Polyolefin composition comprising polypropylene homopolymer, polypropylene block copolymer and recycled plastic material

Abstract

The present invention relates to a polyolefin composition comprising a) from 5% to 30% by weight (based on the total weight of the polyolefin composition) of at least one polypropylene homopolymer, b) from 1% to 15% by weight (based on the total weight of the polyolefin composition) of at least one polypropylene block copolymer, c) from 20% to 50% by weight (based on the total weight of the polyolefin composition) of a mixed plastic polypropylene blend of recycled materials, d) from 35% to 55% by weight (based on the total weight of the polyolefin composition) of glass fibers; and optionally further additives wherein the sum of all the ingredients is always 100% by weight wherein the polyolefin composition has a tensile modulus at 23 DEG C (ISO 527-2) of at least 7000 MPa, a yield tensile stress at 23 DEG C (ISO 527-2) of at least 90 MPa and an impact strength (ISO 179-1, Charpy 1 eA + 23 DEG C) of at least 8.5 kJ / m2.

Description

[0001] The present invention relates to a polyolefin composition comprising at least one polypropylene homopolymer, at least one polypropylene block copolymer and recycled plastic material and an article comprising the polyolefin composition.

[0002] describe

[0003] Polyolefins, particularly polyethylene and polypropylene, are increasingly consumed in large quantities in a wide range of applications, including packaging for food and other items, fibers, automotive components, and a wide variety of manufactured articles. Polyethylene-based materials are a particular problem because these materials are widely used for packaging. Given the large amount of waste collected compared to the amount of waste recycled back into the stream, there remains great potential for intelligent reuse of plastic waste streams and mechanical recycling of plastic waste.

[0004] Typically, a large amount of polypropylene recycled on the market is a mixture of polypropylene (PP) and polyethylene (PE), which is especially true for post-consumer waste streams. In addition, commercial recyclates from post-consumer waste sources are routinely cross-contaminated with non-polyolefin materials (e.g., polyethylene terephthalate, polyamide, polystyrene) or non-polymer substances (such as wood, paper, glass or aluminum). These cross-contaminations greatly limit the final application of the recycling stream, leaving no useful end use. Polyolefin recycling materials (especially from post-consumer waste streams) are a mixture of PE and PP. The better the quality of the recyclate, the less available it is, and the more expensive it is.

[0005] Consumers seeking recyclates require similar stiffness-impact strength as virgin materials. This is also valid for reinforced glass fiber compounds used in structural products. The quality issues of recyclates compared to virgin materials can be overcome to some extent by reinforcing recyclates, where the reinforcing particles physically bind the different domains (PP and PE).

[0006] Compositions comprising virgin polymers (ie polymers used for the first time) and recycled mixed plastics were studied.

[0007] WO 2014167493 A1 describes a method for preparing a polyolefin mixture, comprising the step (a) of mixing together a base polymer mixture MB and a polymer mixture MPR, wherein the mixture MPR is obtained from recycling of post-consumer plastic materials.

[0008] Recycled mixed plastics reinforced with glass fibre (GF) have also been investigated, for example recycled PP or PP / PE blends reinforced with GF or mixed GF with other fillers.

[0009] EP 2845876 B1 describes a composition comprising two or more resins and glass fibers, comprising: a resin mixture containing waste polyethylene (PE) and waste polypropylene (PP); long glass fibers having a length of 10 mm or more; and a rubber-based resin, wherein based on 100 parts by weight of the resin mixture, the composition comprises 3 to 30 parts by weight of the long glass fibers, 10 to 50 parts by weight of the rubber-based resin, and 10 to 35 parts by weight of LDPE.

[0010] EP 3406662 A1 describes a structurally reinforced plastic composite product produced with recycled waste glass fibers and recycled polymer compounds and a method for making the same. The reinforced composite product comprises: recycled fiber glass collected from a waste stream and used as a filler, the recycled fiber glass being 30% to 70% of the total weight of the reinforced composite product; a colorant, the colorant being 1% to 2% of the total weight of the reinforced composite product; and a recycled resin collected from a waste stream and substantially wetted with recycled glass fibers by a black colorant and a chemical binder. The recycled resin comprises at least one of high-density polyethylene (HDPE), polypropylene (PP), or an engineering grade resin.

[0011] WO2018086959 A1 relates to a polyolefin composition and product containing glass fiber filler, which comprises a native homopolymer and a copolymer; 5 wt % to 30 wt % of a glass fiber filler; and a compatibilizer.

[0012] Bajracharya et al. (Experimental and theoretical studies on the properties of injection moulded glass fibre reinforced mixed plastics composites. Composites Part A: Applied Science and Manufacturing, 2016, 84: 393-405) and Bajracharya et al. (Durability characteristics and property prediction of glassfibre reinforced mixed plastics composites. Composites Part B: Engineering, 2017, 116: 16-29) used PE / PP recyclates in the form of flakes collected from post-consumer plastic waste and post-industrial plastic waste by Repeat Plastics (Replas) Pty of Australia. The tensile modulus of the recyclate was 906MPa. It was reinforced with 10% GF, 20% GF and 30% GF (length of 4.0mm and diameter of 13.7μm). The maximum tensile modulus of 3068MPa was achieved by 30% GF.

[0013] Thus, there are examples of reinforced recyclates with good tensile modulus and impact strength at the same time. However, it would be advantageous to provide polyolefin compositions with similar properties to virgin polymers but also containing post-consumer recyclate (PCR) to make the final solution more economically friendly in terms of CO2 footprint.

[0014] It is therefore an object of the present invention to provide a polyolefin composition comprising a blend of virgin polymer and polyolefin material recycled from waste plastic material having an improved stiffness-impact strength balance and high tensile strength.

[0015] This object is achieved by providing a polyolefin composition comprising:

[0016] a) 5 to 30 wt. % (based on the total weight of the polyolefin composition) of at least one polypropylene homopolymer,

[0017] b) 1 to 15 wt. % (based on the total weight of the polyolefin composition) of at least one polypropylene block copolymer,

[0018] c) 20 wt% to 50 wt% (based on the total weight of the polyolefin composition) of a mixed plastic polypropylene blend of recycled material, the mixed plastic polypropylene blend having:

[0019] (i) a crystalline fraction (CF) content determined according to CRYSTEX QC analysis in the range of 85.0 wt.-% to 95.0 wt.-%, and

[0020] (ii) a soluble fraction (SF) content determined according to CRYSTEX QC analysis in the range of 5.0 wt.-% to 15.0 wt.-%, wherein

[0021] (iii) The crystalline fraction (CF) is quantitatively 13 The propylene content (C3(CF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is in the range of 93.0 wt. % to 99.0 wt. %, and wherein

[0022] (iv) The crystalline fraction (CF) is determined by quantitative 13 An ethylene content (C2(CF)) in the range of 1.0 wt% to 6.0 wt% as determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy; and

[0023] (v) the intrinsic viscosity (iV(SF)) of the soluble fraction (SF) is in the range of 1.0 dl / g to 2.0 dl / g, and

[0024] in

[0025] (vi) The CIELAB color space (L*a*b*) of the mixed plastic polypropylene blend is:

[0026] -L* of 30 to 97.0, especially 50 to 97.0;

[0027] --a* from 10.0 to 16.0, especially from -8 to <10.0;

[0028] -- b* of 5.0 to 25.0, especially -2 to 22.0;

[0029] d) 35 to 55 wt. % (based on the total weight of the polyolefin composition) of glass fibers;

[0030] and optionally further additives, wherein the sum of all constituents always amounts to 100% by weight,

[0031] The polyolefin composition has:

[0032] - a tensile modulus at 23°C of at least 7000 MPa (ISO 527-2),

[0033] - a tensile stress at yield at 23°C of at least 90 MPa (ISO 527-2), and

[0034] - At least 8.5 kJ / m 2 Impact strength (ISO179-1, Charpy 1eA+23℃).

[0035] Therefore, high quality polypropylene recyclate is blended with virgin polypropylene homopolymer, virgin polypropylene block copolymer and glass fibers to obtain a polyolefin composition having excellent mechanical properties, in particular, excellent tensile strength and tensile stiffness while keeping the properties of the final composition comparable to virgin polymer.

[0036] The composition comprising recyclate of the present invention is characterized in that high tensile modulus is combined with high tensile stress. The performance of the combination of different types of polymers and recyclate with glass fiber reinforcement is not easy to predict. Due to the interaction between different components, it is particularly difficult to predict tensile modulus and tensile stress. In addition, recyclate polyolefins are usually polluted by polar polymers (for example, PA, PET) or other non-polar polymers (non-PO) (for example PS or filler), which makes the clear calculation of final mechanical properties more difficult.

[0037] The term "virgin" refers to newly produced materials and / or objects prior to first use and not recycled. In the absence of explicit reference to the origin of a polymer, the polymer is a "virgin" polymer.

[0038] For the purposes of this specification and the appended claims, the term "recycled" is used to denote the recovery of materials from post-consumer waste and / or industrial waste. That is, post-consumer waste refers to objects that have completed at least the first use cycle (or life cycle), i.e., have served their first purpose and have passed through the hands of consumers; while industrial waste refers to manufacturing waste that does not usually reach consumers. In the subject matter of the present invention, "recycled polymer" may also contain up to 17% by weight, preferably up to 3% by weight, more preferably up to 1% by weight, and even more preferably up to 0.1% by weight of other components derived from the first use, based on the total weight of the recycled polymer. The type and amount of these components affect the physical properties of the recycled polymer. The physical properties given below relate to the main components of the recycled polymer.

[0039] Mixed plastics are defined as the presence of small amounts of compounds not normally present in virgin polypropylene blends, such as polystyrene, polyamide, polyester, wood, paper, limonene, aldehydes, ketones, fatty acids, metals, and / or long term decomposition products of stabilizers. Virgin polypropylene blends refer to blends that originate directly from the production process without intermediate use. As a matter of definition, "mixed plastics" may be equivalent to detectable amounts of polystyrene and / or polyamide-6 and / or limonene and / or fatty acids.

[0040] According to the present invention, the total amount of all virgin polypropylene homopolymers used in the polyolefin composition of the present invention adds up in the range of 5 to 30 wt.-%, preferably 8 to 25 wt.-%, more preferably 9 to 22 wt.-% (based on the total weight of the polyolefin composition).

[0041] According to the present invention, the total amount of all virgin polypropylene block copolymers used in the polyolefin composition of the present invention adds up in the range of 1 wt.-% to 15 wt.-%, preferably 3 wt.-% to 10 wt.-%, more preferably 4 wt.-% to 8 wt.-% (based on the total weight of the polyolefin composition).

[0042] According to the present invention, the amount of mixed plastic polypropylene blend, preferably recycled from waste plastic material originating from post-consumer waste and / or post-industrial waste, used in the polyolefin composition of the present invention is in the range of 20 wt.-% to 50 wt.-%, preferably 25 wt.-% to 45 wt.-%, more preferably 30 wt.-% to 42 wt.-% (based on the total weight of the polyolefin composition).

[0043] According to the present invention, the amount of glass fiber used in the polyolefin composition of the present invention is in the range of 35 to 55 wt%, preferably 38 to 50 wt%, more preferably 38 to 45 wt% (based on the total weight of the polyolefin composition).

[0044] It is to be understood that further additives may also be included in the polyolefin composition and that in the various embodiments described herein, the sum of all ingredients always totals 100 weight percent.

