Polyolefin composition comprising heterophasic polypropylene polymers and recycled plastic materials for pipes
A polyolefin composition combining heterophasic propylene copolymer and recycled polypropylene blend addresses quality issues, ensuring performance meets pipe industry standards by maintaining or improving thermomechanical properties.
Patent Information
- Application Number
- PCT/EP2025/069694
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-07-11
- Filing Date
- 2025-07-10
- Publication Date
- 2026-01-15
AI Technical Summary
Existing polyolefin compositions, particularly those containing recycled plastics, suffer from inferior quality due to degradation and contamination, limiting their use in applications such as pipes, and there is a need for compositions that maintain or improve thermomechanical properties while incorporating significant amounts of recycled materials to meet industry standards.
A polyolefin composition comprising 40-90 wt% of a heterophasic propylene copolymer with specific ethylene content, melt flow rate, and soluble fraction, combined with 10-60 wt% of a mixed-plastics polypropylene blend from recycled materials, along with optional additives, to achieve properties comparable to virgin polymers.
The composition maintains or enhances thermomechanical properties, allowing it to meet pipe industry standards for pressure tests, impact resistance, and ring stiffness, even with a significant recycled content.
Smart Images

Figure IMGF000021_0001 
Figure IMGF000028_0001 
Figure IMGF000031_0001
Abstract
Description
[0001] Polyolefin composition comprising heterophasic polypropylene polymers and recycled plastic materials for pipes
[0002] The invention relates to a polyolefin composition comprising at least one heterophasic polypropylene copolymer, and recycled plastic material, to an article, in particular a pipe, comprising the polyolefin composition and a process for preparing such polyolefin composition.
[0003] Description
[0004] Polyolefins, in particular polyethylene and polypropylene are increasingly consumed in large amounts in a wide range of applications, including packaging for food and other goods, fibres, automotive components, and a great variety of manufactured articles. Polyethylene based materials are a particular problem as these materials are extensively used in packaging. Taking into account the huge amount of waste collected compared to the amount of waste recycled back into the stream, there is still a great potential for intelligent reuse of plastic waste streams and for mechanical recycling of plastic wastes.
[0005] With their inherent versatility, plastics play crucial roles in a sustainable and resource-efficient economy. However, as more and more plastic has been created and used in a mode of linear economy, plastic waste is nowadays considered a serious social problem. For that, it is important to form a circular economy that brings plastic waste back to a second life, i.e., to recycle it. This not only avoids leaving plastic waste in the environment but also recovers its value.
[0006] The European Commission confirmed in 2017 that it would focus on plastics production and use. The EU goals are that 1 ) by 2025 at least 50% of all plastics packaging in the EU should be recycled and 2) by 2030 all plastic packaging placed in the EU market is reusable or easily recycled. This pushes the brand owners and plastic converters to pursue solutions with recyclates or virgin / recyclate blends. More recently, in 2021 , EU agreed tax on plastic packaging waste. The tax, introduced as of 1 January 2021 , is calculated on the weight of nonrecycled plastic packaging waste "with a call rate of €0.80 / kilogram with a mechanism to avoid excessively regressive impact on national contributions.”
[0007] It is therefore urgently needed to find ways of recycling plastic waste. However, recycled plastics are normally inferior to virgin plastics in their quality due to degradation, contamination and mixing of different plastics. Generally, recycled quantities of polypropylene on the market are mixtures of both polypropylene (PP) and polyethylene (PE), this is especially true for post-consumer waste streams. Moreover, commercial recyclates from post-consumer waste sources are conventionally cross-contaminated with non-polyolefin materials such as polyethylene terephthalate, polyamide, polystyrene or non-polymeric substances like wood, paper, glass or aluminum. These cross-contaminations drastically limit final applications of recycling streams such that no profitable final uses remain. The better the quality of the recyclate is, the less available it is and the more expensive it is.
[0008] The quality issue in recyclates compared to the virgin ones can be to some extent overcome by mixing the recyclates with virgin polymers. Compositions comprising virgin polymers (Le. polymers used for the first time) and recycled mixed plastics have been studied.
[0009] EP3802689B1 refers to a process to produce a composition comprising polypropylene recyclates and a polypropylene resin and possibly a polyethylene resin, an elastomer and fillers. The polypropylene recyclate is characterized by a melt flow rate between 7 and 70 g / 10 min.
[0010] EP3715410 A1 refers to a composition containing polypropylene rich recyclate and a heterophasic copolymer with a low melt flow rate and a low amount of xylene solubles. The polypropylene recyclate is characterized by a melt flow rate of at least 8 g / 10 min.
[0011] Typically products produced form such recycled polymer compositions tend to suffer from crazes and cracks after a short lifetime. Pipes based on such recycled polymer compositions have further inadmissible slow crack performance.
[0012] Though there is not yet any regulation concerning the use of recycled PP (rPP) in pipe industry. The current standards for non-pressure PP pipes are expected to be modified in 2024 to allow incorporation of post-consumer recycled (PGR) PP, and not only production scraps, into PP pipes. The incorporation of PGR PP is expected to deteriorate the pipe performance, hence it is essential to find compositions that meet the requirements of pipe performance in the current industry standards (e.g., EN 1451 -1 and EN 1852-1 ), i.e., pipe ring stiffness of at least 8 kN / m2, pipe impact resistance H5o of at least 1000 mm at -10°C and 4 kg’s load, duration of pipe pressure tests of at least 140 h at 80°C and 4.2 MPa as well as at least 1000 h at 95°C and 2.5 MPa. Thus, it was an object of the invention to provide a polyolefin composition wherein at least a part of virgin polyolefin is replaced by polyolefin material recovered from waste plastic material while thermomechanical properties of such a polyolefin composition are at least maintained or even improved.
[0013] It is in particular an object of the present invention to provide a composition which is suitable for pipe applications complying with the standards of pipes, especially in terms of the pipe pressure test, even though said composition contains a recycled polymer composition in significant amount.
[0014] This object has been solved by providing a polyolefin composition comprising: a) 40-90 wt% (based on the overall weight of the polyolefin composition) of at least one heterophasic propylene copolymer (HECO,) having a total ethylene (C2) content (as determined according to Crystex analysis described in the method section) in the range from 0.5 to 6.0 wt.-% (based on the total weight of the heterophasic propylene copolymer), a soluble fraction (SF) determined according to Crystex analysis described in the method section in the range from 2.0 to 15.0 wt% (based on the total weight of the heterophasic propylene copolymer), and a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C) in the range from 0.1 to 1.0 g / 10 min; b) 10-60 wt% (based on the overall weight of the polyolefin composition) of a mixed- plastics polypropylene blend of recycled material (Blend A) having a soluble fraction (SF) determined according to Crystex analysis as described in the method section in the range from 2.0 to 8.0 wt% (based on the total weight of the mixed-plastic polypropylene blend of recycled material), a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C, ) in the range from 1 .0 to 15.0 g / 10 min, and one or more, preferably all of the following properties determined with camera detection from Optical Control Systems (OCS): an OCS gel index (determined as described in the method section )of less than 65000
[0015] OCS others (> 1000 pm, determined as described in the method section) of less than 1500 1 / m2,
[0016] OCS contaminations (>1000 pm, determined as described in the method section) of less than 85 1 / m2, and / or
[0017] OCS gel (>1000 pm, determined as described in the method section) of less than 300 1 / m2, and c) ) optionally further additives (based on the overall weight of the polyolefin composition), wherein the sum of all ingredients always adds up to 100 wt%.
[0018] Thus, a polyolefin composition is provided that contains recycled plastic material and virgin heterophasic polypropylene polymer. This combination provides a composition wherein at least a part of virgin polymer is replaced by recycled material, wherein properties are almost comparable to the virgin polymers. Such compositions are applicable for pipes.
[0019] The recycled material, i.e., PP recyclate (rPP), used for in the present polyolefin composition is obtained from recycled waste stream of recycled post-consumer waste.
[0020] For the purposes of the present description and of the subsequent claims, the term “recycled” is used to indicate that the material is recovered from post-consumer waste and / or postindustrial waste, wherein recycled material from post-consumer waste is preferred . Namely, post-consumer waste refers to objects having completed at least a first use cycle (or life cycle), i.e. having already served their first purpose and been through the hands of a consumer; while post-industrial waste refers to the manufacturing scrap which does normally not reach a consumer. In the gist of the present invention “recycled polymers” may also comprise up to 20 wt.-%, preferably up to 18 wt.-%, more preferably up to 16 wt.-% and even more preferably up to 14 wt.-%, most preferably up to 12 wt. -%, based on the overall weight of the recycled polymer of other components originating from the first use. Type and amount of these components influence the physical properties of the recycled polymer. The physical properties given below refer to the main component of the recycled polymer.
[0021] As described also further below, typical other components originating from the first use are thermoplastic polymers, like polystyrene (PS) and polyamide 6 (PA 6), talc, chalk, ink, wood, paper, limonene and fatty acids. The content of PS and PA 6 in recycled polymers can be determined by Fourier Transform Infrared Spectroscopy (FTIR) and the content of talc, chalk, wood and paper may be measured by Thermogravimetric Analysis (TGA).
[0022] The term “virgin” denotes the newly produced materials and / or objects prior to first use and not being recycled. In case that the origin of the polymer is not explicitly mentioned the polymer is a “virgin” polymer.
[0023] It is to be understood that the material used for Crystex analysis is based on material without any additives such as fillers, pigments, non-soluble polymers e.g. PET, etc. (see also details to Crystex analysis in the method section), i.e. only material that can be dissolved in 1 , 2, 4, tricholorbenzene at 170°C is used for Crystex analysis. Any non-dissolved material is removed.
[0024] The ingredients of the present polyolefin composition will be described now in more detail.
[0025] Heterophasic polypropylene virgin polymer (HECO)
[0026] A heterophasic propylene copolymer comprises a matrix (M) being a (semicrystalline) polypropylene and an elastomeric propylene copolymer (EPC). The expression "heterophasic propylene copolymer" or "heterophasic" as used in the present invention indicates that the elastomeric propylene copolymer is (finely) dispersed in the (semicrystalline) polypropylene.
[0027] In other words, the (semicrystalline) polypropylene constitutes a matrix in which the elastomeric propylene copolymer forms inclusions in the matrix, i.e. in the (semicrystalline) polypropylene. Thus, the matrix contains (finely) dispersed inclusions being not part of the matrix and said inclusions contain the elastomeric propylene copolymer. The term "inclusion" according to this invention shall preferably indicate that the matrix and the inclusion form different phases within the heterophasic propylene copolymer (HECO), said inclusions are for instance visible by high resolution microscopy, like electron microscopy or atomic force microscopy. The heterophasic propylene copolymer (HECO) according to this invention has a rather high molecular weight and rather low amount of rubber, i.e. of the elastomeric propylene copolymer. In one embodiment, the at least one heterophasic propylene copolymer (HECO) comprises a propylene homopolymer (PPH) as (semicrystalline) matrix and a propylene-ethylene rubber as elastomeric propylene copolymer (EPC).
[0028] The polypropylene matrix (M) is preferably a random propylene copolymer or a propylene homopolymer, the latter being especially preferred. The expression “propylene homopolymer relates to a polypropylene that consists of more than 99.5 wt%, preferably of more than or at least of 99.7 wt% of propylene units. In a preferred embodiment only propylene units are detectable in the propylene homopolymer.
