceding claims in an amount of at least 95 wt%, more preferably at least 98 wt%, most preferably at least 99 wt%.

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