[0045] According to one embodiment, the polyolefin composition of the present invention comprises:

[0046] a) 8 to 28 wt.-%, more preferably 9 to 22 wt.-% (based on the total weight of the polyolefin composition) of at least one polypropylene homopolymer,

[0047] b) 3 to 10 wt.-%, more preferably 4 to 8 wt.-%, based on the total weight of the polyolefin composition, of at least one polypropylene block copolymer,

[0048] c) 25 to 45 wt. %, more preferably 30 to 42 wt. % (based on the total weight of the polyolefin composition) of a mixed plastic polypropylene blend;

[0049] d) 38 to 50 wt. %, preferably 38 to 45 wt. % (based on the total weight of the polyolefin composition) of glass fibers;

[0050] and optionally further additives, wherein the sum of all ingredients adds up to 100% by weight.

[0051] In one embodiment, the polyolefin composition of the present invention is also characterized in that the melt flow rate MFR2 (ISO1133, 2.16 kg, 230°C) is at least 3.0 g / 10 min, preferably at least 3.5 g / 10 min, more preferably at least 4.0 g / 10 min, in particular in the range of 3.0 g / 10 min to 15 g / 10 min, preferably 3.5 g / 10 min to 10 g / 10 min, more preferably 4.0 g / 10 min to 10 g / 10 min.

[0052] In another embodiment, the polyolefin composition of the present invention is characterized by a tensile modulus (ISO 527-2) of at least 8000 MPa, preferably at least 8500 MPa, more preferably at least 9000 MPa, in particular in the range of 8000 MPa to 15000 MPa, more in particular in the range of 8000 MPa to 10000 MPa.

[0053] In another embodiment, the polyolefin composition of the present invention has a tensile stress at yield (50 mm / min, ISO 527-2) at 23°C of at least 95 MPa, preferably at least 100 MPa, more preferably at least 105 MPa, in particular in the range of 90 MPa to 200 MPa, more in particular in the range of 100 MPa to 150 MPa.

[0054] In yet another embodiment, the polyolefin composition of the present invention has a tensile stress at break (50 mm / min, ISO 527-2) at 23°C of at least 90 MPa, preferably at least 95 MPa, more preferably at least 100 MPa, even more preferably at least 105 MPa, in particular in the range of 90 MPa to 200 MPa, more in particular in the range of 100 MPa to 150 MPa.

[0055] In yet another embodiment, the impact strength (ISO 179-1, Charpy 1eA+23°C) of the polyolefin composition of the present invention is at least 9.0 kJ / m 2 , preferably at least 9.5 kJ / m 2 , especially at 9.0 kJ / m2 Up to 15.0kJ / m 2 in the range of 9.5 kJ / m 2 Up to 13.0 kJ / m 2 in the range of 10 kJ / m 2 Up to 12.0 kJ / m 2 within the range.

[0056] Polypropylene virgin homopolymer

[0057] In one embodiment of the polyolefin composition of the present invention, more than one virgin polypropylene homopolymer may be used. However, preferably one virgin polypropylene homopolymer is used.

[0058] Thus, in one embodiment, the polyolefin composition of the present invention may comprise:

[0059] a1) at least one first polypropylene homopolymer;

[0060] a2) at least one second polypropylene homopolymer;

[0061] Wherein the at least one first polypropylene homopolymer and the at least one second polypropylene homopolymer differ from each other in their melt flow rate MFR2 (230° C., 2.16 kg load, measured according to ISO 1133).

[0062] Thus, the polyolefin composition of the present invention may comprise two virgin polypropylene homopolymers having different melt flow rates. This allows for easy adjustment of the melt flow rate of the final polyolefin composition.

[0063] The polypropylene homopolymer used as the virgin homopolymer in the polyolefin composition of the present invention is selected from the group comprising:

[0064] a polypropylene homopolymer (PPH-1) having a melt flow rate MFR2 (230°C, 2.16 kg, measured according to ISO 1133) in the range of 5 to 15 g / 10 min, preferably in the range of 5 to 10 g / 10 min, more preferably 8 g / 10 min; and / or

[0065] A polypropylene homopolymer (PPH-2) having a melt flow rate MFR2 (230°C, 2.16 kg, measured according to ISO 1133) in the range of 10 to 30 g / 10 min, preferably 15 to 25 g / 10 min, more preferably 20 g / 10 min.

[0066] The following describes the properties and characteristics of different polypropylene homopolymers that can be used in the polyolefin composition of the present invention.

[0067] Polypropylene homopolymer (PPH-1):

[0068] The at least one polypropylene homopolymer (PPH-1) has a melt flow rate MFR2 (230°C, 2.16 kg, measured according to ISO 1133) in the range of 5 g / 10 min to 15 g / 10 min, preferably 5 g / 10 min to 10 g / 10 min, more preferably 8 g / 10 min; and a tensile modulus (ISO 178) higher than 800 MPa, preferably higher than 1000 MPa, more preferably higher than 1300 MPa.

[0069] The melting temperature of the polypropylene homopolymer (PPH-1) is at least 150° C., preferably at least 158° C., preferably in the range of 158 to 167° C., like 162° C. The flexural modulus of the polypropylene homopolymer (PPH-1) measured according to ISO 178 may be at least 500 MPa, preferably at least 1000 MPa, preferably in the range of 1200 to 2000 MPa, like 1400 MPa.

[0070] Preferred materials for the polypropylene homopolymer (PPH-1) are commercially available inter alia under the name HD601CF from Borealis AG (Austria).Alternative suitable materials are high crystalline polypropylene homopolymers as described for example in WO 03 / 031174 A2.

[0071] Polypropylene homopolymer (PPH-2):

[0072] The at least one polypropylene homopolymer (PPH-2) has a melt flow rate MFR2 (230°C, 2.16 kg, measured according to ISO 1133) in the range of 10 g / 10 min to 30 g / 10 min, preferably 15 g / 10 min to 25 g / 10 min, preferably 20 g / 10 min; and a tensile modulus (ISO 527-2) higher than 1800 MPa, preferably higher than 2000 MPa, most preferably 2200 MPa.

[0073] The polypropylene homopolymer (PPH-2) consists essentially of propylene units, i.e. more than 99.7 wt.-%, even more preferably at least 99.8 wt.-%, based on the weight of the propylene homopolymer (PPH-2), of propylene units. In a preferred embodiment, only propylene units are detectable in the propylene homopolymer (PPH-2).

[0074] It will be appreciated that the polypropylene homopolymer (PPH-2) is characterized by a small amount of xylene cold soluble (XCS) fraction. Based on the weight of the polypropylene homopolymer (PPH-2), the polypropylene homopolymer (PPH-2) may have the following amount of xylene cold soluble (XCS) fraction: not more than 4.0 wt%, preferably not more than 3.0 wt%, more preferably not more than 2.5 wt%, such as in the range of 0.1 wt% to 4.0 wt%, preferably in the range of 0.1 wt% to 3.0 wt%, more preferably in the range of 0.1 wt% to 2.5 wt%.

[0075] The polypropylene homopolymer (PPH-2) may have a heat deflection temperature (HDT) measured according to ISO 75-2 of at least 90°C, preferably at least 100°C, more preferably at least 115°C, such as in the range of 90 to 160°C, preferably in the range of 100 to 150°C, more preferably in the range of 115 to 130°C.

[0076] The polypropylene homopolymer (PPH-2) may have a Charpy impact strength measured at 23° C. according to ISO 179-1eA of at least 1.0 kJ / m 2 , preferably at least 2.0 kJ / m 2 , such as at 1.0 kJ / m 2 Up to 10kJ / m 2 In the range of 2.0 kJ / m 2 Up to 5.0 kJ / m 2 In the range of 2.5 kJ / m 2 The polypropylene homopolymer (PPH-2) may have a flexural modulus measured according to ISO 178 of at least 500 MPa, preferably at least 1500 MPa, such as in the range of 500 to 3500 MPa, preferably in the range of 1500 to 2500 MPa, such as 2000 MPa.

[0077] The polypropylene homopolymer (PPH-2) may contain a nucleating agent, which is preferably a polymeric nucleating agent, more preferably an α-nucleating agent, such as a polymeric α-nucleating agent. The α-nucleating agent content of the polypropylene homopolymer (PPH-2) is preferably up to 5.0 wt%. In a preferred embodiment, the polypropylene homopolymer (PPH-2) contains no more than 3000 ppm, more preferably 1 ppm to 2000 ppm of α-nucleating agent.

[0078] Polypropylene homopolymer (PPH-2) is known in the art and is commercially available, for example, from Borealis AG under the name HF955MO. Preference is given to using PPH-2.

[0079] Virgin polypropylene block copolymer

[0080] The following describes the properties and characteristics of virgin polypropylene block copolymers that may be used in the polyolefin compositions of the present invention.

[0081] Polypropylene Block Copolymer (PBC-1)

[0082] In one embodiment, the at least one polypropylene block copolymer (PBC-1) has a melt flow rate (230°C / 2.16 kg) of at least 0.10 g / 10 min, preferably at least 0.20 g / 10 min, in particular in the range of 0.20 to 2.0 g / 10 min, more in particular in the range of 0.20 to 1.5 g / 10 min, for example 0.20 to 0.32 g / 10 min.

[0083] The polypropylene block copolymer (PBC-1) may have a Charpy notched impact strength (NIS) measured at 23° C. according to ISO 179-1eA of at least 40 kJ / m 2 , preferably at least 50 kJ / m 2 , such as at 40kJ / m 2 Up to 60kJ / m 2 In the range of 45 kJ / m 2 Up to 55kJ / m 2 In the range of 50 kJ / m 2 The yield tensile stress of the polypropylene block copolymer (PBC-1) measured according to ISO 527-2 may be at least 25 MPa, preferably at least 30 MPa, such as in the range of 25 MPa to 45 MPa, preferably in the range of 30 MPa to 35 MPa, such as 31 MPa. The density may be 800 kg / m 3 Up to 1000kg / m 3 In the range of 850 kg / m 3 Up to 950kg / m 3 In the range of 900kg / m 3 .

[0084] Polypropylene block copolymer (PBC-1) is known in the art and is commercially available, for example, from Borealis AG as BA212E.

[0085] Mixed plastics polypropylene blends from recycled materials

[0086] The mixed plastic polypropylene blend is obtained from the recycled scrap stream of post-consumer plastic waste.

[0087] Several possible raw materials from municipal waste collection systems are commercially available and allow the provision of post-consumer plastic waste. Depending on the involvement of the consumer, the purity of these raw materials will be different, which is usually indicated by the collection system. The intermediates can also be screened after step b) for the presence of obviously very old ("old-style") mainly colorless / natural plastic products. Discoloration (e.g., significant yellowing) and / or significant scratches of the mainly colorless / natural plastic products allow sorting. Such a step makes it possible to remove the so-called substances of very high concern. These substances, such as Pb, Hg, polybrominated diphenyl ethers, etc., have been banned for quite some time, but still exist in the real world because consumers tend to pile up plastic products (e.g., in the form of plastic toys) for many years and eventually discard them into the collection system. Additional screening steps can be assisted by analytical control of the substances of very high concern.

[0088] Odor control and evaluation can be performed by a variety of methods. Demets, Ruben et al. "Development and application of an analytical method to quantify odour removal in plastic waste recycling processes." Resources, Conservation and Recycling 161 (2020): 104907, in particular, provides an overview, which is incorporated herein by reference.