[0029] The elastomeric propylene copolymer (EPC) comprises units derived from propylene and ethylene and / or C4 to C20 alpha-olefins, more preferably from ethylene and / or C4 to C10 alpha-olefins and most preferably from ethylene.
[0030] The heterophasic propylene copolymer (HECO) can contain typical additives known in the art, like antioxidants or process additives. It is especially preferred that the heterophasic propylene copolymer (HECO) is alpha-nucleated, i.e. contains an alpha-nucleating agent.
[0031] The alpha-nucleating agent is preferably selected from the group consisting of
[0032] (i) salts of monocarboxylic acids and polycarboxylic acids, e.g. sodium benzoate or aluminum tert-butylbenzoate, and
[0033] (ii) dibenzylidenesorbitol (e.g. 1 ,3 : 2,4 dibenzylidenesorbitol) and C1 -C8-alkylsubstituted dibenzylidenesorbitol derivatives, such as methyldibenzylidenesorbitol, ethyldibenzylidenesorbitol or dimethyldibenzylidenesorbitol (e.g. 1 ,3 2,4 di(methylbenzylidene) sorbitol), or substituted nonitol-derivatives, such as 1 ,2, 3, -trideoxy 4,6:5,7-bis-O-[(4-propylphenyl) methylene]-nonitol, and
[0034] (iii) salts of diesters of phosphoric acid, e.g. sodium 2,2’-methylenebis (4,6-di-tert-butylphenyl) phosphate or aluminum- hydroxy-bis[2,2’-methylene-bis(4,6-di-t-butylphenyl)phosphate], and
[0035] (iv) vinylcycloalkane polymer or vinylalkane polymer, and
[0036] (v) mixtures thereof.
[0037] The at least one heterophasic propylene copolymer (HECO) may have a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C) in the range from 0.1 to 0.9 g / 10 min, preferably from 0.13 to 0.7 g / 10min, more preferably from 0.15 to 0.5 g / 10min.
[0038] The at least one heterophasic propylene copolymer (HECO) has in the Crystex analysis one or more, preferably all of the following properties: a total ethylene (C2) content in the range of 0.5 to less than 5.5 wt.-%, preferably from 0.8 to 5.3 wt%, more preferably from 1 .0 to 5.2 wt%, even more preferably from 1 .0 to less than 4.5 wt.-%, preferably from 1 .0 to 4.3 wt%, more preferably from 1 .3 to 4.2 wt% (based on the total weight of the heterophasic propylene copolymer), an intrinsic viscosity (IV) in the range from 1 .0 to 6.0 dl / g, preferably in the range from 2.0 to 5.5 dl / g, more preferably in the range from 3.0 to 5.0 dl / g, and / or a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF)) in the range from 0.3 to 5.0 wt.-% (based on the total weight of the crystalline fraction), preferably from 0.4 to 3.0 wt%, more preferably from 0.5 to 2.0 wt%. an intrinsic viscosity (IV(CF)) in the range from 2.0 to 6.0 dl / g, preferably in the range from 2.5 to 5.5 dl / g, more preferably in the range from 3.0 to 5.0 dl / g. and / or a soluble fraction (SF) content in the range of 2.5 to 14.5 wt%, preferably in the range of 3.0 to 13.0 wt%, more preferably in the range of 3.5 to 11 .5 wt% (based on the total weight of the heterophasic propylene copolymer); the soluble fraction (SF) having one or more, preferably all of the following properties: an ethylene content (C2(SF)) in the range from 15.0 to 40.0 wt.-% (based on the total weight of the soluble fraction), preferably from 20.0 to 35.0 wt%, more preferably from 20.0 to 33.0 wt%. an intrinsic viscosity (IV(SF)) in the range from 1 .0 to 6.0 dl / g, preferably in the range from 1 .5 to 5.0 dl / g, more preferably in the range from 2.0 to 4.0 dl / g.
[0039] The at least one heterophasic propylene copolymer (HECO) has an impact strength (ISO179- 1 , Charpy notched 1 eA +23°C, measured as described in the method section) of at least 8 kJ / m2, preferably at least 10 kJ / m2, in particular in a range from 8.0 to 80.0 kJ / m2, more particular in a range fro 10.0 to 70.0 kJ / m2, even more particular in a range from 10.0 to 60.0 kJ / m2.
[0040] The at least one heterophasic propylene copolymer (HECO) may have an impact strength (ISO179-1 , Charpy notched 1 eA -20°C, measured as described in the method section) of at least 1 .0 kJ / m2, preferably at least 1 .5 kJ / m2, more preferably of at least 2.0 kJ / m2, in particular in a range from 1 .0 to 5.0 kJ / m2, more particular in a range from 1 .5 to 4.5 kJ / m2, even more particular in a range from 2.0 to 4.0 kJ / m2.
[0041] Preferred heterophasic copolymers are described now in more detail. Heterophasic polypropylene copolymer HECO-1
[0042] The at least one heterophasic propylene copolymer (HECO-1 ) has in the Crystex analysis one or more, preferably all of the following properties: a total ethylene (C2) content from 0.5 to less than 4.0 wt.-%, preferably from 1 .0 to 3.5 wt%, more preferably from 1 .2 to 3.0 wt%, such as from 1 .2 to 2.5 wt% (based on the total weight of the heterophasic propylene copolymer), and / or an intrinsic viscosity (IV) in the range from 1 .0 to 6.0 dl / g, preferably in the range from 2.0 to 5.5 dl / g, more preferably in the range from 3.0 to 5.0 dl / g, and / or a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF)) in the range from 0.3 to 3.0 wt.-% (based on the total weight of the crystalline fraction), preferably from 0.4 to 2.0 wt%, more preferably from 0.5 to 1 .5 wt%. an intrinsic viscosity (IV(CF)) in the range from 2.0 to 6.0 dl / g, preferably in the range from 2.5 to 5.5 dl / g, more preferably in the range from 3.0 to 5.0 dl / g. and / or a soluble fraction (SF) content in the range of 2.5 to 9.5 wt%, preferably in the range of 3.0 to 8.5 wt%, more preferably in the range of 3.5 to 7.5 wt% (based on the total weight of the heterophasic propylene copolymer) the soluble fraction (SF) having one or more, preferably all of the following properties: an ethylene content (C2(SF)) in the range from 15.0 to 35.0 wt.-% (based on the total weight of the soluble fraction), preferably from 18.0 to 30.0 wt%, more preferably from 20.0 to 25.0 wt%. an intrinsic viscosity (IV(SF)) in the range from 1 .0 to 6.0 dl / g, preferably in the range from 1 .5 to 5.0 dl / g, more preferably in the range from 2.0 to 4.0 dl / g.
[0043] The at least one heterophasic propylene copolymer (HECO-1 ) may have a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C) in the range from 0.1 and 0.9 g / 10 min, preferably from 0.13 to 0.7 g / 10min, more preferably from 0.15 to 0.4 g / 10min. The least one heterophasic propylene copolymer (HECO-1) may have an impact strength (ISO179-1 , Charpy notched 1 eA +23°C, measured as described in the method section) of at least 8 kJ / m2,preferably at least 10 kJ / m2, in particular in a range from 8.0 to 50.0 kJ / m2, more particular in a range from 10.0 to 40.0 kJ / m2, even more particular in a range from 10 to 35 kJ / m2.
[0044] The least one heterophasic propylene copolymer (HECO-1) may have an impact strength (ISO179-1 , Charpy notched 1 eA -20°C, measured as described in the method section) of at least 1 .0 kJ / m2, preferably at least 1 .5 kJ / m2, more preferably of at least 2.0 kJ / m2, in particular in a range from 1 .0 to 4.0 kJ / m2, more particular in a range from 1 .5 to 3.5 kJ / m2, even more particular in a range from 2.0 to 3.0 kJ / m2.
[0045] A process for obtaining said heterophasic polypropylene copolymer HECO-1 is described in detail in the method section.
[0046] Heterophasic polypropylene copolymer HECO-2
[0047] The at least one heterophasic propylene copolymer (HECO-2) has in the Crystex analysis one or more, preferably all of the following properties: a total ethylene (C2) content from 1 .5 to less than 5.5 wt.-%, preferably from 2.0 to 5.2 wt%, more preferably from 2.5 to 5.0 wt%, such as from 3.0 to 4.8 wt% (based on the total weight of the heterophasic propylene copolymer) an intrinsic viscosity (IV) in the range from 1 .0 to 6.0 dl / g, preferably in the range from 2.0 to 5.5 dl / g, more preferably in the range from 3.0 to 5.0 dl / g, and / or a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF)) in the range from 0.5 to 5.0 wt.-% (based on the total weight of the crystalline fraction), preferably from 1 .0 to 3.0 wt%, more preferably from 1 .2 to 2.0 wt%. an intrinsic viscosity (IV(CF)) in the range from 2.0 to 6.0 dl / g, preferably in the range from 2.5 to 5.5 dl / g, more preferably in the range from 3.0 to 5.0 dl / g, and / or a soluble fraction (SF) content in the range of 4.0 to 14.5 wt%, preferably in the range of 5.0 to 13.0 wt%, more preferably in the range of 6.0 to 11 .5 wt% (based on the total weight of the heterophasic propylene copolymer); the soluble fraction (SF) having one or more, preferably all of the following properties: an ethylene content (C2(SF)) in the range from 20.0 to 40.0 wt.-% (based on the total weight of the soluble fraction), preferably from 25.0 to 35.0 wt%, more preferably from 30.0 to 33.0 wt%. an intrinsic viscosity (IV(SF)) in the range from 1 .0 to 6.0 dl / g, preferably in the range from 1 .5 to 5.0 dl / g, more preferably in the range from 2.0 to 4.0 dl / g.
[0048] The at least one heterophasic propylene copolymer (HECO-2) has a melt flow rate MFR2( measured according to ISO 1133, 2.16 kg, 230°C) in the range from 0.1 to 0.9 g / 10 min, preferably from 0.13 to 0.7 g / 10min, more preferably from 0.15 to 0.4 g / 10min.
[0049] The at least one heterophasic propylene copolymer (HECO-2) has an impact strength (ISO179-1 , Charpy notched 1 eA +23°C, measured as described in the method section) of at least 20 kJ / m2, preferably at least 25 kJ / m2, more preferably of at least 30 kJ / m2, in particular in a range from 20.0 to 80.0 kJ / m2, more particular in a range from25.0 to70.0 kJ / m2, even more particular in a range from 30.0 to 60.0 kJ / m2.
[0050] The at least one heterophasic propylene copolymer (HECO-2) has an impact strength (ISO179-1 , Charpy notched 1 eA -20°C, measured as described in the method section) of at least 1 .5 kJ / m2, preferably at least 2.0 kJ / m2, more preferably of at least 2.5 kJ / m2, in particular in a range from 1 .5 to 5.0 kJ / m2, more particular in a range from 2.0 to 4.5 kJ / m2, even more particular in a range from 2.5 to 4.0 kJ / m2.
[0051] A process for obtaining said heterophasic polypropylene copolymer HECO-2 is described in detail in the method section.
[0052] Mixed-plastics polypropylene blend of recycled material
[0053] The mixed-plastics polypropylene blend is obtained from recycled waste stream of recycled post-consumer waste. In one aspect the recyclate blend may be a polypropylene (PP) rich material of recycled plastic material that comprises significantly more polypropylene than polyethylene. The PP rich material may be obtained by selective processing, shredding, washing, optionally extrusion, degassing and filtration and / or by separation according to type and colors such as NIR or Raman sorting and VIS sorting.