[0089] The melt flow rate (ISO 1133, 2.16 kg; 230°C) of the mixed plastic polypropylene blend is typically 2.0 g / 10 min to 50 g / 10 min. The melt flow rate can be affected by diverting the post-consumer plastic waste stream, for example but not limited to: originating from the extended producer responsibility system (such as from the German DSD), or sorting a large number of pre-sorted fractions from municipal solid waste and recombining them in an appropriate manner. As another way to change the melt flow rate of the final mixed plastic polypropylene blend, peroxides can be introduced in the final granulation step. Typically the MFR range is 2.0 g / 10 min to 50 g / 10 min, preferably 5.0 g / 10 min to 40 g / 10 min, more preferably 10 g / 10 min to 30 g / 10 min, most preferably 15 g / 10 min to 25 g / 10 min. This MFR range is particularly suitable for non-visbreaking mixed plastic polypropylene blends. Visbreaking allows to increase the MFR to 30 g / 10 min or 40 g / 10 min.

[0090] Typically, recovery properties can be assessed by the presence of one or more of the following:

[0091] a) Polystyrene

[0092] b) Polyamide-6

[0093] c) Limonene as determined by using solid phase microextraction (HS-SPME-GC-MS)

[0094] d) Fatty acids as determined by using solid phase microextraction (HS-SPME-GC-MS).

[0095] Presence means detectable limit. The detection limit of limonene and fatty acids in solid phase microextraction (HS-SPME-GC-MS) is below 0.1 ppm, ie trace amounts of these substances easily allow to conclude the recovery properties.

[0096] The following amounts are preferred:

[0097] a) Polystyrene: 0 wt% to 2.0 wt%; more preferably 0 wt% to 0.5 wt%

[0098] b) Polyamide-6: 0 wt% to 1.5 wt%; more preferably 0 wt% to 0.5 wt%

[0099] c) Limonene as determined by using solid phase microextraction (HS-SPME-GC-MS): 0.1 ppm to 50 ppm

[0100] d) Fatty acids as determined by using solid phase microextraction (HS-SPME-GC-MS): 0.1 ppm to 200 ppm, more preferably 50 ppm.

[0101] It goes without saying that the amounts of a), b), c) and d) should be as low as possible. In a particularly preferred embodiment, the mixed plastic polypropylene blend is polystyrene-free and polyamide-free, which means that both polymers are below the detection limit.

[0102] Different mixed plastic polypropylene blends can be used.

[0103] Mixed plastic polypropylene blend (blend A1)

[0104] In one embodiment, the mixed plastic polypropylene blend (Blend A1) has:

[0105] (i) a crystalline fraction (CF) content determined according to CRYSTEX QC analysis in the range of 86.0 wt.-% to 94.0 wt.-%, more preferably 90.0 wt.-% to 94.0 wt.-%, and

[0106] (ii) a soluble fraction (SF) content determined according to CRYSTEX QC analysis in the range of 6.0 wt.-% to 14.0 wt.-%, more preferably 6.0 wt.-% to 10.0 wt.-%, wherein

[0107] (iii) The crystalline fraction (CF) is quantitatively 13 The propylene content (C3(CF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is in the range of 93.0 wt.-% to 99.0 wt.-%, preferably 95.0 wt.-% to 98.0 wt.-%; and wherein

[0108] (iv) The crystalline fraction (CF) is determined by quantitative 13 An ethylene content (C2(CF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is in the range of 1 wt% to 7 wt%, more preferably 2.0 wt% to 5.0 wt%, even more preferably 2.5 wt% to 3.5 wt%; and

[0109] (v) the intrinsic viscosity (iV(SF)) of the soluble fraction (SF) is in the range of 1.2 dl / g to less than 1.8 dl / g, preferably 1.40 dl / g to 1.70 dl / g;

[0110] in

[0111] (vi) The CIELAB color space (L*a*b*) of the mixed plastic polypropylene blend is:

[0112] - L* from 40 to 85, preferably from 50 to 75;

[0113] --a* of 8.00 to 10, more preferably -5.0 to 0.0;

[0114] b* of -0.0 to below 10.0, more preferably 0.0 to below 5.00.

[0115] The melt flow rate MFR2 (ISO 1133, 2.16 kg, 230°C) of the mixed plastic polypropylene blend (blend A1) is preferably at least 10.0 g / 10 min, preferably at least 12.0 g / 10 min, more preferably at least 14.0 g / 10 min, in particular in the range of 10.0 g / 10 min to 30.0 g / 10 min, preferably 12.0 g / 10 min to 25.0 g / 10 min, more preferably 14.0 g / 10 min to 20.0 g / 10 min.

[0116] Blend A1 preferably has a crystalline fraction (CF) content determined according to CRYSTEX QC analysis in the range of 90.0 to 94.0 wt.-% and a soluble fraction (SF) content determined according to CRYSTEX QC analysis in the range of 6.0 to 10.0 wt.-%.

[0117] The soluble fraction (SF) of the mixed plastic polypropylene blend (Blend A1) obtained by CRYSTEX QC analysis was determined by quantitative 13 The ethylene content (C2(SF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is preferably in the range of 20.0 wt.-% to 30.0 wt.-%, more preferably 20.0 wt.-% to 28.0 wt.-%, even more preferably 22.0 wt.-% to 26.0 wt.-%, most preferably 23.0 wt.-% to 25.0 wt.-%.

[0118] Preferably, the mixed plastic polypropylene blend (Blend-A1) is characterized by an odor (VDA 270-B3) of 5.0 or less, preferably 4.7 or less, more preferably 4.0 or less, such as 3.5.

[0119] In another aspect, the mixed plastic polypropylene blend (Blend A1) has a Large Amplitude Oscillatory Shear-Non-Linear Factor (LAOS-NLF) greater than 2.6 (190° C.; 1000%), wherein

[0120]

[0121] in

[0122] G1' is the first-order Fourier coefficient

[0123] G3' is the third-order Fourier coefficient

[0124] The tensile modulus (ISO 527-2, at a crosshead speed of 1 mm / min; 23°C) of the mixed plastic polypropylene blend (Blend-A1) using injection molded test specimens (dog bone, 4 mm thick) as described in EN ISO 1873-2 is at least 1300 MPa, preferably at least 1330 MPa, such as 1440 MPa.

[0125] The mixed plastic polypropylene blend (Blend A1) proved to be processable, as reflected by a shear thinning factor (STF) (ratio of η0.05 to η300) above 9.0, preferably above 10.0.

[0126] The Charpy notched impact strength (non-instrumented, ISO 179-1, at +23°C) of the mixed plastic polypropylene blend (Blend-A1) is preferably above 4.5 kJ / m 2 , more preferably higher than 5.0 kJ / m 2 , most preferably above 5.4 kJ / m 2 , for example 6.9 kJ / m 2 .

[0127] The method for obtaining the mixed plastic polypropylene blend A1 comprises the following steps:

[0128] a) providing a precursor mixed plastic recycling stream (A);

[0129] b) screening the precursor mixed plastic recycling stream (A) to produce a screened mixed plastic recycling stream (B) of only articles having a longest dimension in the range of 30 mm to 400 mm;

[0130] c) sorting the screened mixed plastic recycling stream (B) by one or more optical sorters, wherein the screened mixed plastic recycling stream (B) is sorted at least by color, and optionally also by polyolefin type and / or article form, thereby producing one or more single-color sorted polyolefin recycling streams (C) and mixed color sorted polyolefin recycling streams (CM), wherein each of the one or more single-color sorted polyolefin recycling streams (C) and mixed color sorted polyolefin recycling streams (CM) is subjected to step d) and subsequent steps separately;

[0131] d) chopping the sorted polyolefin recovery stream (C or CM) to form a flake polyolefin recovery stream (D);

[0132] e) washing the flaky polyolefin recovery stream (D) with a first aqueous washing solution (W1) without inputting heat energy, thereby producing a first suspended polyolefin recovery stream (E);

[0133] f) removing at least a portion of the first aqueous wash solution (W1), preferably substantially all of the first aqueous wash solution (W1), from the first suspended polyolefin recovery stream (E) to obtain a first washed polyolefin recovery stream (F);

[0134] g) washing the first washed polyolefin recovery stream (F) with a second aqueous washing solution (W2) to produce a second suspended polyolefin recovery stream (G), wherein sufficient thermal energy is introduced into the second suspended polyolefin recovery stream (G) to provide a temperature in the range of 65° C. to 95° C. during washing;

[0135] h) removing the second aqueous wash solution (W2) and any material not floating on the surface of the second aqueous wash solution from the second suspended polyolefin recovery stream (G) to obtain a second washed polyolefin recovery stream (H);

[0136] i) drying the second washed polyolefin recovery stream (H) to obtain a dried polyolefin recovery stream (I);

[0137] j) optionally separating the dried polyolefin recovery stream (I) into a light fraction and a heavy fraction polyolefin recovery stream (J);

[0138] k) optionally, further sorting the heavy fraction polyolefin recovery stream (J) or, in the absence of step j), the dried polyolefin recovery stream (I) by one or more optical sorters to sort the one or more target polyolefins by removing any flakes comprising materials other than the one or more target polyolefins to produce a purified polyolefin recovery stream (K);

[0139] l) optionally, melt extruding, preferably pelletizing, the purified polyolefin recovery stream (K), preferably wherein the additive (Ad) is added in the molten state, to form an extruded, preferably pelletized, recovered polyolefin product (L); and

[0140] m) optionally aerating the recycled polyolefin product (L) or, in the absence of step l), aerating the purified polyolefin recycled stream (K) to remove volatile organic compounds, thereby producing an aerated recycled polyolefin product (M), which is an aerated extruded, preferably pelletized recycled polyolefin product (M1) or an aerated recycled polyolefin flake (M2),

[0141] The order of steps l) and m) can be interchanged so that the purified polyolefin recycling stream (K) is first aerated to form aerated recycled polyolefin flakes (M2), which are subsequently extruded to form an extruded, preferably pelletized, aerated recycled polyolefin product (M3), which is a polypropylene mixed color blend A1 as described above.

[0142] Mixed plastic polypropylene blend (blend A2)

[0143] In another embodiment, the mixed plastic polypropylene blend (Blend A2) has:

[0144] (i) a crystalline fraction (CF) content determined according to CRYSTEX QC analysis in the range of 86.0 wt.-% to 94.0 wt.-%, preferably 91.0 wt.-% to 94.0 wt.-%, and

[0145] (ii) a soluble fraction (SF) content determined according to CRYSTEX QC analysis in the range of 6.0 wt.-% to 14.0 wt.-%, more preferably 6.0 wt.-% to 9.0 wt.-%, wherein

[0146] (iii) The crystalline fraction (CF) is quantitatively 13 The propylene content (C3(CF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is in the range of 95.0 wt.-% to 99.0 wt.-%, preferably 96.0 wt.-% to 98.0 wt.-%, and wherein

[0147] (iv) The crystalline fraction (CF) is determined by quantitative 13 An ethylene content (C2(CF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is in the range of 1.0 to 5.0 wt. %, preferably 2.0 to 4.0 wt. %, more preferably 2.5 to 3.5 wt. %; and

[0148] (v) the intrinsic viscosity (iV(SF)) of the soluble fraction (SF) is in the range of 1.1 dl / g to less than 1.5 dl / g, preferably 1.25 dl / g to less than 1.45 dl / g;

[0149] in

[0150] (vi) The CIELAB color space (L*a*b*) of the mixed plastic polypropylene blend is:

[0151] - L* from 72.0 to 97.0, preferably from 80.0 to 97.0;

[0152] --a* from 5.0 to 0.0;

[0153] -0.0 to b* below 22.0.

[0154] The melt flow rate MFR2 (ISO 1133, 2.16 kg, 230°C) of the mixed plastic polypropylene blend (blend A2) is preferably at least 4.0 g / 10 min, preferably at least 6.0 g / 10 min, more preferably at least 7.0 g / 10 min, in particular in the range of 4.0 g / 10 min to 12.0 g / 10 min, preferably 6.0 g / 10 min to 10.0 g / 10 min, more preferably 7.0 g / 10 min to 9.0 g / 10 min.

[0155] In one embodiment, the crystalline fraction (CF) content of blend A2 determined according to CRYSTEX QC analysis is preferably in the range of 91.0 wt. % to 94.0 wt. %, preferably 92 wt. % to 93 wt. %, and the soluble fraction (SF) content determined according to CRYSTEX QC analysis is in the range of 6.0 wt. % to 9.0 wt. %, preferably 7.0 wt. % to 8.0 wt. %.

[0156] The soluble fraction (SF) of the mixed plastic polypropylene blend (Blend A2) obtained by CRYSTEX QC analysis was determined by quantitative 13 The ethylene content (C2(SF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is preferably in the range of 10.0 wt.-% to 25.0 wt.-%, more preferably 12.0 wt.-% to 25.0 wt.-%, even more preferably 12.0 wt.-% to 20.0 wt.-%, most preferably 14.0 wt.-% to 19.0 wt.-%.

[0157] Preferably, the mixed plastic polypropylene blend (Blend-A2) is characterized by an odor (VDA 270-B3) of 4.0 or less, preferably 3.0.

[0158] In another aspect, the mixed plastic polypropylene blend has a large amplitude oscillatory shear-nonlinear factor (LAOS-NLF) greater than 2.3 (190° C.; 1000%), wherein

[0159]

[0160] in

[0161] G1' is the first-order Fourier coefficient

[0162] G3' is the third-order Fourier coefficient

[0163] The tensile modulus (ISO 527-2, at a crosshead speed of 1 mm / min; 23° C.) of the injection molded test specimen (dog bone, 4 mm thick) of the mixed plastic polypropylene blend as described in EN ISO 1873-2 is at least 1200 MPa, preferably at least 1250 MPa. Typically, the tensile modulus (ISO 527-2, at a crosshead speed of 1 mm / min; 23° C.) of the second embodiment will not be higher than 1400 MPa.

[0164] The mixed plastic polypropylene blends are shown to have excellent processability, which is reflected by a shear thinning factor (STF) (ratio of η0.05 to η300) above 13.0, preferably above 14.0.

[0165] The Charpy notched impact strength (non-instrumented, ISO 179-1, at +23°C) of the mixed plastic polypropylene blend is preferably above 6.0 kJ / m 2 , more preferably higher than 8.0 kJ / m 2 , most preferably above 8.3 kJ / m 2 , for example 8.5 kJ / m 2 .

[0166] In a particularly preferred embodiment, the mixed plastic polypropylene blend (blend A2) has a notched Charpy impact strength (NIS) (1eA) at +23°C according to ISO 179-1eA (non-instrumented, ISO 179-1, at +23°C) of at least 8.0 kJ / m 2 , preferably 8.3 kJ / m 2 , wherein the soluble fraction (SF) obtained by CRYSTEX QC analysis is further determined by quantitative 13 The ethylene content (C2(SF)) determined by FT-IR spectroscopy calibrated by C-NMR spectroscopy is in the range of 12.0 wt. % to 20.0 wt. %, and further preferably the CIELAB color space (L*a*b) of the mixed plastic polypropylene blend is:

[0167] - L* from 72.0 to 97.0, preferably from 80.0 to 97.0;

[0168] --a* from 5.0 to 0.0;

[0169] -0.0 to b* below 22.0.

[0170] In this particularly preferred embodiment, the crystalline fraction (CF) content of blend A2 determined according to CRYSTEX QC analysis is preferably in the range of 91.0 wt.-% to 94.0 wt.-%, and the soluble fraction (SF) content determined according to CRYSTEX QC analysis is in the range of 6.0 wt.-% to 9.0 wt.-%.

[0171] The method for obtaining the mixed plastic polypropylene blend A2 comprises the following steps:

[0172] a) Provide post-consumer plastic waste;

[0173] b) Sorting of items made of polystyrene, polyamide, polyethylene, metal, paper and wood, thus providing post-consumer plastic materials;

[0174] c) sorting the colored items to provide post-consumer plastic materials including primarily white bottles, primarily white yogurt cups, primarily white jars, primarily colorless panels, primarily colorless components, etc.;

[0175] d) subjecting selected predominantly white or colorless post-consumer plastic materials to grinding, washing with various detergents in aqueous solution, followed by drying, pneumatic screening and screening;

[0176] e) subjecting the pre-treated post-consumer plastic material to further sorting to eliminate non-polyolefin and color fractions;

[0177] f) extruding the material and producing the polypropylene blend according to the invention in the form of pellets;

[0178] g) optionally, aerating, preferably at a temperature of at least 100°C by preheating the post-consumer plastic material to a temperature in the range of 100°C to 130°C using an air stream at such a temperature.

[0179] Fiberglass

[0180] As mentioned above, the polyolefin composition according to the present invention comprises glass fibers, in particular short glass fibers. The average fiber length of the glass fibers used in the polyolefin composition according to the present invention is preferably in the range of 2.0 mm to 10.0 mm, preferably in the range of 2.0 mm to 8.0 mm, even more preferably in the range of 2.0 mm to 6.0 mm, still more preferably in the range of 3.0 mm to 5.5 mm, even more preferably in the range of 3.5 mm to 5.0 mm.

[0181] Further preferably, the average diameter of the short glass fibers used in the fiber-reinforced composite material is preferably 5 μm to 20 μm, more preferably 8 μm to 18 μm, still more preferably 8 μm to 15 μm, even more preferably 10 μm to 15 μm, preferably 11 μm to 14 μm, preferably 12 μm to 14 μm, more preferably 12.3 μm to 13.7 μm, even more preferably 12.5 μm to 13.5 μm.

[0182] In a preferred embodiment, glass fibers having a fiber length of 3.0 mm to 5.0 mm (4.0 mm on average) and a fiber diameter of 12.3 μm to 13.7 μm (13 μm on average) are used. In another preferred embodiment, glass fibers having a fiber length of 3.5 mm to 5.5 mm (4.5 mm on average) and a fiber diameter of 12 μm to 14 μm (13 μm on average) are used.

[0183] Coupling agent / dosing agent

[0184] In one embodiment, the polyolefin composition according to the present invention comprises at least one coupling agent. At least one coupling agent is a functionalized polypropylene, in particular, a polypropylene functionalized with maleic anhydride (MAH). The amount of the coupling agent in the polyolefin composition can be 1 wt % to 2 wt %, for example 1 wt % or 1.25 wt %.

[0185] In one embodiment, the polyolefin composition may contain at least one dosing agent for receiving fillers / pigments during extrusion. The at least one dosing agent may have a melt flow rate MFR2 of 1 g / 10 min to 5 g / 10 min, preferably 2 g / 10 min to 3 g / 10 min and 800 kg / m 3 Up to 100kg / m 3 , preferably 900kg / m 3 Up to 950kg / m 3 Such polymers are commercially available from Borealis AG. The amount of the dosing agent in the polyolefin composition may be from 1 wt % to 2 wt %, for example from 1.2 wt % to 1.4 wt %.

[0186] additive

[0187] In another embodiment, the polyolefin composition may include other additives. Examples of additives used in the composition are pigments or dyes (e.g., carbon black), stabilizers (antioxidants), antacids and / or anti-UV agents, antistatic agents, nucleators, and utilization agents (e.g., processing aids). Preferred additives are carbon black, at least one antioxidant, and / or at least one UV stabilizer.

[0188] Typically, the amount of these additives ranges from 0 wt% to 5.0 wt%, preferably from 0.01 wt% to 3.0 wt%, more preferably from 0.01 wt% to 2.0 wt%, based on the weight of the total composition.

[0189] Examples of antioxidants commonly used in the art are sterically hindered phenols (e.g. CAS No. 6683-19-8, also known as Irganox 1010FF TM sold by BASF), phosphorus-based antioxidants (e.g. CAS No. 31570-04-4, also as Hostanox PAR 24 (FF) TM sold by Clariant or as Irgafos 168 (FF) TM by BASF), sulfur-based antioxidants (e.g. CAS No. 693-36-7, sold as Irganox PS-802FL TMSold by BASF), nitrogen-based antioxidants (e.g. 4,4'-bis(1,1'-dimethylbenzyl)diphenylamine), or antioxidant blends. Preferred antioxidants may be tris(2,4-di-tert-butylphenyl)phosphite and / or octadecyl 3-(3',5'-di-tert-butyl-4-hydroxyphenyl)propionate.

[0190] Antacids are also generally known in the art. Examples are calcium stearate, sodium stearate, zinc stearate, magnesium oxide and zinc oxide, synthetic hydrotalcite (e.g. SHT, CAS No. 11097-59-9), lactic acid esters / salts and lactyl esters / salts, and calcium stearate (CAS No. 1592-23-0) and zinc stearate (CAS No. 557-05-1).

[0191] Common anti-adhesion agents are natural silicon dioxide, such as diatomaceous earth (e.g. CAS No. 60676-86-0 (SuperfFloss TM ), CAS number 60676-86-0 (SuperFloss E TM ) or CAS No. 60676-86-0 (Celite499 TM )); synthetic silica (e.g., CAS No. 7631-86-9, CAS No. 7631-86-9, CAS No. 7631-86-9, CAS No. 7631-86-9, CAS No. 7631-86-9, CAS No. 7631-86-9, CAS No. 112926-00-8, CAS No. 7631-86-9 or CAS No. 7631-86-9); silicates (e.g., aluminum silicate (kaolin )CAS No. 1318-74-7, sodium aluminum silicate CAS No. 1344-00-9, calcined kaolin CAS No. 92704-41-1, aluminum silicate CAS No. 1327-36-2 or calcium silicate CAS No. 1344-95-2); synthetic zeolite (e.g. sodium calcium aluminosilicate hydrate CAS No. 1344-01-0, CAS No. 1344-01-0 or sodium calcium aluminosilicate hydrate CAS No. 1344-01-0).

[0192] The anti-UV agent is, for example, bis(2,2,6,6-tetramethyl-4-piperidinyl)-sebacate (CAS No. 52829-07-9, Tinuvin 770); 2-hydroxy-4-n-octyloxy-benzophenone (CAS No. 1843-05-6, Chimassorb 81). Preferred UV stabilizers can be low molecular weight UV stabilizers and / or high molecular weight UV stabilizers, such as n-hexadecyl-3,5-di-tert-butyl-4-hydroxybenzoate; a mixture of esters of 2,2,6,6-tetramethyl-4-piperidinol and higher fatty acids (mainly stearic acid); and / or poly((6-morpholino-s-triazine-2,4-diyl)(1,2,2,6,6-pentamethyl-4-piperidinyl)imino)hexamethylene(1,2,2,6,6-pentamethyl-4-piperidinyl)imino)).