[0054] In an embodiment, the mixed-plastics polypropylene blend of recycled material (Blend A) comprises iPP content of 75 to 99 wt%, preferably of 80-98 wt%, more preferably of 85 - 95 wt% (based on the total weight of the recyclate blend) determined according to IR method as described in the method section, which is recovered from a waste plastic material derived from post-consumer and / or post-industrial waste..
[0055] In still a further embodiment, the mixed-plastics polypropylene blend of recycled material (Blend A) has in the Crystex analysis one or more, preferably all of the following properties: a total ethylene (C2) content in the range from 1 .0 to 20.0 wt.-%, preferably from 2.0 to 18.0 wt%, more preferably from 5.0 to 15.0 wt%, even more preferably from 5.5 to 13.0 wt%, (based on the total weight of the mixed-plastic polypropylene blend of recycled material); and / or an intrinsic viscosity (IV) in the range from 1 .0 to 3.0 dl / g, preferably in the range from 1 .2 to 2.7 dl / g, more preferably in the range from 1 .5 to 2.5 dl / g; and / or a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF) in the range from 1 .0 to 20.0 wt.-%, preferably from 2.0 to 18.0 wt%, more preferably from 5.0 to 15.0 wt%, even more preferably from 6.0 to 13.0 wt % (based on the total weight of the crystalline fraction),; and / or an intrinsic viscosity (IV(CF)), in the range from 1 .0 to 3.0 dl / g, preferably in the range from 1 .2 to 2.7 dl / g, more preferably in the range from 1 .5 to 2.5 dl / g; a soluble fraction (SF) in the range from 2.0 to 7.5 wt%, preferably in a range from 2.5 to 7.0 wt%, more preferably in a range from 3.0 to 7.0 wt%, even more preferably in a range from 3.3 to 6.8 wt%, such as from 3.5 to 6.5 wt%, (based on the total weight of the mixed- plastic polypropylene blend of recycled material) the soluble fraction (SF) having one or more, preferably all of the following properties if determinable: an ethylene content (C2(SF)) in the range from 0.01 to 40.0 wt.-% (based on the total weight of the soluble fraction), preferably from 0.1 to 35.0 wt%, more preferably from 0.5.0 to 32.0 wt%, even more preferably from 1.0 to 32.0 wt%, even more preferably from 2.0 to 32.0 wt%, even more preferably from 3.0 to 30.0 wt%, even more preferably from 4.0 to 30.0 wt%, even more preferably from 5.0 to 30.0 wt%. an intrinsic viscosity (IV(SF)) in the range from 0.2 to 3.5 dl / g, preferably in the range from 0 0.3 to 3.2 dl / g, more preferably in the range from 0.4 to 2.7 dl / g, even more preferably in the range from 0.5 to 2.5 dl / g.
[0056] The mixed-plastics polypropylene blend of recycled material (Blend A) has an ash content of at most 7.0 wt%, preferably of at most 6.0 wt%, more preferably of at most 5.0 wt% (based on the overall weight of the recyclate blend), such as in the range from 0.5 to 7.0 wt%, preferably from 1 .0 to 6.0 wt%, more preferably from 1 .1 to 5.0 wt%, such as 1 .1 to 3.5 wt%
[0057] In an embodiment, the mixed-plastics polypropylene blend of recycled material (Blend A) has a melt flow rate (ISO1133, 2.16kg; 230°C) in the range from 1 .0 to 12.0 g / 10 min, preferably from 1 .0 to 9.0 g / 10 min, preferably from 1 .5 to 8.0 g / 10 min, more preferably from 2.0 to 7.0 g / 10min, even more preferably from 3.0 to 6.5 g / 10min, still more preferably from 4.0 to 6.4 g / 10min.
[0058] In yet another embodiment, the mixed-plastics polypropylene blend of recycled material (Blend A) has one or more, preferably all of the following properties:
[0059] DMTA (torsional)_E' +23°C (determined as described in the method section) of at least 680 MPa, preferably of at least 700 MPa, more preferably of at least 730 MPa, such as in a range from 500 to 1000 MPa, preferably from 550 to 950 MPa, more preferably from 600 to 925 MPa, even more preferably from 650 to 900 MPa,
[0060] DMTA (torsional)_E' +60°C (determined as described in the method section) of at least 350 MPa, preferably of at least 370 MPa, more preferably of at least 400 MPa, such as in a range from 200 to 700 MPa, preferably from 250 to 600 MPa, more preferably from 300 to 500 MPa, even more preferably from 300 to 450 MPa,
[0061] DMTA (torsional)_E' +90°C (determined as described in the method section) of at least 200 MPa, preferably of at least 230 MPa, more preferably of at least 250 MPa, such as in a range from 100 to 600 MPa, preferably from 150 to 500 MPa, more preferably from 180 to 400 MPa, even more preferably from 180 to 300 MPa,
[0062] DMTA (torsional)_E' -30°C (MPa) (determined as described in the method section) of at least 1600 MPa, preferably of at least 1700 MPa, more preferably of at least 1800 MPa, such as in a range from 1400 to 2500 MPa, preferably from 1500 to 2000 MPa, more preferably from 1550 to 1950 MPa, DMTA (torsional)_E' 0°C (MPa) (determined as described in the method section) of at least 1000 MPa, preferably of at least 1100 MPa, more preferably of at least 1200 MPa, such as in a range from 800 to 2500 MPa, preferably from 850 to 2000 MPa, more preferably from 900 to 1500 MPa, even more preferably from 950 to 1400 MPa.
[0063] In a preferred embodiment, the mixed-plastics polypropylene blend of recycled material (Blend A) has one or more, preferably all of the following properties: an OCS gel index (determined as described in the method section)) of less than 50,000, preferably of less than 30,000, more preferably of less than 10,000, even more preferably of less than 5000, such as from 500 to less than 65,000, in particular from 800 to less than 5,000, more in particular from 1000 to less than 30,000, even more in particular from 1200 to less than 10,000, such as from 1500 to less than 5000, preferably from 1800 to 4500, more preferably from 2000 to 4000, even more preferably from 2000 to 3500, an OCS others (> 1000 pm, determined as described in the method section) of less than 1000 1 / m2, preferably of less than 500 1 / m2, more preferably of less than 100 1 / m2, even more preferably of less than 50 1 / m2, such as in a range from 0.1 to less than 1500 1 / m2, preferably in range from 0.2 to less than 1000 1 / m2, more preferably in a range from 0.5 to less than 500 1 / m2, even more preferably in a range from 0.7 to less than 100 1 / m2, still more preferably in a range from 1 .0 to less than 50 1 / m2, such as in a range from 1 .0 to 45 1 / m2, in particular in a range from 1 .0 to 40.0 1 / m2. an OCS contaminations (>1000 pm, determined as described in the method section) of less than 80 1 / m2, preferably of less than 75 1 / m2, more preferably of less than 70 1 / m2, even more preferably of less than 65 1 / m2, still more preferably of less than 60.0 0 1 / m2, such as in a range from 0.1 to less than 80 1 / m2, preferably in range from 0.2 to less than 75 1 / m2, more preferably in a range from 0.5 to less than 70 1 / m2, even more preferably in a range from 1 .0 to less than 70 1 / m2, still more preferably in a range from 1 .0 to less than 65 1 / m2, such as in a range from 1 .0 to 60.0 1 / m2, in particular in a range from 1 .0 to 50.0 1 / m2, and / or an OCS gel (> 1000 pm, determined as described in the method section) of less than 200 1 / m2, preferably of less than 100 1 / m2, more preferably of less than 50 1 / m2, even more preferably of less than 40 1 / m2, such as in a range from 0.1 to less than 300 1 / m2, preferably in range from 0.2 to less than 200 1 / m2, more preferably in a range from 0.5 to less than 150 1 / m2, even more preferably in a range from 0.6 to less than 100 1 / m2, still more preferably in a range from 1 .0 to less than 50 1 / m2, such as in a range from 1.1 to 20 1 / m2, in particular in a range 1.1 from to 10.0 1 / m2. In another embodiment the mixed-plastics polypropylene blend of recycled material (Blend A) comprises further components selected from the group comprising polystyrene, stabilizers, polyamide, talc, chalk, paper, wood, metal, limonene, fatty acid and mixtures thereof., in particular polystyrene, polyamide-6 as determined by FTIR, limonene as determined by using solid phase microextraction (HS-SPME-GC-MS), .
[0064] Due to the recycling origin, the blend may contain: organic fillers, and / or inorganic fillers, and / or additives in amounts of up to 10 wt%, preferably up to 5 wt% with respect to the weight of the blend.
[0065] As stated above, the recyclate blend (Blend A) may include one or more further components, selected from:
[0066] - up to 3.0 wt%, preferably up to 2.0 wt% of polystyrene and / or copolymers such as ABS,
[0067] - up to 3.0 wt% stabilizers, preferably up to 2.0 wt% stabilizers,
[0068] - up to 4.0 wt% polyamide, preferably up to 2.0 wt% polyamide,
[0069] - up to 3.0 wt% talc, preferably up to 1 .0 wt% talc,
[0070] - up to 1 .0 wt% paper, preferably up to 0.5 wt% paper,
[0071] - up to 1 .0 wt% wood, preferably up to 0.5 wt% wood, and
[0072] - up to 0.5 wt% metal, preferably up to 0.1 wt% metal,
[0073] - 0.1 ppm - 100 ppm of limonene as determined by using solid phase microextraction (HS-SPME-GC-MS), and
[0074] - 0 - 200 ppm total fatty acid content as determined by using solid phase microextraction (HS-SPME-GC-MS), wherein all amounts are given with respect to the total weight of the recyclate blend.
[0075] The properties of a preferred polypropylene recyclate blend that may be used is now described.
[0076] Polypropylene recyclate Blend A-1
[0077] The mixed-plastics polypropylene blend of recycled material (Blend A-1 ) has an IPP content of 75 to 95 wt%, preferably of 80-92 wt%. more preferably of 85 - 90 wt% (based on the total weight of the recyclate blend) determined according to IR method as described in the method section. Furthermore, the preferred mixed-plastics polypropylene blend of recycled material (Blend A- 1 ) has in the CRYSTEX analysis one or more, preferably all of the following properties: a total ethylene (C2) content in the range from 1 .0 to 20.0 wt.-%, preferably from 2.0 to 15.0 wt%, more preferably from 5.0 to 13.0 wt%, even more preferably from 9.0 to 12.0 wt%, even preferably from 9.0 to 11.5 wt% (based on the total weight of the mixed-plastic polypropylene blend of recycled material), and / or an intrinsic viscosity (IV) in the range from 1 .0 to 3.0 dl / g, preferably in the range from 1 .2 to 2.7 dl / g, more preferably in the range from 1 .5 to 2.5 dl / g; even more preferably in the range from 1 .7 to 2.2 dl / g; and / or a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF) in the range from 1 .0 to 20.0 wt.-%, preferably from 2.0 to 15.0 wt%, more preferably from 5.0 to 13.0 wt%, even more preferably from 6.0 to 12.0 wt %; even preferably from 9.0 to 11.5 wt% based on the total weight of the crystalline fraction); and / or an intrinsic viscosity (IV(CF)), in the range from 1 .0 to 3.0 dl / g, preferably in the range from 1 .2 to 2.7 dl / g, more preferably in the range from 1 .5 to 2.5 dl / g; even more preferably in the range from 1 .7 to 2.2 dl / g; a soluble fraction (SF) determined according to Crystex analysis as described in the method section in the range from 2.0 to 7.0 wt%, preferably in a range from 2.5 to 6.5 wt%, more preferably in a range from 3.0 to 6.0 wt%, even more preferably in a range from 3.5 to 5.5 wt%, such as from 4.0 to 5.0 wt%.(based on the total weight of the mixed-plastic polypropylene blend of recycled material) the soluble fraction (SF) having one or more, preferably all of the following properties, if determinable: an ethylene content (C2(SF)) in the range from 0.1 to 25.0 wt.-% (based on the total weight of the soluble fraction), preferably from 4.0 to 20.0 wt%, more preferably from 5.0 to 18.0 wt%. an intrinsic viscosity (IV(SF)) in the range from 0.2 to 3.0 dl / g, preferably in the range from 0.3 to 2.5 dl / g, more preferably in the range from 0.4 to 2.0 dl / g.