[0193] Alpha nucleating agents such as sodium benzoate (CAS No. 532-32-1); 1,3:2,4-bis(3,4-dimethylbenzylidene)sorbitol (CAS 135861-56-2, Millad 3988).

[0194] The alpha nucleating agent may also be one of the following:

[0195] (i) soluble nucleating agents such as sorbitol derivatives, for example di(alkylbenzylidene)sorbitols such as 1,3:2,4-dibenzylidene sorbitol, 1,3:2,4-di(4-methylbenzylidene) sorbitol, 1,3:2,4-di(4-ethylbenzylidene) sorbitol and 1,3:2,4-bis(3,4-dimethylbenzylidene) sorbitol; and nonitol derivatives such as 1,2,3-trideoxy phenyl]-2,2-dimethyl-propionamide.

[0196] (ii) salts of mono- and polycarboxylic acids, for example sodium benzoate or aluminium tert-butylbenzoate;

[0197] (iii) salts of diesters of phosphoric acid, for example sodium 2,2'-methylenebis(4,6-di-tert-butylphenyl)phosphate or hydroxy-bis[2,2'-methylene-bis(4,6-di-tert-butylphenyl)phosphate]aluminum and hydroxybis(2,4,8,10-tetra-tert-butyl-6-hydroxy-12H-dibenzo(d,g)(1,3,2)dioxaphosphine 6-oxide)aluminum; and

[0198] (iv) Inorganic nucleating agents, such as talc.

[0199] Suitable antistatic agents are, for example, glycerol esters (CAS No. 97593-29-8) or ethoxylated amines (CAS No. 71786-60-2 or 61791-31-9) or ethoxylated amides (CAS No. 204-393-1).

[0200] These additives are generally added in amounts of 100 ppm to 2.000 ppm for each individual component of the polymer.

[0201] Hereinafter, more specific embodiments of the composition of the present invention are described.

[0202] In a first embodiment, a polyolefin composition is provided comprising:

[0203] a) 9 to 22 wt.-% (based on the total weight of the polyolefin composition) of at least one polypropylene homopolymer,

[0204] b) 4 to 6 wt.-% (based on the total weight of the polyolefin composition) of at least one polypropylene block copolymer,

[0205] c) 25 to 45 wt. % (based on the total weight of the polyolefin composition) of a mixed plastic polypropylene blend (Blend A1);

[0206] d) 38 to 42 wt. % (based on the total weight of the polyolefin composition) of glass fibers;

[0207] and optionally further additives, wherein the sum of all ingredients adds up to 100% by weight.

[0208] Such a first polyolefin composition may have:

[0209] - a melt flow rate MFR2 (230° C., 2.16 kg, measured according to ISO 1133) in the range of 3.0 to 8.0 g / 10 min; preferably in the range of 3.3 to 7.0 g / 10 min, more preferably in the range of 3.5 to 6.0 g / 10 min;

[0210] - a tensile modulus of at least 8500 MPa, preferably at least 9000 MPa (ISO 527-2),

[0211] - a tensile stress at yield of at least 95 MPa, preferably at least 100 MPa at 23°C,

[0212] a tensile stress at break of at least 95 MPa, preferably at least 100 MPa at 23° C.,

[0213] - At least 9.0 kJ / m 2 , preferably at least 9.5 kJ / m 2 Impact strength (ISO179-1, Charpy 1eA+23℃).

[0214] In a second embodiment, a polyolefin composition is provided comprising:

[0215] a) 9 to 22 wt.-% (based on the total weight of the polyolefin composition) of at least one polypropylene homopolymer,

[0216] b) 4 to 6 wt.-% (based on the total weight of the polyolefin composition) of at least one polypropylene block copolymer,

[0217] c) 25 to 45 wt. % (based on the total weight of the polyolefin composition) of a mixed plastic polypropylene blend (blend A2);

[0218] d) 38 to 42 wt. % (based on the total weight of the polyolefin composition) of glass fibers;

[0219] and optionally further additives, wherein the sum of all ingredients adds up to 100% by weight.

[0220] Such a second polyolefin composition may have:

[0221] - a melt flow rate MFR2 (230° C., 2.16 kg, measured according to ISO 1133) in the range of 3.5 to 8.0 g / 10 min; preferably in the range of 4.0 to 7.0 g / 10 min, more preferably in the range of 4.3 to 6.0 g / 10 min;

[0222] - a tensile modulus (ISO 527-2) of at least 8500 MPa, preferably at least 8700 MPa,

[0223] - a tensile stress at yield of at least 100 MPa, preferably at least 105 MPa at 23°C,

[0224] - a tensile stress at break of at least 100 MPa, preferably at least 105 MPa at 23°C,

[0225] - At least 10.0 kJ / m 2 , preferably at least 11 kJ / m 2 Impact strength (ISO179-1, Charpy 1eA+23℃).

[0226] It is worth noting that the impact strength, yield tensile stress and break tensile stress are different depending on the type of mixed plastic polypropylene blend (i.e., blend A1 or blend A2). In particular, the use of mixed plastic polypropylene blends as in blend A2 improves the impact strength, yield tensile stress and break tensile stress.

[0227] It will be appreciated that the present invention also relates to a process for producing a polyolefin composition as defined herein. Said process comprises the following steps:

[0228] - providing a mixture having the desired amounts of at least one polypropylene homopolymer, at least one polypropylene block copolymer, a mixed plastic polypropylene blend of recycled material, glass fibers and at least one coupling agent;

[0229] - melting the mixture in an extruder; and

[0230] - Optionally pelletizing the polyolefin composition obtained.

[0231] For purposes of the present invention, mixing and melting may be performed using any suitable melting and mixing means known in the art.

[0232] However, the melting and mixing steps are preferably carried out in a mixer and / or blender, a high shear mixer or a low shear mixer, a high speed blender or a twin screw extruder. Most preferably, the melting and mixing steps are carried out in a twin screw extruder, such as a co-rotating twin screw extruder. Such twin screw extruders are well known in the art, and the skilled person will adjust the melting and mixing conditions (e.g., melt temperature, screw speed, etc.) according to the process equipment.

[0233] The polyolefin composition according to the present invention can be used in a wide range of applications, for example for the manufacture of structural products, pumps, fans, appliances, automotive parts, pipes and fittings, packaging, caps and closures.

[0234] Experimental Section

[0235] The following examples are included to illustrate certain aspects and embodiments of the present invention as described in the claims. However, it should be understood by those skilled in the art that the following description is illustrative only and should not be construed in any way as limiting the present invention.

[0236] Test Method

[0237] Unless otherwise defined, the following term definitions and determination methods apply to the above general description of the invention as well as the following examples.

[0238] a) CRYSTEX

[0239] Determination of the crystalline and soluble fractions and their respective characteristics (IV and ethylene content)

[0240] The crystalline fraction (CF) and soluble fraction (SF) of the polypropylene (PP) composition and the comonomer content and intrinsic viscosity of each fraction were analyzed by using a CRYSTEX instrument, Polymer Char (Valencia, Spain). Details of the technology and methods 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).

[0241] The crystalline and amorphous fractions were separated by temperature cycles of dissolution at 160° C., crystallization at 40° C. and redissolution in 1,2,4-trichlorobenzene at 160° C. Quantification of SF and CF as well as determination of the ethylene content (C2) were achieved by an integrated infrared detector (IR4) and determination of the intrinsic viscosity (IV) using an online 2-capillary viscometer.

[0242] The IR4 detector measures two distinct bands (CH3 stretching vibration (centered at about 2960 cm) used to determine the concentration and ethylene content in ethylene-propylene copolymers. -1 ) and CH stretching vibration (2700cm -1 Up to 3000cm -1 ). The IR4 detector was calibrated with a series of 8EP copolymers with known ethylene contents ranging from 2 wt% to 69 wt% (determined by 13C-NMR) and at various concentrations ranging from 2 mg / ml to 13 mg / ml, respectively. For the various polymer concentrations expected during Crystex analysis, in order to obtain both concentration and ethylene content characteristics, the following calibration equation was applied:

[0243] Concentration = a + b * absorbance (CH) + c * (absorbance (CH)) 2+d*Absorbance(CH3)+e*(Absorbance(CH3)) 2 +f*Absorbance(CH)*Absorbance(CH3) (Equation 1)

[0244] CH3 / 1000C = a+b*absorbance(CH3)+c*absorbance(CH3)+d*(absorbance(CH3) / absorbance(CH3))+e*(absorbance(CH3) / absorbance(CH3)) 2 (Equation 2)

[0245] Constants a to e of Equation 1 and constants a to f of Equation 2 are determined by using least squares regression analysis.

[0246] The CH3 / 1000C is converted to ethylene content in weight % using the following relationship:

[0247] Weight % (ethylene in EP copolymer) = 100 - CH3 / 1000TC*0.3 (Equation 3)

[0248] The amount of the soluble fraction (SF) and the crystalline fraction (CF) are related to the amount of "xylene cold solubles" (XCS) and the xylene cold insoluble (XCI) fraction, respectively, determined according to the standard gravimetric method according to ISO 16152 by the XS calibration. The XS calibration was achieved by testing various EP copolymers with XS contents ranging from 2 wt% to 31 wt%. The determined XS calibration is linear:

[0249] Weight %XS=1.01*weight %SF (Equation 4)

[0250] The intrinsic viscosity (IV) of the parent EP copolymer and its soluble and crystalline fractions was determined by using an online 2-capillary viscometer and correlated to the corresponding IV determined by the standard method in decalin according to ISO 1628-3. The calibration was achieved with various EP PP copolymers with IV = 2 dL / g to 4 dL / g. The calibration curve determined was linear:

[0251] IV(dL / g)=a*Vsp / c (Equation 5)

[0252] The sample to be analyzed was weighed out at a concentration of 10 mg / ml to 20 mg / ml. To avoid injection of possible gels and / or polymers such as PET and PA that are not soluble in TCB at 160°C, the weighed sample was loaded into a stainless steel mesh MW 0,077 / D 0,05 mmm.

[0253] After automatically filling the vial with 1,2,4-TCB containing 250 mg / l 2,6-tert-butyl-4-methylphenol (BHT) as an antioxidant, the sample was dissolved at 160° C. with continuous stirring at 400 rpm until complete dissolution was achieved (usually for 60 minutes). To avoid sample degradation, the polymer solution was enveloped with a N2 atmosphere during dissolution.

[0254] A defined volume of the sample solution is injected into a column filled with an inert support, where crystallization of the sample and separation of the soluble fraction from the crystalline part is carried out. This process is repeated twice. During the first injection, the entire sample is measured at high temperature, and the IV [dl / g] and C2 [wt%] of the PP composition are determined. During the second injection, the soluble fraction (at low temperature) and the crystalline fraction (at high temperature) are measured in the case of a crystallization cycle (wt% SF, wt% C2, IV).

[0255] b) Quantification of microstructure by NMR spectroscopy (calibration only)

[0256] Calibration was performed using quantitative nuclear magnetic resonance (NMR) spectroscopy.

[0257] Quantitative 13C{1H} NMR spectra were recorded in solution using a Bruker Avance Neo 400 NMR spectrometer operating at 400.15 MHz and 100.62 MHz for 1H and 13C, respectively. All spectra were recorded at 125°C using a 13C optimized 10 mm extended temperature probe head, using nitrogen for all pneumatics. About 200 mg of material was dissolved in about 3 ml of 1,2-tetrachloroethane-d2 (TCE-d2) along with about 3 mg of BHT (2,6-di-tert-butyl-4-methylphenol, CAS 128-37-0) and chromium-(III)-acetylacetone (Cr(acac)3) to give a 60 mM solution of the relaxant in the solvent as described in G. Singh, A. Kothari, V. Gupta, Polymer Testing 2009, 28(5), 475.

[0258] In order to ensure a uniform solution, after the initial sample preparation in the heating block, the NMR tube was further heated in a rotary oven for at least 1 hour. After being inserted into the magnet, the tube was rotated at 10 Hz. This setting was selected mainly for the quantitative determination required for high resolution and accurate ethylene content quantification. Standard single pulse excitation without NOE was adopted, using optimized sharp angle, 1 second cycle delay and double-stage WALTZ16 decoupling scheme, as described in Z.Zhou, R.Kuemmerle, X.Qiu, D.Redwine, R.Cong, A.Taha, D.Baugh, B.Winniford, J.Mag.Reson.187 (2007) 225 and V.Busico, P.Carbonniere, R.Cipullo, C.Pellecchia, J.Severn, G.Talarico, Macromol.Rapid Commun.2007, 28, 1128. A total of 6144 (6k) transients were obtained for each spectrum.

[0259] The quantitative 13C{1H}NMR spectra were processed, integrated and the relevant quantitative properties were determined from the integration. All chemical shifts were indirectly referenced to the central methylene of the ethylene block (EEE) at 30.00 ppm using the chemical shift of the solvent. This approach allows for comparable reference even when this structural unit is not present.

[0260] Characteristic signals corresponding to ethylene incorporation were observed (as described in Cheng, HN, Macromolecules 1984, 17, 1950) and the comonomer fraction was calculated as the fraction of ethylene in the polymer relative to all monomers in the polymer:

[0261] fE=(E / (P+E)

[0262] The comonomer fraction was quantified by integration of multiple signals in the 13C{1H} spectrum across the entire spectral region using the method of WJ. Wang and S. Zhu, Macromolecules 2000, 331157. The integration region was slightly adjusted to improve applicability to the entire range of comonomer content encountered.

[0263] The mole percent of comonomer incorporation is calculated from the mole fraction:

[0264] E[mol%]=100*fE

[0265] The weight percent of comonomer incorporation is calculated from the mole fraction:

[0266] E[weight%]=100*(fE*28.06) / ((fE*28.06)+((1-fE)*42.08)).

[0267] c) Tensile modulus and tensile strain at yield / break are measured according to ISO 527-2 (crosshead speed = 1 mm / min; test speed 50 mm / min at 23° C.) using injection molded test specimens as described in EN ISO 1873-2 (dog bone, 4 mm thick). The measurements are carried out after a conditioning time of 96 hours for the test specimens.

[0268] d) Impact strength was determined as notched Charpy impact strength (1eA) according to ISO 179-1eA at +23°C on injection moulded test specimens of 80 mm x 10 mm x 4 mm prepared according to EN ISO 1873-2 (non-instrumented, ISO 179-1 at +23°C).

[0269] e) Inorganic residues: TGA was performed using a Perkin Elmer TGA 8000 according to DIN ISO 1172:1996. About 10 mg to 20 mg of material was placed in a platinum pan. The temperature was equilibrated at 50°C for 10 minutes and then increased to 950°C under nitrogen at a heating rate of 20°C / min. The ash content was estimated as weight % at 850°C.

[0270] f) MFR: Melt flow rate measured at 230° C. with a load of 2.16 kg (MFR2). The melt flow rate is the amount of polymer in grams which the test apparatus standardized to ISO 1133 extrude in 10 minutes at a temperature of 230° C. under a load of 2.16 kg.

[0271] g) Amount of metal

[0272] Determined by x-ray fluorescence (XRF).

[0273] h) Amount of paper and wood (for comparison purposes only)

[0274] Paper and wood can be identified by conventional laboratory methods including grinding, flotation, microscopy and thermogravimetric analysis (TGA).

[0275] i) Benzene content

[0276] By HS GC-MS as described below 80°C / 2 hours.

[0277] Static Headspace Analysis

[0278] The parameters of the applied static headspace gas chromatography mass spectrometry (HS / GC / MS) method are described here.

[0279] Weigh 4.000 ± 0.100 g of sample in a 20 ml HS vial and seal tightly with a PTFE cap.

[0280] The mass spectrometer was operated in scan mode and a total ion chromatogram (TIC) was recorded for each analysis. More detailed information on applicable method parameters and data evaluation is given below:

[0281] -HS parameters (Agilent G1888 headspace sampler)

[0282] Vial equilibration time: 120 minutes

[0283] Oven temperature: 80℃

[0284] Loop temperature: 205℃

[0285] Transfer line temperature: 210°C

[0286] Low shake

[0287] -GC parameters (Agilent 7890A GC system)

[0288] Column: ZB-WAX 7HG-G007-22 (30m×250μm×1μm)

[0289] Carrier gas: Helium 5.0

[0290] Flow rate: 2ml / min

[0291] Split: 5:1

[0292] GC oven program: 35°C for 0.1 min

[0293] 10℃ / min up to 250℃

[0294] 250℃ for 1 minute

[0295] -MS parameters (Agilent 5975C Inert XL MSD)

[0296] Acquisition Mode: Scan

[0297] Scan parameters:

[0298] Low Quality: 20

[0299] High quality: 200

[0300] Threshold: 10

[0301] - Software / Data Evaluation

[0302] MSD ChemStation E.02.02.1431

[0303] MassHunter GC / MS Acquisition B.07.05.2479

[0304] AMDIS GC / MS Analysis Version 2.71

[0305] NIST Mass Spectral Library Version 2.0g

[0306] -AMDIS Deconvolution Parameters

[0307] Minimum Match Factor: 80

[0308] Threshold: Low

[0309] Scan Direction: High to Low

[0310] Data File Format: Agilent File

[0311] Instrument Type: Quadrupole

[0312] Component Width: 20

[0313] Adjacent Peak Subtraction: Two

[0314] Resolution: High

[0315] Sensitivity: Very High

[0316] Shape Requirement: Medium

[0317] Solvent Tail: 44 m / z

[0318] Column Bleed: 207 m / z

[0319] Minimum Model Peaks: 2

[0320] Minimum S / N: 10

[0321] Minimum Specific Peak: 0.5

[0322] Data Evaluation

[0323] The TIC data was further deconvoluted using the AMDIS software (see parameters above) and compared with a custom target library based on the mass spectral library (NIST). In the custom target library, individual mass spectra of the selected substances (e.g., benzene) are included. A substance is only accepted as "preliminarily identified" if the identified peak shows a minimum match factor of 80 and is confirmed as a match by an experienced mass spectrometry expert.

[0324] In this study, the expression "below the detection limit (<LOD)" refers to cases where the match factor is below 80 (AMDIS) or the peak itself cannot even be identified. The results only refer to the measured samples, measurement times, and applied parameters.

[0325] j) CIELAB color space (L*a*b*)

[0326] In the CIE L*a*b* uniform color space measured according to DIN EN ISO 11664-4, the color coordinates are: L*—lightness coordinate; a*—red / green coordinate, where +a* represents red and -a* represents green; b*—yellow / blue coordinate, where +b* represents yellow and -b* represents blue. The L*, a* and b* coordinate axes define the three-dimensional CIE color space. Standard Konica / Minolta colorimeter CM-3700A.

[0327] k) Odor VDA270-B3

[0328] VDA 270 is to determine the odor characteristics of decorative materials in motor vehicles. In this study, the odor was determined according to VDA 270 (2018) variable B3. After lifting the can lid as little as possible, each assessor evaluated the odor of each sample according to the VDA 270 scale. The six scales consist of the following levels: Level 1: Imperceptible; Level 2: Perceptible, non-interfering; Level 3: Clearly perceptible, but not interfering; Level 4: Interference; Level 5: Strong interference; Level 6: Unacceptable. The assessors remained calm during the evaluation and were not allowed to be biased by discussing personal results during the test. They were also not allowed to adjust their evaluation after testing another sample. For statistical reasons (and as accepted by VDA 270), assessors must use all steps in their evaluation. Therefore, the odor level is based on the average of all individual evaluations and is rounded to an integer.

[0329] l) Limonene detection

[0330] Quantification of limonene can be performed using solid phase microextraction (HS-SPME-GC-MS) by standard addition.

[0331] 50mg of ground sample was weighed into a 20mL headspace vial, and after adding different concentrations of limonene and a glass-coated magnetic stirring bar, the vial was closed with a magnetic cap lined with silicone / PTFE. Microcapillaries (10pL) were used to add a known concentration of diluted limonene standards to the sample. Addition of 0ng, 2ng, 20ng and 100ng was equal to 0mg / kg, 0.1mg / kg, 1mg / kg and 5mg / kg limonene, and when added, the standard amount of 6.6mg / kg, 11mg / kg and 16.5mg / kg limonene was used in combination with some samples tested in this application. For quantitative purposes, ions-93 obtained in SIM mode were used. Enrichment of volatile fractions was carried out by headspace solid phase microextraction with 2cm stable flexible 50 / 30pm DVB / Carboxen / PDMS fiber at 60°C for 20 minutes. Desorption was directly carried out in the heated injection port of the GCMS system at 270°C.

[0332] GCMS parameters:

[0333] Column: 30m HP 5MS 0.25*0.25

[0334] Syringe: Splitless, with 0.75 mm SPME liner, 270 °C

[0335] Temperature program: -10℃ (1 minute)

[0336] Carrier gas: Helium 5.0, linear velocity of 31 cm / s, constant flow

[0337] MS: Single quadrupole, direct interface, 280°C interface temperature

[0338] Acquisition: SIM scan mode

[0339] Scan parameters: 20amu to 300amu

[0340] SIM parameters: m / Z 93, 100 ms dwell time

[0341] m) Fatty acid detection

[0342] Quantification of fatty acids was performed using headspace solid phase microextraction (HS-SPME-GC-MS) by standard addition.

[0343] 50mg of ground sample is weighed in 20mL headspace vial, after adding different concentrations of limonene and glass-coated magnetic stirring bar, the vial is closed with a magnetic cover lined with silicone / PTFE. Use 10 μ L microcapillaries to add known concentrations of diluted free fatty acid mixture (acetic acid, propionic acid, butyric acid, valeric acid, caproic acid and octanoic acid) standards in sample at three different levels. Add 0ng, 50ng, 100ng and 500ng to equal each independent acid of 0mg / kg, 1mg / kg, 2mg / kg and 10mg / kg. For quantitative, for all acids except propionic acid, use ion 60 obtained under SIM mode, propionic acid uses ion 74.