[0078] The preferred mixed-plastics polypropylene blend of recycled material (Blend A-1) has further an ash content of at most 6.0 wt%, preferably of at most 5.0 wt%, more preferably of at most 4.5 wt% (based on the overall weight of the recyclate blend), such as in the range from 2.0 to 6.0 wt%, preferably from 2.5 to 5.0 wt%, more preferably from 2.8 to 4.5 wt%, such as 3.0 to
[0079] 3.5 wt%
[0080] Furthermore, the preferred mixed-plastics polypropylene blend of recycled material (Blend A- 1 ) has one or more, preferably all of the following properties:
[0081] DMTA (torsional)_E' +23°C (determined as described in the method section) in a range from 500 to 1000 MPa, preferably from 600 to 950 MPa, more preferably from 650 to 900 MPa, even more preferably from 700 to 800 MPa,
[0082] DMTA (torsional)_E' +60°C (determined as described in the method section) in a range from 200 to 700 MPa, preferably from 250 to 600 MPa, more preferably from 300 to 500 MPa, even more preferably from 350 to 450 MPa,
[0083] DMTA (torsional)_E' +90°C (determined as described in the method section) in a range from 100 to 600 MPa, preferably from 150 to 500 MPa, more preferably from 180 to 400 MPa, even more preferably from 200 to 300 MPa,
[0084] DMTA (torsional)_E' -30°C (MPa) (determined as described in the method section) in a range from 1400 to 2500 MPa, preferably from 1500 to 2000 MPa, more preferably from 1550 to 1900 MPa, and / or
[0085] DMTA (torsional)_E' 0°C (MPa) (determined as described in the method section) in a range from 800 to 2500 MPa, preferably from 900 to 2000 MPa, more preferably from 1000 to 1500 MPa, even more preferably from 1150 to 1250 MPa.
[0086] The preferred mixed-plastics polypropylene blend of recycled material (Blend A-1 ) has a melt flow rate (ISO1133, 2.16kg; 230°C) in the range from 1.0 to 12.0 g / 10 min, preferably from 1 .0 to less than 9.0 g / 10 min, preferably from 1 .5 to 8.0 g / 10 min, more preferably from 2.0 to 7.0 g / 1 Omin, even more preferably from 4.0 to 6.5 g / 1 Omin, still more preferably from 5.0 to 6.4 g / 10min.
[0087] Still further, the preferred mixed-plastics polypropylene blend of recycled material (Blend A-1 ) has one or more, preferably all of the following properties: an OCS gel index (determined as described in the method section) in a range from 500 to less than 5000, in particular from 800 to less than 4000, more in particular from 1000 to less than 3000, even more in particular from 1200 to less than 2500, such as from 1500 to less than 2500, preferably from 1800 to 2500, more preferably from 2000 to 2500, an OCS others (> 1000 pm, determined as described in the method section) of in a range from 5.0 to less than 100 1 / m2, preferably in range from 10.0 to less than 80 1 / m2, more preferably in a range from 15.0 to less than 60 1 / m2, even more preferably in a range from 20.0 to less than 50 1 / m2, still more such as in a range from 20.0 to 40 1 / m2, in particular in a range from 20.0 to 30.0 1 / m2, an OCS contaminations (>1000 pm, determined as described in the method section) in a range from 5.0 to less than 85 1 / m2, preferably in range from 10.0 to less than 80 1 / m2, more preferably in a range from 15.0 to less than 75 1 / m2, even more preferably in a range from 20.0 to less than 70 1 / m2, still more preferably in a range from 25.0 to less than 65 1 / m2, such as in a range from 30.0 to 60.0 1 / m2, in particular in a range from 35.0 to 50.0 1 / m2, and / or an OCS gel (> 1000 pm, determined as described in the method section) in a range from 0.8 to less than 300 1 / m2, preferably in range from 1.0 to less than 200 1 / m2, more preferably in a range from 1 .3 to less than 150 1 / m2, even more preferably in a range from 1 .5 to less than 100 1 / m2, still more preferably in a range from 1 .8 to less than 50 1 / m2, such as in a range from 2.0 to 4.0 1 / m2, in particular in a range from 2.0 to 3.0 1 / m2.
[0088] Polypropylene recyclate Blend A-2
[0089] The mixed-plastics polypropylene blend of recycled material (Blend A-2) has an iPP content of 75 to 95 wt%, preferably of 80-92 wt%. more preferably of 85 - 90 wt% (based on the total weight of the recyclate blend) determined according to IR method as described in the method section.
[0090] Furthermore, the preferred mixed-plastics polypropylene blend of recycled material (Blend A- 2) has in the CRYSTEX analysis one or more, preferably all of the following properties: a total ethylene (C2) content in the range from 1 .0 to 15.0 wt.-%, preferably from 2.0 to 12.0 wt%, more preferably from 2.5 to 10.0 wt%, even more preferably from 3.0 to 8.0 wt%, even preferably from 4.0 to 7.0 wt% (based on the total weight of the mixed- plastic polypropylene blend of recycled material), and / or an intrinsic viscosity (IV) in the range from 1 .0 to 3.0 dl / g, preferably in the range from 1.2 to 2.7 dl / g, more preferably in the range from 1.5 to 2.5 dl / g; even more preferably in the range from 1 .5 to 2.0 dl / g; and / or a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF) in the range from 1 .0 to 15.0 wt.-%, preferably from 2.0 to 12.0 wt%, more preferably from 2.5 to 10.0 wt%, even more preferably from 3.0 to 8.0 wt %; even preferably from 4.0 to 7.0 wt% based on the total weight of the crystalline fraction); and / or an intrinsic viscosity (IV(CF)), in the range from 1 .0 to 3.0 dl / g, preferably in the range from 1.2 to 2.7 dl / g, more preferably in the range from 1.5 to 2.5 dl / g; even more preferably in the range from 1 .5 to 2.0 dl / g; a soluble fraction (SF) determined according to Crystex analysis as described in the method section in the range from 2.0 to 7.0 wt%, preferably in a range from 2.5 to 6.5 wt%, more preferably in a range from 3.0 to 6.0 wt%, even more preferably in a range from 3.5 to 5.5 wt%, such as from 4.0 to 5.0 wt%.(based on the total weight of the mixed-plastic polypropylene blend of recycled material) the soluble fraction (SF) having one or more, preferably all of the following properties, if determinable: an ethylene content (C2(SF)) in the range from 0.1 to 20.0 wt.-% (based on the total weight of the soluble fraction), preferably from 1.0 to 15.0 wt%, more preferably from 1 .5 to 5.0 wt%, even more preferably from 2.0 to 5.0 wt%. an intrinsic viscosity (IV(SF)) in the range from 0.2 to 3.0 dl / g, preferably in the range from 0.3 to 2.7 dl / g, more preferably in the range from 0.4 to 2.5 dl / g.
[0091] The preferred mixed-plastics polypropylene blend of recycled material (Blend A-2) has further an ash content of at most 6.0 wt%, preferably of at most 5.0 wt%, more preferably of at most
[0092] 4.5 wt% (based on the overall weight of the recyclate blend), such as in the range from 2.0 to 6.0 wt%, preferably from 2.5 to 5.0 wt%, more preferably from 2.8 to 4.5 wt%, such as 3.0 to
[0093] 3.5 wt%
[0094] Furthermore, the preferred mixed-plastics polypropylene blend of recycled material (Blend A- 2) has one or more, preferably all of the following properties:
[0095] DMTA (torsional)_E‘ +23°C (determined as described in the method section) in a range from 500 to 1000 MPa, preferably from 600 to 950 MPa, more preferably from 650 to 900 MPa, even more preferably from 700 to 900 MPa,
[0096] DMTA (torsional)_E‘ +60°C (determined as described in the method section) in a range from 200 to 700 MPa, preferably from 250 to 600 MPa, more preferably from 300 to 500 MPa, even more preferably from 350 to 450 MPa, DMTA (torsional)_E' +90°C (determined as described in the method section) in a range from 100 to 600 MPa, preferably from 150 to 500 MPa, more preferably from 180 to 400 MPa, even more preferably from 200 to 300 MPa,
[0097] DMTA (torsional)_E' -30°C (MPa) (determined as described in the method section) in a range from 1400 to 2500 MPa, preferably from 1500 to 2000 MPa, more preferably from 1600 to 1950 MPa, and / or
[0098] DMTA (torsional)_E' 0°C (MPa) (determined as described in the method section) in a range from 800 to 2500 MPa, preferably from 900 to 2000 MPa, more preferably from 1000 to 1500 MPa, even more preferably from 1200 to 1400 MPa.
[0099] The preferred mixed-plastics polypropylene blend of recycled material (Blend A-2) has a melt flow rate (ISO1133, 2.16kg; 230°C) in the range from 1.0 to 12.0 g / 10 min, preferably from 1 .0 to less than 9.0 g / 10 min, preferably from 1 .5 to 8.0 g / 10 min, more preferably from 2.0 to 7.0 g / 1 Omin, even more preferably from 4.0 to 6.5 g / 1 Omin, still more preferably from 5.0 to 6.4 g / 10min.
[0100] Still further, the preferred mixed-plastics polypropylene blend of recycled material (Blend A-2) has one or more, preferably all of the following properties: an OCS gel index (determined as described in the method section) in a range from 500 to less than 5000, in particular from 800 to less than 4500, more in particular from 1000 to less than 4000, even more in particular from 1200 to less than 3800, such as from 1500 to less than 3700, preferably from 1800 to 3600, more preferably from 2000 to 3500, an OCS others (> 1000 pm, determined as described in the method section) of in a range from 0.2 to less than 15 1 / m2, preferably in range from 0.4 to less than 10 1 / m2, more preferably in a range from 0.5 to less than 8 1 / m2, even more preferably in a range from 0.6 to less than 5 1 / m2, still more such as in a range from 0.65 to 3 1 / m2, in particular in a range from 0.7 to 1.0 1 / m2, an OCS contaminations (>1000 pm, determined as described in the method section) in a range from 0.1 to less than 15 1 / m2, preferably in range from 0.2 to less than 10 1 / m2, more preferably in a range from 0.25 to less than 8 1 / m2, even more preferably in a range from 0.3 to less than 5 1 / m2, still more preferably in a range from 0.35 to less than 3 1 / m2, such as in a range from 0.4 to 2.0 1 / m2, in particular in a range from 0.45 to 1 .0 1 / m2, and / or an OCS gel (> 1000 pm, determined as described in the method section) in a range from 0.1 to less than 15 1 / m2, preferably in range from 0.2 to less than 10 1 / m2, more preferably in a range from 0.3 to less than 8 1 / m2, even more preferably in a range from 0.4 to less than 5 1 / m2, still more preferably in a range from 0.45 to less than 3 1 / m2, such as in a range from 0.5 to 2.0 1 / m2, in particular in a range from 0.55 to 1 .0 1 / m2.
[0101] In one embodiment the polyolefin composition may comprise at least one dosing agent for accepting pigments and other additives during extrusion. The at least one dosing agent may be a polypropylene homopolymer with melt flow rates MFR2 from 0.1 to 5.0 g / 10 min, preferably from 0.2 to 1.0 g / 10 min. Such a polymer is commercially available from Borealis AG. The amount of dosing agent in the polyolefin composition may be from 0.5 to 2 wt%, such as from 0.8 to 1 .2 wt%.
[0102] Additives
[0103] Examples of additives for use in the present polyolefin composition are pigments or dyes (for example carbon black), stabilizers (anti-oxidant agents), anti-acids and / or anti-UVs, antistatic agents, nucleating agents and utilization agents (such as processing aid agents). Preferred additives comprise at least one antioxidant, at least one anti-acid and optionally carbon black.
[0104] Generally, the amount of these additives is in the range from 0 to 8 wt%, preferably in the range 0 to 5.0 wt%, more preferably in the range of 0.01 to 4.0 wt%, even more preferably in the range from 0.1 to 3.5 wt% based on the weight of the total polyolefin composition.
[0105] It is generally to be understood that the amount of additives present in the polyolefin composition may also include the amounts of additives present in the virgin polymer in addition to the externally added additives (e.g., additives that are added during compounding). On the other hand, as not all the additives present in the recycled polymer can be quantified, the amount of such additives is not considered in the amount of additives present in the polyolefin composition.
[0106] Examples of antioxidants which are commonly used in the art, are sterically hindered phenols (such as CAS No. 6683-19-8, also sold as Irganox 1010 FF™ by BASF), phosphorous based antioxidants (such as CAS No. 31570-04-4, also sold as Hostanox PAR 24 (FF)™ by Clariant, or Irgafos 168 (FF)TM by BASF), sulphur based antioxidants (such as CAS No. 693- 36-7, sold as Irganox PS-802 FL™ by BASF), nitrogen-based antioxidants (such as 4,4’- bis(1 ,1 ’- dimethylbenzyl)diphenylamine), or antioxidant blends. Preferred antioxidants may be Tris (2,4- di-f-butylphenyl) phosphite and / or Octadecyl 3-(3’,5’-di-tert. butyl-4-hydroxyphenyl)propionate.
[0107] Anti-acids are also commonly known in the art. Examples are sodium stearates, magnesium and zinc oxides, synthetic hydrotalcite (e.g. SHT, CAS-No. 11097-59-9), lactates and lactylates, as well as calcium stearate (CAS No. 1592-23-0) and zinc stearate (CAS No. 557- 05-1 ).
[0108] Common antiblocking agents are natural silica such as diatomaceous earth (such as CAS No. 60676-86-0 (SuperfFloss™), CAS-No. 60676-86-0 (SuperFloss E™), or CAS-No. 60676-86-0 (Celite 499™)), synthetic silica (such as 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 (such as aluminium 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 zeolites (such as sodium calcium aluminosilicate hydrate CAS-No. 1344- 01 -0, CAS-No. 1344-01 -0, or sodium calcium aluminosilicate, hydrate CAS-No. 1344-01 -0).
[0109] Anti-UVs are, for example, Bis-(2,2,6,6-tetramethyl-4-piperidyl)-sebacate (CAS -No. 52829- 07-9, Tinuvin 770); 2-hydroxy-4-n-octoxy-benzophenone (CAS-No. 1843-05-6, Chimassorb 81 ). Preferred UV stabilizers may be low and / or high molecular weight UV stabilizers such as n-Hexadecyl- 3,5-di-t-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-piperidyl)imino)hexameth-ylene (1 , 2,2,6, 6-pentamethyl-4- piperidyl)imino)).
[0110] Suitable alpha nucleating agents are, for example, sodium benzoate (CAS No. 532-32-1 ); 1 ,3:2,4-bis(3,4-dimethylbenzylidene)sorbitol (CAS 135861 -56-2, Millad 3988). 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 ).
[0111] Usually these additives, except for pigments or dyes, are added in quantities of 100 - 4000 ppm for each individual additive based on the overall weight of the polyolefin composition The polyolefin composition
[0112] According to an embodiment the present polyolefin composition comprises a) in the range of from 42 to 87 wt%, preferably from 45 to 85 wt%, more preferably from 47 to 80 wt%, even more preferably from 65 to 77 wt.-%, still more preferably from 68 to 76 wt%, (based on the overall weight of the polyolefin composition) of at least one heterophasic propylene copolymer (HECO) with a total ethylene (C2) content (as determined according to Crystex analysis as described in the method section) in the range from 0.5 to 6.0 wt.-% (based on the total weight of the heterophasic propylene copolymer), a soluble fraction (SF) determined according to Crystex analysis described in this patent in the range from 2.0 to 15.0 wt% (based on the total weight of the heterophasic propylene copolymer), and a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C, ) in the range from 0.1 to 1 g / 10 min; b) in the range from 13 to 58 wt%, preferably from 15 to 55 wt%, more preferably from 20 to 53 wt%, even more preferably from 23 to 35 wt%, still more preferably from 24 to 32 wt% (based on the overall weight of the polyolefin composition) of a mixed-plastics polypropylene blend of recycled material (Blend A) having a soluble fraction (SF) determined according to Crystex analysis described in the method section in the range from 2.0 to 8.0 wt% (based on the total weight of the mixed-plastic polypropylene blend of recycled material), a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C, ) in the range from 1.0 to 15 .0 g / 10 min, and one or more, preferably all of the following properties: an OCS gel index (determined as described in the method section) of less than 65000. OCS others (> 1000 pm, determined as described in the method section) of less than 1500 1 / m2,OCS contaminations (>1000 pm, determined as described in the method section) of less than 85 1 / m2, and / or OCS gel (>1000 pm, determined as described in the method section) of less than 300 1 / m2, and c) optionally further additives (based on the overall weight of the polyolefin composition), wherein the sum of all ingredients always adds up to 100 wt%.
[0113] In preferred embodiments the present polyolefin composition may comprise
[0114] - 40 wt% of at least one heterophasic propylene copolymer (HECO) and 60 wt% polypropylene recyclate (rPP);
[0115] - 50 wt% heterophasic propylene copolymer (HECO) and 50 wt% polypropylene recyclate (rPP);
[0116] - 60 wt% of at least one heterophasic propylene copolymer (HECO) and 40 wt% polypropylene recyclate (rPP); - 66 wt% of at least one heterophasic propylene copolymer (HECO) and 34 wt% polypropylene recyclate (rPP);
[0117] - 68 wt% of at least one heterophasic propylene copolymer (HECO) and 32 wt% polypropylene recyclate (rPP);
[0118] - 70 wt% of at least one heterophasic propylene copolymer (HECO) and 30 wt% polypropylene recyclate (rPP);
[0119] - 75 wt% of at least one heterophasic propylene copolymer (HECO) and 25 wt% polypropylene recyclate (rPP);
[0120] - 80 wt% of at least one heterophasic propylene copolymer (HECO) and 20 wt% polypropylene recyclate (rPP);
[0121] - 85 wt% of at least one heterophasic propylene copolymer (HECO) and 15 wt% polypropylene recyclate (rPP);
[0122] - 90 wt% of at least one heterophasic propylene copolymer (HECO) and 10 wt% polypropylene recyclate (rPP).
[0123] It is to be understood that small amounts of additives (for example in the range from 0 to 8 wt%, preferably in the range 0 to 5.0 wt%, more preferably in the range of 0.01 to 4.0 wt%, even more preferably in the range from 0.1 to 3.5 wt%) such as antioxidants, pigments etc., may be present in the described compositions. Thus, the amount of heterophasic propylene copolymer (HECO) and / or polypropylene recyclate may deviate slightly from the above ratio. However, based on the overall weight of the polyolefin composition, the sum of all ingredients always add up to 100 wt%.
[0124] In one embodiment, the polyolefin composition comprises at least two heterophasic propylene copolymers, as will be described in more detail below.
[0125] In an embodiment, the polyolefin composition may have a ring stiffness (determined as described in the method section) of at least 7.0 kN / m2, preferably of at least 7.5 kN / m2, more preferably of at least 8.0 kN / m2, even more preferably of at least 9.2 kN / m2, still more preferably of at least 9.5 kN / m2, as in the range from 7.0 kN / m2to 20.0 kN / m2, preferably in the range from 7.5 kN / m2to 15.0 kN / m2, more preferably in the range from 8.0 kN / m2to 12.0 kN / m2.
[0126] In still another embodiment, the polyolefin composition may have an impact strength (ISO179- 1 , Charpy notched 1 eA +23°C, measured as described in the method section) of at least 3.0 kJ / m2, preferably of at least 5.0 kJ / m2, still more preferably of at least 6.0 kJ / m2, in particular in a range from 3.0 to 20.0 kj / m2, more particular in a range from 5.0 to 15.0 kj / m2, even more particular in a range from 6.0 to 10.0 kJ / m2.
[0127] The polyolefin composition may further have an impact strength (ISO179-1 , Charpy notched 1 eA -20°C, measured as described in the method section) of at least 1 .0 kJ / m2, preferably of at least 1 .3 kJ / m2, still more preferably of at least 1 .5 kJ / m2, in particular in a range from 1 .0 to 15.0 kJ / m2, more particular in a range from 1 .3 to 10.0 kJ / m2, even more particular in a range from 1 .5 to 5.0 kJ / m2.
[0128] Furthermore, the polyolefin composition may have a melt flow rate MFR2 (measured according to ISO 1133, 2.16 kg, 230°C) of at most 3.0 g / 10 min; preferably of at most 2.5 g / 10 min, more preferably of at most 2.0 g / 10 min, even more preferably of at most 1 .5 g / 1 Omin, such as in the range from 0.3 to 3.0 g / 10 min, preferably from 0.5 to 2.5 g / 1 Omin, more preferably 0.6 to 2.0 g / 10 min, even more preferably from 0.7 to 1 .5 g / 1 Omin.
[0129] In still another embodiment, the polyolefin composition may have one or more, preferably all of the following properties: an OCS gel index (determined as described in the method section) of less than 2.000, preferably of less than 1800, more preferably of less than 1500, even more preferably of less than 1200, still more preferably of less than 1000, such as from 50 to less than 2000, in particular from 60 to less than 1800, more in particular from 70 and less than 1500, even more in particular from 80 and less than 1200, such as from 90 to less than 1000, preferably from 100 to 500, more preferably from 100 to 300, even more preferably from 100 to 250, an OCS others (> 1000 pm, determined as described in the method section) of less than 10.0 1 / m2, preferably of less than 8.0 1 / m2, more preferably of less than 5.0 1 / m2, even more preferably of less than 2.0 1 / m2, Such as in a range from 0 to less than 8.0 1 / m2, preferably in range from 0 to less than 5.0 1 / m2, more preferably in a range from 0 to less than 3.0 1 / m2, even more preferably in a range from 0 to less than 2.0 1 / m2, still more preferably in a range from 0 to less than 1 .5 1 / m2, an OCS contaminations (>1000 pm, determined as described in the method section) of less than 3.5 1 / m2, preferably of less than 3.0 1 / m2, more preferably of less than 2.5 1 / m2, even more preferably of less than 2.0 1 / m2, still more preferably of less than 1 .0 1 / m2, such as in a range from 0 to less than 3.5 1 / m2, preferably in range fromO to less than 3.0 1 / m2, more preferably in a range from 0 to less than 2.5 1 / m2, even more preferably in a range from 0 to less than 2.0 1 / m2, still more preferably in a range from Oto less than 1 .0 1 / m2, and / or an OCS gel (>1000 urn, determined as described in the method section) of less than 15.0 1 / m2, preferably of less than 10.0 1 / m2, more preferably of less than 5.0 1 / m2, even more preferably of less than 2.0 1 / m2’ still more preferably of less than 1.0 1 / m2, such as in a range from 0.0 to less than 15.0 1 / m2, preferably in range from 0.0 to less than 10.0 1 / m2, more preferably in a range from 0.0 to less than 5.0 1 / m2, even more preferably in a range from 0.0 to less than 2.0 1 / m2, still more preferably in a range from 0.0 to less than 1 .0 1 / m2.