[0344] GCMS parameters:

[0345] Column: 20m ZB Wax plus 0.25*0.25

[0346] Syringe: Split 5:1, with glass lined splitter liner, 250°C

[0347] Temperature program: 40℃ (1 minute) @6℃ / min to 120℃, @15℃ to 245℃ (5 minutes)

[0348] Carrier gas: Helium 5.0, linear velocity of 40 cm / s, constant flow

[0349] MS: Single quadrupole, direct interface, 220°C interface temperature

[0350] Acquisition: SIM scan mode

[0351] Scan parameters: 46amu to 250amu, 6.6 scans / second

[0352] SIM parameters: m / z 60, 74, 6.6 scans / sec

[0353] n) The presence of polyamide-6 and polystyrene

[0354] By FTIR spectroscopy using 1601 cm -1 (PS) and 3300cm -1 Absorption of the band at (PA6).

[0355] o) Determination of contaminants on the board

[0356] The plates were injection moulded and had dimensions of 150 mm x 80 mm x 2 mm. High resolution images (photographs) were then taken of 5 plates (which were placed close to each other). The images were then analysed by software allowing automatic counting of the number of visual defects (by naked eye) due to contaminants.

[0357] p) Dynamic shear measurement (η(2.7 kPa) and η(300 rad / sec))

[0358] The characterization of polymer melts by dynamic shear measurements complies with ISO standards 6721-1 and 6721-10. The measurements were performed on an Anton Paar MCR501 stress-controlled rotational rheometer equipped with a 25 mm parallel plate geometry. The measurements were performed on compression molded plates using a nitrogen atmosphere and setting the strain in the linear viscoelastic range. The oscillatory shear tests were performed at 230°C, applying a frequency range of 0.01 rad / sec to 600 rad / sec and setting a gap of 1.3 mm.

[0359] In a dynamic shear experiment, the probe is subjected to uniform deformation under sinusoidally varying shear strain or shear stress (strain-controlled mode and stress-controlled mode, respectively). For a controlled strain experiment, the probe is subjected to a sinusoidal strain that can be expressed by:

[0360] γ(t)=γ0sin(ωt) (1)

[0361] If the applied strain is in the linear viscoelastic range, the resulting sinusoidal stress response can be given by:

[0362] σ(t)=σ0sin(ωt+δ) (2)

[0363] in

[0364] σ0 and γ0 are stress amplitude and strain amplitude respectively

[0365] ω frequency is the angular frequency

[0366] δ is the phase shift (loss angle between applied strain and stress response)

[0367] t is time

[0368] Dynamic test results are usually expressed by several different rheological functions, namely shear storage modulus G', shear loss modulus G", complex shear modulus G*, complex shear viscosity η*, dynamic shear viscosity η', out-of-phase component of complex shear viscosity η", and loss tangent tan δ, which can be expressed as follows:

[0369]

[0370] G * =G'+iG"[Pa] (5)

[0371] η * =η′-iη"[Pa.s] (6)

[0372]

[0373] η(x kPa) is determined according to Equation 9.

[0374] η(x kPa)=for (G * = x kPa) * [Pa.s] (9)

[0375] For example, η(2.7 kPa) is defined by the complex viscosity value determined for a complex modulus value equal to 2.7 kPa.

[0376] η (x rad / second) is determined according to Equation 10.

[0377] η(xrad / sec) = η for (ω = xrad / sec) * [Pa.s] (10)

[0378] For example, η(300 rad / sec) is defined by the complex viscosity value determined at a frequency sweep of 300 rad / sec.

[0379] q) The shear thinning factor (STF) is defined as

[0380]

[0381] This value was determined by a single-point interpolation procedure as defined by the Rheoplus software. In the case where a given G* value was not achieved experimentally, this value was determined by extrapolation using the same procedure as before. In both cases (interpolation or extrapolation), the options "Interpolate from y value to x value by parameter" and "Logarithmic interpolation type" from Rheoplus were applied ([1] Rheological characterization of polyethylene fractions" Heino, E.L., Lehtinen, A., Tanner J., J., Neste Oy, Porvoo, Finland, Theor.Appl.Rheol., Proc.Int.Congr.Rheol, 11th (1992), 1, 360-362; [2] The influence of molecular structure on somerheological properties of polyethylene", Heino, EL, Borealis Polymers Oy, Porvoo, Finland, Annual Transactions of the Nordic Rheology Society, 1995.) [3] Definition of terms relating to the non-ultimate mechanical properties ofpolymers, Pure & Appl. Chem., Volume 70, Issue 3, Pages 701 to 754, 1998.)

[0382] r) Large Amplitude Oscillatory Shear (LAOS)

[0383] The study of nonlinear viscoelastic behavior under shear flow is performed using large amplitude oscillatory shear. The method requires the application of a sinusoidal strain amplitude γ0 applied at a given angular frequency ω for a given time t. If the applied sinusoidal strain is high enough, a nonlinear response is generated. In this case, the stress σ is a function of the applied strain amplitude, time, and angular frequency. Under these conditions, the nonlinear stress response is still a periodic function; however, it can no longer be represented by a single harmonic sinusoid. The stress generated by the nonlinear viscoelastic response [0-0] can be represented by a Fourier series including higher harmonic contributions:

[0384] σ(t,ω,γ0)=γ0.Σ n [G′ n (ω,γ0).sin(nωt)+G" n (ω,γ0).cos(nωt)] (1)

[0385] Where, σ-stress response

[0386] t-time

[0387] ω-Frequency

[0388] γ0-strain amplitude

[0389] n - number of harmonics

[0390] G' n -nth order elastic Fourier coefficient

[0391] G” n -nth order viscosity Fourier coefficient

[0392] Large amplitude oscillatory shear (LAOS) was applied to analyze the nonlinear viscoelastic response. Time sweep measurements were performed on the RPA 2000 rheometer from Alpha Technologies connected to a standard double cone die. During the measurement process, the test box was sealed and a pressure of about 6MPa was applied. A temperature of 190°C, an angular frequency of 0.628rad / second, and a strain of 1000% were applied to carry out the LAOS test. In order to ensure that steady-state conditions were reached, the nonlinear response was determined only after at least 20 cycles were completed for each measurement. The large amplitude oscillatory shear nonlinear factor (LAOS_NLF) is defined as follows:

[0393]

[0394] Where G'1 - first order Fourier coefficient

[0395] G'3 - third order Fourier coefficient

[0396] (JMDealy, KFWissbrun, Melt Rheology and Its Role in Plastics Processing: Theory and Applications; edited by Van Nostrand Reinhold, New York (1990); S. Filipe, Non-Linear Rheology of Polymer Melts, AIP Conference Proceedings 1152, pages 168 to 174 (2009); M. Wilhelm, Macromol. Mat. Eng. 287, 83-105 (2002); S. Filipe, K. Hofstadler, K. Klimke, ATTran, Non-Linear Rheological Parameters for Characterization of Molecular Structural Properties in Polyolefins, Proceedings of Annual European Rheology Conference,135(2010); S.Filipe,K.Klimke,ATTran,J.Reussner,Proceedings of Novel Non-Linear Rheological Parameters for Molecular Structural Characterization of Polyolefins, Novel Trends in Rheology IV, Zlin, Check Republik (2011); K. Klimke, S. Filipe, ATTran, Non-linear rheological parameters for characterization of molecular structural properties in polyolefins, Proceedings of European Polymer Conference, Granada, Spain (2011)).

[0397] In Table 1, several examples (Comparative Examples - CE; Inventive Examples - IE) are summarized.

[0398] Different blends of recycled materials are used. The blends are characterized by the following properties:

[0399] Blend A1: C2 (CF) content 2 wt% to 3 wt%, C2 (SF) content 24 wt% to 25 wt%, C3 (CF) content 95 wt% to 96 wt%, MFR2 14 g / 10 min to 17 g / 10 min, tensile modulus 1300 MPa to 1450 MPa, impact strength (Charpy test 23 ° C) 5 KJ / m 2 Up to 6KJ / m 2 .

[0400] Blend A2: C2 (CF) content 2 wt% to 3 wt%, C2 (SF) content 17 wt% to 18 wt%, C3 (CF) content 97 wt% to 98 wt%, MFR2 7 g / 10 min to 8 g / 10 min, tensile modulus 1250 MPa to 1300 MPa, impact strength (Charpy test 23 ° C) 8 KJ / m 2 Up to 9KJ / m 2 .

[0401] The blend A1 / A2 is obtained by a method for obtaining mixed plastic polypropylene as described above, which method includes the following steps: further sorting old ("old style") mainly colorless / natural plastic products which can be identified by discoloration (e.g., significant yellowing) and / or significant scratches of the mainly colorless / natural plastic products.

[0402] In the comparative examples, additional recyclate blends of mixed plastic polypropylene were used. These additional blends are characterized by a higher ethylene C2 content.

[0403] Blend A3: Total C2 content 9 wt% to 10 wt%, C2(CF) content 8 wt% to 12 wt%, C2(SF) content 29 wt% to 34 wt%,

[0404] Blend A3 is a post-consumer recycled polypropylene based material with a 920 kg / m 3 Density (determined according to DIN EN ISO 1183); melt flow rate of 14.1 g / 10 min (determined according to DIN EN ISO 1133, 230°C / 2.16 kg); moisture content of less than 0.1% (determined via a moisture infrared analyzer, 105°C); tensile modulus of greater than 1100 MPa (determined according to DIN EN ISO 527, 1 mm / min); yield stress of greater than 25 MPa (determined according to DIN EN ISO 527, 50 mm / min); and tensile strain of greater than 180% (determined according to DIN EN ISO 527, 50 mm / min).

[0405] Blend A4: total C2 content 10 wt% to 12 wt%, C2 (CF) content 7 wt% to 10 wt%, C2 (SF) content 24 wt% to 34 wt%,

[0406] Blend A4 is a post-consumer recycled polypropylene based material with a 916 kg / m 3 Density (determined according to DIN EN ISO 1183); melt flow rate of 36 g / 10 min (determined according to DIN EN ISO 1133, 230°C / 2.16 kg); moisture content of less than 0.1% (determined via a moisture infrared analyzer, 105°C); tensile modulus of greater than 1100 MPa (determined according to DIN EN ISO 527, 1 mm / min); yield stress of greater than 24 MPa (determined according to DIN EN ISO 527, 50 mm / min); and tensile strain of greater than 18% (determined according to DIN EN ISO 527, 50 mm / min).

[0407] Table 1 relates to polyolefin compositions comprising:

[0408] - Comparative Example (CE1): a polypropylene homopolymer (PPH-2); a blend of recycled materials (Blend A1) and 20 wt.% glass fibers;

[0409] - Comparative example (CE2): blend of recycled material (Blend A1) and 30 wt.% glass fibers;

[0410] - Comparative Example (CE3): a blend of a polypropylene homopolymer (PPH-1), recycled material (Blend A1) and 30 wt.% glass fibers;

[0411] - Comparative Example (CE4): a polypropylene homopolymer (PPH-2), a polypropylene block copolymer (BCP-1) and 40 wt% glass fibers;

[0412] - Comparative example (CE5): blend of recycled material (Blend A1) and 40 wt.% glass fibers;

[0413] - Comparative example (CE6): a blend of a polypropylene homopolymer (PPH-2), a polypropylene block copolymer (BCP-1), recycled material (Blend A3) and 40 wt.% glass fibers;

[0414] - Comparative example (CE7): a blend of a polypropylene homopolymer (PPH-2), a polypropylene block copolymer (BCP-1), recycled material (Blend A4) and 40 wt.% glass fibers;

[0415] - Inventive example (IE1): a blend of a polypropylene homopolymer (PPH-2), a polypropylene block copolymer (BCP-1), recycled material (Blend A1) and 40 wt% glass fibers;

[0416] - Inventive example (IE2): a blend of a polypropylene homopolymer (PPH-2), a polypropylene block copolymer (BCP-1), recycled material (Blend A1) and 40 wt% glass fibers;

[0417] - Inventive Example (IE3): a blend of a polypropylene homopolymer (PPH-2), a polypropylene block copolymer (BCP-1), recycled material (Blend A2) and 40 wt% glass fibers;

[0418] Glass fibers can be obtained from one of the following suppliers: OC (Owens Corning), PPG / NEG, Johns Manville, 3B, Jushi, Taiwan Glass (China), Camelyaf, CPIC, Taishan, using glass fiber 1.2 (average length 4 mm, average diameter 13 μm) and glass fiber 4.1 (average length 4.5 mm, average diameter 13 μm).