[0130] According to a further embodiment, the present polyolefin composition has one or more, preferably all of the following properties:
[0131] DMTA (torsional)_E' +23°C (determined as described in the method section) of at least 600 MPa, preferably of at least 700 MPa, more preferably of at least 800 MPa, such as in a range from 600 to 2000 MPa, preferably from 700 to 1500 MPa, more preferably from 800 to 1000 MPa, even more preferably from 830 to 950 MPa;
[0132] DMTA (torsional)_E' +60°C (determined as described in the method section) of at least 300 MPa, preferably of at least 350 MPa, more preferably of at least 400 MPa, such as in a range from 300 to 800 MPa, preferably from 350 to 700 MPa, more preferably from 350 to 600 MPa, even more preferably from 400 to 500 MPa,
[0133] DMTA (torsional)_E' +90°C (determined as described in the method section) of at least 100 MPa, preferably of at least 150 MPa, more preferably of at least 200 MPa, such as in a range from 100 to 600 MPa, preferably from 150 to 500 MPa, more preferably from 200 to 400 MPa, even more preferably from 250 to 350 MPa,
[0134] DMTA (torsional)_E' -30°C (MPa) (determined as described in the method section) of at least 1700 MPa, preferably of at least 1800 MPa, more preferably of at least 1850 MPa, such as in a range from 1700 to 2500 MPa, preferably from 1720 to 2300 MPa, more preferably from 1750 to 2100 MPa, even more preferably from 1760 to 2000 MPa,
[0135] DMTA (torsional)_E' 0°C (MPa) (determined as described in the method section) of at least 1000 MPa, preferably of at least 1100 MPa, more preferably of at least 1200 MPa, such as in a range from 1000 to 2500 MPa, preferably from 1100 to 2000 MPa, more preferably from 1200 to 1500 MPa, even more preferably from 1250 to 1400 MPa.
[0136] In another embodiment, the polyolefin composition (when testing pipe properties) may have a failure time in pipe pressures testing (at +80°C, 4.2 MPa, determined as described in the method section) of at least 600 hours, preferably at least 700 hours, more preferably of at least 1000 hours, such as in the range from 600 hours to 5000 hours, preferably in the range from 700 hours to 4000 hours, more preferably in the range from 900 hours to 3000 hours. In another embodiment, the polyolefin composition (when testing pipe properties) may have a failure time in pipe pressures testing (at +95°C, 2.5 MPa, determined as described in the method section) of at least 1800 hours, preferably at least 1900 hours, more preferably of at least 2000 hours, such as in the range from 1800 hours to 6000 hours, preferably in the range from 1900 hours to 5000 hours, more preferably in the range from 2000 hours to 4000 hours.
[0137] In still a further embodiment, the polyolefin composition has in the Crystex analysis one or more, preferably all of the following properties: a total ethylene (C2) content in the range from 1 .0 to 20.0 wt.-%, preferably from 1 .5 to 15.0 wt%, more preferably from 2.0 to 10.0 wt%, even more preferably from 2.5 to 8.0 wt%, and / or an intrinsic viscosity (IV) in the range from 1 .0 to 5.0 dl / g, preferably in the range 1 .5 to 4.5 dl / g, more preferably in the range from 2.0 to 4.0 dl / g; even more preferably in the range from 2.5 to 3.5 dl / g; and / or a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF) in the range from 0.5 to 15.0 wt.-%, preferably from 0.7 to 10.0 wt%, more preferably from 0.9 to 8.0 wt%, even more preferably from 1 .0 to 4.5 wt %; and / or an intrinsic viscosity (IV(CF))in the range from 1.5 to 5.0 dl / g, preferably in the range from 2.0 to 4.0 dl / g, more preferably in the range from 2.2 to 3.5 dl / g, and / or a soluble fraction (SF) in the range from 2.0 to 20.0 wt.-%, preferably from 3.0 to 17.0 wt%, more preferably from 4.0 to 15.0 wt%, even more preferably from 5.0 to 13.0; still more preferably from 5.5 to 10.0 wt%. the soluble fraction (SF) having one or more, preferably all of the following properties: an ethylene content (C2(SF)) in the range from 10 to 40.0 wt.-% (based on the total weight of the soluble fraction), preferably from 12.0 to 35.0 wt%, more preferably from 13.0 to 32.0 wt%, and an intrinsic viscosity (IV(SF)) in the range from 0.5 to 3.0 dl / g, preferably in the range from 0.8 to 2.5 dl / g, more preferably in the range from 1 .0 to 2.2 dl / g. PC-1 comprisinq HECO-1 and Blend A-1
[0138] In an embodiment, the present polyolefin composition PC-1 comprises: a) in the range from 47 to 80 wt%, preferably from 65 to 77 wt.-%, more preferably from 68 to 76 wt% (based on the overall weight of the polyolefin composition) of at the least one heterophasic propylene copolymer HECO-1 ; b) in the range 20 to 53 wt%, even more preferably from 23 to 35 wt%, still more preferably from 24 to 32 wt% (based on the overall weight of the polyolefin composition) of a mixed-plastics polypropylene blend of recycled material Blend A-1 , c) optionally further additives (based on the overall weight of the polyolefin composition), wherein the sum of all ingredients always adds up to 100 wt%.
[0139] The polypropylene composition PC-1 comprising the least one heterophasic propylene copolymer HECO-1 and the blend of recycled material Blend A-1 may have one or more, preferably all of the following properties:
[0140] - a ring stiffness (determined as described in the method section) of at least 8.5 kN / m2, preferably of at least 9.0 kN / m2, even more preferably of at least 9.2 kN / m2, still more preferably of at least 9.5 kN / m2, as in the range from 8.5 kN / m2to 20.0 kN / m2, preferably in the range from 9.0 kN / m2to 15.0 kN / m2, more preferably in the range from 9.2 kN / m2to 12.0 kN / m2,
[0141] - an impact strength (ISO179-1 , Charpy notched 1 eA +23°C, measured as described in the method section) of at least 5.0 kJ / m2, preferably of at least 5.5 kJ / m2, still more preferably of at least 6.0 kJ / m2, in particular in a range from 5.0 to 20.0 kJ / m2, more particular in a range from 5.5 to 15.0 kJ / m2, even more particular in a range from 6.0 to 10.0 kJ / m2,
[0142] - an impact strength (ISO179-1 , Charpy notched 1 eA -20°C, measured as described in the method section) of at least 1 .0 kJ / m2, preferably of at least 1 .3 kJ / m2, still more preferably of at least 1 .5 kJ / m2, in particular in a range from 1 .0 to 15.0 kJ / m2, more particular in a range from 1.3 to 10.0 kJ / m2, even more particular in a range from 1 .5 to 5.0 kJ / m2,
[0143] - a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C) of at most 3.0 g / 10 min; preferably of at most 2.5 g / 10 min, more preferably of at most 2.0 g / 10 min, even more preferably of at most 1.5 g / 10min, such as in the range from 0.3 to 3.0 g / 10 min, preferably from 0.5 to 2.5 g / 10min, more preferably 0.6 to 2.0 g / 10 min, even more preferably from 0.7 to 1.5 g / 10min,
[0144] - an OCS gel index (determined as described in the method section) of less than 1500, preferably of less than 1200, more preferably of less than 1000, such as from 100 and less than 1500, in particular from 150 and less than 1200, such as from 160 to less than 1000, preferably from 170 to 500, more preferably from 180 to 300, even more preferably from 200 to 250,
[0145] - an OCS others (> 1000 pm, determined as described in the method section) of less than 3.0 1 / m2, preferably of less than 2.0 1 / m2, such as in a range from 0.2 to less than 3.0 1 / m2, preferably in a range from 0.4 to less than 2.0 1 / m2, still more preferably in a range from 0.6 to less than 1 .5 1 / m2;
[0146] - an OCS contaminations (>1000 pm, determined as described in the method section) of less than 2.0 1 / m2, preferably of less than 1 .0 1 / m2, such as in a range from 0.15 to less than 2.0 1 / m2, preferably in a range from 0.15 to less than 1.0 1 / m2,
[0147] - an OCS gel (>1000 pm, determined as described in the method section) of less than 1 .0 1 / m2, such as in a range from 0.0 to less than 1 .0 1 / m2,
[0148] DMTA (torsional)_E' +23°C (determined as described in the method section) of at least 600 MPa, preferably of at least 700 MPa, more preferably of at least 800 MPa, such as in a range from 600 to 2000 MPa, preferably from 700 to 1500 MPa, more preferably from 800 to 1000 MPa, even more preferably from 850 to 950 MPa;
[0149] - DMTA (torsional)_E' +60°C (determined as described in the method section) of at least 350 MPa, preferably of at least 400 MPa, such as in a range from 350 to 700 MPa, preferably from 350 to 600 MPa, even more preferably from 400 to 500 MPa,
[0150] - DMTA (torsional)_E' +90°C (determined as described in the method section) of at least 150 MPa, preferably of at least 200 MPa, such as in a range from 150 to 500 MPa, preferably from 200 to 400 MPa, more preferably from 250 to 350 MPa, DMTA (torsional)_E' -30°C (MPa) (determined as described in the method section) of at least 1800 MPa, more preferably of at least 1850 MPa, such as in a range from 1800 to 2300 MPa, preferably from 1850 to 2100 MPa, more preferably from 1900 to 2000 MPa,
[0151] DMTA (torsional)_E' 0°C (MPa) (determined as described in the method section) of at least 1100 MPa, preferably of at least 1200 MPa, such as in a range from 1100 to 2000 MPa, more preferably from 1200 to 1500 MPa, even more preferably from 1250 to 1400 MPa, - a failure time in pipe pressures testing (at +80°C, 4.2 MPa, determined as described in the method section) of at least 1300 hours, preferably of at least 1400 hours, such as in the range from 1300 hours to 4000 hours, preferably in the range from 1400 hours to 3000 hours,
[0152] - a failure time in pipe pressures testing (at +95°C, 2.5 MPa, determined as described in the method section) of at least 2200 hours, preferably of at least 2250 hours, such as in the range from 2200 hours to 5000 hours, preferably in the range from 2250 hours to 4000 hours.
[0153] In still a further embodiment, the polyolefin composition PC-1 has in the Crystex analysis one or more, preferably all of the following properties:
[0154] - a total ethylene (C2) content in the range from 2.0 to 10.0 wt%, preferably from 2.5 to 8.0 wt%, more preferably from 3.0 to 8.0 wt%, and / or an intrinsic viscosity (IV) in the range from 2.0 to 4.0 dl / g; preferably in the range from 2.5 to 3.5 dl / g; and / or
[0155] - a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF) in the range from 1 .0 to 10.0 wt.-%, preferably from
[0156] 1 .5 to 8.0 wt%, more preferably from 2.0 to 8.0 wt%, even more preferably from 2.5 to
[0157] 4.5 wt %; and / or an intrinsic viscosity (IV(CF)) in the range from 2.0 to 4.0 dl / g, preferably in the range from 2.5 to 3.5 dl / g, and / or
[0158] - a soluble fraction (SF) in the range from 2.0 to 15.0 wt.-%, preferably from 3.0 to 13.0 wt%, more preferably from 4.0 to 10.0 wt%, even more preferably from 5.0 to 8.0; still more preferably from 5.5 to 7.0 wt%.
[0159] - the soluble fraction (SF) having one or more, preferably all of the following properties: an ethylene content (C2(SF)) in the range from 10 to 30.0 wt.-% (based on the total weight of the soluble fraction), preferably from 12.0 to 25.0 wt%, more preferably from 13.0 to 20.0 wt%, and an intrinsic viscosity (IV(SF)) in the range from 0.5 to 3.0 dl / g, preferably in the range from 0.8 to 2.5 dl / g, more preferably in the range from 1 .0 to 2.2 dl / g. HECO-2 and Blend A-2
[0160] In another embodiment, the present polyolefin composition PC-2 comprises: a) in the range of from 40 to 90 wt%, preferably from 42 to 87 wt%, in particular preferably from 45 to 85 wt%, more preferably from 47 to 80 wt%, even more preferably from 49 to 76 wt.-%, (based on the overall weight of the polyolefin composition) of the at least one heterophasic propylene copolymer HECO-2; b) in the range from 10 to 60 wt%, preferably from 13 to 58 wt%, in particular preferably from 15 to 55 wt%, more preferably from 20 to 53 wt%, even more preferably from 24 to 51 wt% (based on the overall weight of the polyolefin composition) of a mixed-plastics polypropylene blend of recycled material Blend A-2, c) optionally further additives (based on the overall weight of the polyolefin composition), wherein the sum of all ingredients always adds up to 100 wt%.
[0161] The polypropylene composition PC-2 comprising the least one heterophasic propylene copolymer HECO-2 and the blend of recycled material Blend A-2 may have one or all of the following properties:
[0162] - a ring stiffness (determined as described in the method section) of at least 7.5 kN / m2, preferably of at least 8.0 kN / m2, more preferably of at least 8.5 kN / m2, such as in the range from 7.5 kN / m2to 20.0 kN / m2, preferably in the range from 8.0 kN / m2to 15.0 kN / m2, more preferably in the range from 8.5 kN / m2to 12.0 kN / m2,
[0163] - an impact strength (ISO179-1 , Charpy notched 1 eA +23°C, measured as described in the method section) of at least 5.0 kJ / m2, preferably of at least 5.5 kJ / m2, still more preferably of at least 6.0 kJ / m2, in particular in a range from 5.0 to 20.0 kJ / m2, more particular in a range from 5.5 to 15.0 kJ / m2, even more particular in a range from 6.0 to 10.0 kJ / m2,
[0164] - an impact strength (ISO179-1 , Charpy notched 1 eA -20°C, measured as described in the method section) of at least 1 .0 kJ / m2, preferably of at least 1 .3 kJ / m2, still more preferably of at least 1 .5 kJ / m2, in particular in a range from 1 .0 to 15.0 kJ / m2, more particular in a range from 1.3 to 10.0 kJ / m2, even more particular in a range from 1 .5 to 5.0 kJ / m2,
[0165] - a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C) of at most 3.0 g / 10 min; preferably of at most 2.5 g / 10 min, more preferably of at most 2.0 g / 10 min, even more preferably of at most 1.5 g / 10min, such as in the range from 0.3 to 3.0 g / 10 min, preferably from 0.5 to 2.5 g / 10min, more preferably 0.6 to 2.0 g / 10 min, even more preferably from 0.7 to 1.5 g / 10min,
[0166] - an OCS gel index (determined as described in the method section) of less than 1000, preferably of less than 800, more preferably of less than 600, such as from 50 and to less than 1000, in particular from 80 and to less than 800, such as from 100 to less than 600, preferably from 100 to 500, more preferably from 100 to 400,
[0167] - an OCS others (> 1000 pm, determined as described in the method section) of less than 2.0 1 / m2, preferably of less than 1 .5 1 / m2, such as in a range from 0.0 to less than 2.0 1 / m2, preferably in a range from 0.0 to less than 1.5 1 / m2, still more preferably in a range from 0.0 to less than 1 .0 1 / m2;
[0168] - an OCS contaminations (>1000 pm, determined as described in the method section) of less than 2.0 1 / m2, preferably of less than 1 .0 1 / m2, such as in a range from 0.0 to less than 2.0 1 / m2, preferably in a range from 0.0 to less than 1 .0 1 / m2,
[0169] - an OCS gel (>1000 pm, determined as described in the method section) of less than 1 .0 1 / m2, such as in a range from 0.0 to less than 1 .0 1 / m2,
[0170] DMTA (torsional)_E' +23°C (determined as described in the method section) of at least 600 MPa, preferably of at least 700 MPa, more preferably of at least 800 MPa, such as in a range from 600 to 2000 MPa, preferably from 700 to 1500 MPa, more preferably from 800 to 1000 MPa, even more preferably from 800 to 900 MPa;
[0171] - DMTA (torsional)_E' +60°C (determined as described in the method section) of at least 350 MPa, preferably of at least 400 MPa, such as in a range from 350 to 700 MPa, preferably from 350 to 600 MPa, even more preferably from 400 to 500 MPa,
[0172] - DMTA (torsional)_E' +90°C (determined as described in the method section) of at least 150 MPa, preferably of at least 200 MPa, such as in a range from 150 to 500 MPa, preferably from 200 to 400 MPa, more preferably from 250 to 350 MPa, DMTA (torsional)_E' -30°C (MPa) (determined as described in the method section) of at least 1600 MPa, more preferably of at least 1700 MPa, such as in a range from 1600 to 2300 MPa, preferably from 1700 to 2100 MPa, more preferably from 1750 to 1900 MPa,
[0173] DMTA (torsional)_E' 0°C (MPa) (determined as described in the method section) of at least 1100 MPa, preferably of at least 1200 MPa, such as in a range from 1100 to 2000 MPa, more preferably from 1200 to 1500 MPa, even more preferably from 1200 to 1400 MPa, - a failure time in pipe pressures testing (at +80°C, 4.2 MPa, determined as described in the method section) of at least 600 hours, preferably of at least 700 hours, such as in the range from 600 hours to 3000 hours, more preferably in the range from 700 hours to 2000 hours,
[0174] - a failure time in pipe pressures testing (at +95°C, 2.5 MPa, determined as described in the method section) of at least 1800 hours, preferably of at least 2000 hours, such as in the range from 1800 hours to 4000 hours, preferably in the range from 2000 hours to 3000 hours.
[0175] In still a further embodiment, the polyolefin composition PC-2 has in the Crystex analysis one or more, preferably all of the following properties:
[0176] - a total ethylene (C2) content in the range from 2.0 to 10.0 wt%, preferably from 2.5 to 8.0 wt%, more preferably from 3.0 to 8.0 wt%, and / or an intrinsic viscosity (IV) in the range from 2.0 to 4.0 dl / g; preferably in the range from 2.5 to 3.5 dl / g; and / or
[0177] - a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF) in the range from 1 .0 to 10.0 wt.-%, preferably from
[0178] 1 .5 to 8.0 wt%, more preferably from 2.0 to 8.0 wt%, even more preferably from 2.5 to
[0179] 4.5 wt %; and / or an intrinsic viscosity (IV(CF)) in the range from 2.0 to 4.0 dl / g, preferably in the range from 2.5 to 3.5 dl / g, and / or
[0180] - a soluble fraction (SF) in the range from 3.0 to 15.0 wt%, more preferably from 4.0 to 13.0 wt%, even more preferably from 5.0 to 10.0; still more preferably from 7.0 to 9.0 wt%.
[0181] - the soluble fraction (SF) having one or more, preferably all of the following properties: an ethylene content (C2(SF)) in the range from 10 to 40.0 wt.-% (based on the total weight of the soluble fraction), preferably from 15.0 to 35.0 wt%, more preferably from 20.0 to 30.0 wt%, and an intrinsic viscosity (IV(SF)) in the range from 1 .0 to 3.5 dl / g, preferably in the range from 1 .5 to 3.0 dl / g, more preferably in the range from 2.0 to 2.8 dl / g. HECO-1 , HECO-2 and Blend A-2
[0182] In an embodiment, the present polyolefin composition PC-3 comprises: a) in the range of from 47 to 80 wt%, preferably from 65 to 77 wt.-%, more preferably from 68 to 76 wt% (based on the overall weight of the polyolefin composition) of a mixture of the at least one heterophasic propylene copolymer HECO- 1 and the least one heterophasic propylene copolymer HECO-2; b) in the range from 20 to 53 wt%, even more preferably from 23 to 35 wt%, still more preferably from 24 to 32 wt% (based on the overall weight of the polyolefin composition) of a mixed-plastics polypropylene blend of recycled material Blend A-2, c) optionally further additives (based on the overall weight of the polyolefin composition), wherein the sum of all ingredients always adds up to 100 wt%.
[0183] In an embodiment, the at least one heterophasic propylene copolymer HECO-1 and the least one heterophasic propylene copolymer HECO-2 may be present in the mixture in a weight ratio from 5:95 to 95:5, preferably from 10:90 to 90:10, more preferably from 20:80 to 80:20, even more preferably from 30:70 to 70:30, such as from 33:67 to 50:50.
[0184] For example, at least 20 wt%, preferably at least 30 wt%, more preferably at least 34 wt% of the at least one heterophasic propylene copolymer HECO-1 and at least 30 wt%, preferably at least 34wt%, more preferably at least 40 wt% , such as at least 45wt% of the least one heterophasic propylene copolymer HECO-2 may be present in the mixture, wherein the sum of the at least one heterophasic propylene copolymer HECO-1 and the least one heterophasic propylene copolymer HECO-2 always adds up to a sum within the above mentioned range of range of from 47 to 80 wt%, preferably from 65 to 77 wt.-%, more preferably from 68 to 76 wt% (based on the overall weight of the polyolefin composition).