[0419] The following additives were used: antioxidants: AO1 (Irganox 1010 (FF)), AO2 (Irganox B 225 (FF)), AO3 (Irganox PS-802FL); black pigment (Plasblak PE6121, commercially available from Cabot); dosing agent: HC001A-B1, PP homopolymer powder; coupling agent: AP 1.5, polypropylene highly functionalized with maleic anhydride.

[0420] As can be seen from Table 1, the values ​​of tensile strength measured for IE1, IE2, IE3 are higher than those for CE1 to CE3 and CE5 to CE7. In addition, IE1, IE2, and IE3 provide a tensile modulus of >8.8 GPa, significantly higher than that provided by CE1 to CE3. In addition, the Charpy impact strength of IE1 to IE3 is higher than any of CE1 to CE3 and CE6 to CE7. Only CE4 (an example without any recycled material blend) has a better tensile modulus and tensile strength than any of IE1 to IE3.

[0421] It is noted that using the recyclate blends of IE1 to IE3 with lower C2 content provides polyolefin compositions with improved tensile strength and impact strength (Charpy) compared to the recyclates in both CE6 to CE7 with higher C2 content.

[0422]

[0423]

Claims

1. A polyolefin composition comprising: a) 5 to 30 wt.-% (based on the total weight of the polyolefin composition) of at least one polypropylene homopolymer, b) 1 to 15 wt. % (based on the total weight of the polyolefin composition) of at least one polypropylene block copolymer, c) 20 wt% to 50 wt% (based on the total weight of the polyolefin composition) of a mixed plastic polypropylene blend of recycled material, the mixed plastic polypropylene blend having: (i) a crystalline fraction (CF) content determined according to CRYSTEX QC analysis in the range of 85.0 wt.-% to 95.0 wt.-%, and (ii) a soluble fraction (SF) content determined according to CRYSTEX QC analysis in the range of 5.0 wt.-% to 15.0 wt.-%, wherein (iii) The crystalline fraction (CF) is quantitatively 13 The propylene content (C3(CF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is in the range of 93.0 wt. % to 99.0 wt. %, and wherein (iv) The crystalline fraction (CF) is quantitatively 13 An ethylene content (C2(CF)) in the range of 1.0 wt% to 6.0 wt% as determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy; and (v) the intrinsic viscosity (iV(SF)) of the soluble fraction (SF) is in the range of 1.0 dl / g to 2.0 dl / g, and in (vi) The CIELAB color space (L*a*b*) of the mixed plastic polypropylene blend is: -L* of 30 to 97.0, especially 50 to 97.0; --a* from 10.0 to 16.0, especially from -8 to <10.0; - b* of 5.0 to 25.0, in particular -2 to 22.0, d) 35 to 55 wt. % (based on the total weight of the polyolefin composition) of glass fibers; and optionally further additives, wherein the sum of all constituents always amounts to 100% by weight, The polyolefin composition is characterized in that: - a tensile modulus at 23°C of at least 7000 MPa (ISO 527-2), - a tensile stress at yield at 23°C of at least 90 MPa (ISO 527-2), and - At least 8.5 kJ / m 2 Impact strength (ISO179-1, Charpy 1eA+23℃).

2. The polyolefin composition according to claim 1, characterized in that the polyolefin composition comprises: a) 8 to 28 wt.-%, more preferably 9 to 22 wt.-% (based on the total weight of the polyolefin composition) of said at least one polypropylene homopolymer, b) 3 to 10 wt.-%, more preferably 4 to 8 wt.-%, based on the total weight of the polyolefin composition, of at least one polypropylene block copolymer, c) 25 to 45 wt. %, more preferably 30 to 42 wt. % (based on the total weight of the polyolefin composition) of said mixed plastic polypropylene blend; d) 38 to 50 wt. %, preferably 38 to 45 wt. % (based on the total weight of the polyolefin composition) of glass fibers; and optionally further additives, wherein the sum of all ingredients adds up to 100% by weight.

3. The polyolefin composition according to claim 1 , characterized in that the melt flow rate MFR2 (ISO 1133, 2.16 kg, 230° C.) is at least 3.0 g / 10 min, preferably at least 3.5 g / 10 min, more preferably at least 4.0 g / 10 min, in particular in the range of 3.0 g / 10 min to 15 g / 10 min, preferably 3.5 g / 10 min to 10 g / 10 min, more preferably 4.0 g / 10 min to 10 g / 10 min.

4. The polyolefin composition according to claim 1 , characterized in that the tensile modulus (ISO 527-2) is at least 8000 MPa, preferably at least 8500 MPa, more preferably at least 9000 MPa, in particular in the range of 8000 MPa to 15000 MPa, more in particular in the range of 8000 MPa to 10000 MPa.

5. The polyolefin composition according to claim 1 , characterized in that the tensile stress at yield (50 mm / min, ISO 527-2) at 23° C. is at least 95 MPa, preferably at least 100 MPa, more preferably at least 105 MPa, in particular in the range of 90 MPa to 200 MPa, more in particular in the range of 100 MPa to 150 MPa.

6. The polyolefin composition according to claim 1 , characterized in that the tensile stress at break (50 mm / min, ISO 527-2) at 23° C. is at least 90 MPa, preferably at least 95 MPa, more preferably at least 100 MPa, even more preferably at least 105 MPa, in particular in the range of 90 MPa to 200 MPa, more in particular in the range of 100 MPa to 150 MPa.

7. The polyolefin composition according to claim 1, characterized in that the impact strength (ISO 179-1, Charpy 1eA+23° C.) is at least 9.0 kJ / m 2 , preferably at least 9.5 kJ / m 2 , especially at 9.0 kJ / m 2 Up to 15.0kJ / m 2 in the range of 9.5 kJ / m 2 Up to 13.0 kJ / m 2 in the range of 10.0 kJ / m 2 Up to 12.0 kJ / m 2 within the range.

8. Polyolefin composition according to one of the preceding claims, characterised in that the at least one polypropylene homopolymer comprises: a polypropylene homopolymer (PPH-1) having a melt flow rate MFR2 (230°C, 2.16 kg, measured according to ISO 1133) in the range of 5 to 15 g / 10 min, preferably in the range of 5 to 10 g / 10 min, more preferably 8 g / 10 min; and / or A polypropylene homopolymer (PPH-2) having a melt flow rate MFR2 (230°C, 2.16 kg, measured according to ISO 1133) in the range of 10 to 30 g / 10 min, preferably 15 to 25 g / 10 min, more preferably 20 g / 10 min.

9. The polyolefin composition according to claim 1 , wherein the at least one polypropylene block copolymer has a melt flow rate (230° C. / 2.16 kg) of at least 0.2 g / 10 min, preferably at least 0.3 g / 10 min, in particular in the range of 0.2 to 2.0 g / 10 min, more in particular in the range of 0.2 to 1.5 g / 10 min.

10. The polyolefin composition according to claim 1, characterized in that the mixed plastic polypropylene blend (blend A1) has: (i) a crystalline fraction (CF) content determined according to CRYSTEX QC analysis in the range of 86.0 wt.-% to 94.0 wt.-%, more preferably 90.0 wt.-% to 94.0 wt.-%, and (ii) a soluble fraction (SF) content determined according to CRYSTEX QC analysis in the range of 6.0 wt.-% to 14.0 wt.-%, more preferably 6.0 wt.-% to 10.0 wt.-%, wherein (iii) The crystalline fraction (CF) is quantitatively 13 The propylene content (C3(CF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is in the range of 93.0 wt.-% to 99.0 wt.-%, preferably 95.0 wt.-% to 98.0 wt.-%; and wherein (iv) The crystalline fraction (CF) is quantitatively 13 An ethylene content (C2(CF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is in the range of 1 wt% to 7 wt%, more preferably 2.0 wt% to 5.0 wt%, even more preferably 2.5 wt% to 3.5 wt%; and (v) the intrinsic viscosity (iV(SF)) of the soluble fraction (SF) is in the range of 1.2 dl / g to less than 1.8 dl / g, preferably 1.40 dl / g to 1.70 dl / g; in (vi) The CIELAB color space (L*a*b*) of the mixed plastic polypropylene blend is: - L* from 40 to 85, preferably from 50 to 75; --a* of 8.00 to 10, more preferably -5.0 to 0.0; b* of -0.0 to below 10.0, more preferably 0.0 to below 5.

00.

11. Polyolefin composition according to one of the preceding claims, characterised in that the mixed plastic polypropylene blend (blend A2) has: (i) a crystalline fraction (CF) content determined according to CRYSTEX QC analysis in the range of 86.0 wt.-% to 94.0 wt.-%, preferably 91.0 wt.-% to 94.0 wt.-%, and (ii) a soluble fraction (SF) content determined according to CRYSTEX QC analysis in the range of 6.0 wt.-% to 14.0 wt.-%, more preferably 6.0 wt.-% to 9.0 wt.-%, wherein (iii) The crystalline fraction (CF) is quantitatively 13 The propylene content (C3(CF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is in the range of 95.0 wt.-% to 99.0 wt.-%, preferably 96.0 wt.-% to 98.0 wt.-%, and wherein (iv) The crystalline fraction (CF) is quantitatively 13 An ethylene content (C2(CF)) determined by FT-IR spectroscopy calibrated with C-NMR spectroscopy is in the range of 1.0 to 5.0 wt. %, preferably 2.0 to 4.0 wt. %, more preferably 2.5 to 3.5 wt. %; and (v) the intrinsic viscosity (iV(SF)) of the soluble fraction (SF) is in the range of 1.1 dl / g to less than 1.5 dl / g, preferably 1.25 dl / g to less than 1.45 dl / g; in (vi) The CIELAB color space (L*a*b*) of the mixed plastic polypropylene blend is: - L* from 72.0 to 97.0, preferably from 80.0 to 97.0; --a* from 5.0 to 0.0; -0.0 to b* below 22.

0.

12. The polyolefin composition according to claim 1 , wherein the glass fibers have a length of 2.0 to 10.0 mm, preferably in the range of 2.0 to 8.0 mm, even more preferably in the range of 2.0 to 6.0 mm, and a diameter of 5 to 20 μm, more preferably 8 to 18 μm, still more preferably 8 to 15 μm.

13. Polyolefin composition according to one of the preceding claims, characterized in that it comprises at least one coupling agent, in particular a polypropylene functionalized with maleic anhydride (MAH).

14. An article comprising the polyolefin composition according to one of the preceding claims.

15. The article of claim 14, wherein the article is one of a structural product, a pump, a fan, an appliance, an automotive part, a pipe, and a fitting.

Images