[0185] The polypropylene composition PC-3 comprising the least one heterophasic propylene copolymer HECO-1 and the least one heterophasic propylene copolymer HECO-2 and the blend of recycled material Blend A-2 may have one or more, preferably all of the following properties: a ring stiffness (determined as described in the method section) of at least 8.0 kN / m2, preferably of at least 8.5 kN / m2, more preferably of at least 9.0 kN / m2, still more preferably of at least 9.2 kN / m2, as in the range from 8.0 kN / m2to 20.0 kN / m2, preferably in the range from 8.5 kN / m2to 15.0 kN / m2, more preferably in the range from 9.0 kN / m2to 12.0 kN / m2,
[0186] - an impact strength (ISO179-1 , Charpy notched 1 eA +23°C, measured as described in the method section) of at least 6.0 kJ / m2, preferably of at least 6.5 kJ / m2, still more preferably of at least 7.0 kJ / m2, in particular in a range from 6.0 to 20.0 kJ / m2, more particular in a range from 6.5 to 15.0 kJ / m2, even more particular in a range from 7.0 to 10.0 kJ / m2,
[0187] - an impact strength (ISO179-1 , Charpy notched 1 eA -20°C, measured as described in the method section) of at least 1 .5 kJ / m2, preferably of at least 1 .7 kJ / m2, still more preferably of at least 2.0 kJ / m2, in particular in a range from 1 .5 to 15.0 kJ / m2, more particular in a range from 1.7 to 10.0 kJ / m2, even more particular in a range from 2.0 to 5.0 kJ / m2,
[0188] - a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C) of at most 3.0 g / 10 min; preferably of at most 2.5 g / 10 min, more preferably of at most 2.0 g / 10 min, even more preferably of at most 1.5 g / 10min, such as in the range from 0.3 to 3.0 g / 10 min, preferably from 0.5 to 2.5 g / 10min, more preferably 0.6 to 2.0 g / 10 min, even more preferably from 0.7 to 1.5 g / 10min,
[0189] - an OCS gel index (determined as described in the method section) of less than 1000, preferably of less than 800, more preferably of less than 500, such as from 50 and to less than 1000, in particular from 80 and to less than 800, such as from 100 to less than 500, preferably from 100 to 400, more preferably from 100 to 300, even more preferably from 100 to 200,
[0190] - an OCS others (> 1000 pm, determined as described in the method section) of less than 2.0 1 / m2, preferably of less than 1 .5 1 / m2, such as in a range from 0.0 to less than 2.0 1 / m2, preferably in a range from 0.0 to less than 1.5 1 / m2, still more preferably in a range from 0.0 to less than 1 .0 1 / m2;
[0191] - an OCS contaminations (>1000 pm, determined as described in the method section) of less than 2.0 1 / m2, preferably of less than 1 .0 1 / m2, such as in a range from 0.0 to less than 2.0 1 / m2, preferably in a range from 0.0 to less than 1 .0 1 / m2,
[0192] - an OCS gel (>1000 pm, determined as described in the method section) of less than 1 .0 1 / m2, such as in a range from 0.0 to less than 1 .0 1 / m2,
[0193] - DMTA (torsional)_E' +23°C (determined as described in the method section) of at least 600 MPa, preferably of at least 700 MPa, more preferably of at least 800 MPa, such as in a range from 600 to 2000 MPa, preferably from 700 to 1500 MPa, more preferably from 800 to 1000 MPa, even more preferably from 830 to 950 MPa; - DMTA (torsional)_E' +60°C (determined as described in the method section) of at least 350 MPa, preferably of at least 400 MPa, such as in a range from 350 to 700 MPa, preferably from 350 to 600 MPa, even more preferably from 400 to 500 MPa,
[0194] - DMTA (torsional)_E' +90°C (determined as described in the method section) of at least 150 MPa, preferably of at least 200 MPa, such as in a range from 150 to 500 MPa, preferably from 200 to 400 MPa, more preferably from 250 to 350 MPa, DMTA (torsional)_E' -30°C (MPa) (determined as described in the method section) of at least 1800 MPa, more preferably of at least 1850 MPa, such as in a range from 1800 to 2300 MPa, preferably from 1850 to 2100 MPa, more preferably from 1800 to 2000 MPa,
[0195] DMTA (torsional)_E' 0°C (MPa) (determined as described in the method section) of at least 1100 MPa, preferably of at least 1200 MPa, such as in a range from 1100 to 2000 MPa, more preferably from 1200 to 1500 MPa, even more preferably from 1250 to 1400 MPa,
[0196] - a failure time in pipe pressures testing (at +80°C, 4.2 MPa, determined as described in the method section) of at least 800 hours, preferably of at least 900 hours, such as in the range from 800 hours to 4000 hours, more preferably in the range from 900 hours to 3000 hours,
[0197] - a failure time in pipe pressures testing (at +95°C, 2.5 MPa, determined as described in the method section) of at least 2000 hours, preferably of at least 2500 hours, such as in the range from 2000 hours to 5000 hours, preferably in the range from 2500 hours to 4000 hours.
[0198] In still a further embodiment, the polyolefin composition PC-3 has in the Crystex analysis one or more, preferably all of the following properties:
[0199] - a total ethylene (C2) content in the range from 2.0 to 10.0 wt%, preferably from 2.5 to 8.0 wt%, more preferably from 3.0 to 8.0 wt%, and / or an intrinsic viscosity (IV) in the range from 2.0 to 4.0 dl / g; preferably in the range from 2.5 to 3.5 dl / g; and / or
[0200] - a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF) in the range from 1 .0 to 10.0 wt.-%, preferably from 1 .5 to 8.0 wt%, more preferably from 2.0 to 5.0 wt%, even more preferably from 2.0 to 3.0 wt %; and / or an intrinsic viscosity (IV(CF)) in the range from 2.0 to 4.0 dl / g, preferably in the range from 2.5 to 3.5 dl / g, and / or
[0201] - a soluble fraction (SF) in the range from 2.0 to 15.0 wt.-%, preferably from 3.0 to 13.0 wt%, more preferably from 5.0 to 10.0 wt%, even more preferably from 6.0 to 8.0 wt%.
[0202] - the soluble fraction (SF) having one or more, preferably all of the following properties: an ethylene content (C2(SF)) in the range from 10 to 40.0 wt.-% (based on the total weight of the soluble fraction), preferably from 15.0 to 35.0 wt%, more preferably from 20.0 to 30.0 wt%, and an intrinsic viscosity (IV(SF)) in the range from 1 .0 to 3.5 dl / g, preferably in the range from 1 .5 to 3.0 dl / g, more preferably in the range from 2.0 to 2.5 dl / g.
[0203] The present invention is also directed to an article comprising the polyolefin composition according to the invention.
[0204] The polyolefin composition according to the invention can be used for a wide range of applications, in particular for pipes.
[0205] Process for preparinq the
[0206] It is appreciated that the present invention also refers to a process for producing the polyolefin compositions as defined herein. The process comprises the steps of
[0207] - providing the at least one heterophasic propylene copolymer and the blend of recycled plastic material,
[0208] - feeding / dosing the at least one heterophasic propylene copolymer and the blend of recycled plastic material separately or as a mixture into at least one extruder,
[0209] - melting the mixture in the at least one extruder, and
[0210] - optionally pelletizing the obtained polyolefin composition.
[0211] The inventive composition is preferably obtained by blending, preferably by melt mixing of the components in an extruder. The term "blending" according to this invention covers a dry mixing as well as melt mixing, like melt extruding, of substances. In case of melt mixing it is preferred to feed the substances into an extruder either as a dry blend or separately via different feeders. In case of melt mixing the obtained composition is preferably in the form of pellets. It is possible first to blend, like to melt mix, the recyclate and the heterophasic propylene copolymer (HECO) obtaining thereby a mixture, like pellets in case of melt mixing, and subsequently this mixture, e.g. said pellets, is / are blended, preferably melt mixed, with the other components of the composition, like the additives (AD). However it is preferred to produce the composition in one step, i.e. adding all components in one mixing step.
[0212] In a preferred embodiment, the inventive composition is obtainable by melt mixing the components in a co-rotating twin screw extruder at a screw speed of preferably not more than 600 rpm, more preferably not more than 500 rpm, even more preferably not more than 400 rpm, such as in a range between 100 and 600 rpm, preferably in a range between150 and 500 rpm, more preferably in a range between 200 and 400 rpm; and / or at a barrel temperature of not more than 270 °C, preferably not more than 260 °C, more preferably not more than 250°C, still more preferably not more than 240°C.
[0213] For instance, in case of melt mixing the components of the composition may be added via one feeder (the components may have been pre-dry mixed) or the components may be added via different feeders into the extruder obtaining thereby the composition preferably in form of pellets.
[0214] Accordingly in case the composition consists of the recyclate, the heterophasic propylene copolymer (HECO) and the optional additives (AD), both components or all three components, in case additives (AD) are present, are dry mixed or preferably melt mixed, more preferably melt extruded, obtaining thereby the composition either in form of a dry mixture or in case of melt mixing or melt extruding in form of pellets. It is also possible that the virgin, recycled PP and optionally additives are mixed and extruded into pipes directly.
[0215] Alternatively first a dry mixture or pellets obtained by melt mixing of the recyclate and the heterophasic propylene copolymer (HECO) is produced and subsequently the inventive composition is obtained by mixing to said dry mixture or to said melted mixture, like the pellets, the additives (AD) in the way of dry mixing or preferably by way of melt mixing, thereby obtaining the composition either in form of a dry blend or as melted mixture, like pellets. Experimental Section
[0216] The following Examples are included to demonstrate certain aspects and embodiments of the invention as described in the claims. It should be appreciated by those of skill in the art, however, that the following description is illustrative only and should not be taken in any way as a restriction of the invention.
[0217] Process and processing
[0218] Compounding
[0219] The compounds were produced on a Coperion W&P ZSK32 co-rotating, twin-screw extruder (screw diameter of 32mm and l_ / D=48) at barrel temperatures of 180 to 230°C and screw speed of 300 rpm.
[0220] Pipe extrusion
[0221] The pipe samples were produced on semi-commercial pipe extrusion lines from Krauss-Maffei GmbH. The line consists of an extruder with a 0 45 mm screw with an L / D ratio of 36D. The extruder temperature was set at 180-225°C, the melt temperature was 200-230°C and was recorded after 120 min of process stabilization. The extruder is followed by a pipe tool, which is equipped with a 0 132 mm annular die with a die gap of 2-50 mm. The line was run at a constant throughput of 120 kg / h and a line speed of about 1 .5 m / min, with water temperature of 30°C in the vacuum spray bath, vacuum level of 0.3 bars in the vacuum cooling tank. The pipe was produced with a thickness of 4 mm and outer diameter of 110 mm.
[0222] Test method description
[0223] Amount of “iPP”, “PVC”, “PA”, “PET”, “PS” and “C2 rich” determination by Transmission infra-Red spectroscopy (IR)
[0224] Sample preparation:
[0225] All calibration samples and samples to be analyzed are prepared in similar way, on molten pressed plates.
[0226] Around 2 to 3 g of compounds to be analyzed are molten at 190°C. Subsequently, for 20 seconds 60 to 80 bar pressure is applied in a hydraulic heating press. Next, the samples are cooled down to room temperature in 40 second in a cold press under the same pressure, in order to control the morphology of the compound. The thickness of the plates are controlled by metallic calibrated frame plates 2.5 cm by 2.5 cm, 100 to 200 pm thick (depending MFR from the sample); two plates are produced in parallel at the same moment and in the same conditions. The thickness of each plate is measured before any FTIR measurements; all plates are between 100 to 200 pm thick.
[0227] To control the plate surface and to avoid any interference during the measurement, all plates are pressed between two double-sided silicone release papers.
[0228] In case of powder samples or heterogeneous compounds, the pressing process would be repeated three times to increase homogeneity by pressed and cutting the sample in the same conditions as described before.
[0229] Spectrometer:
[0230] Standard transmission FTIR spectroscope such as Bruker Vertex 70 FTIR spectrometer is used with the following set-up:
[0231] • a spectral range of 4000-400 cm-1,
[0232] • an aperture of 6 mm,
[0233] • a spectral resolution of 2 cm-1,
[0234] • with 16 background scans, 16 spectrum scans,
[0235] • an interferogram zero filling factor of 32
[0236] • Norton Beer strong apodisation.
[0237] Spectrum are recorded and analysed in Bruker Opus software.
[0238] Calibration samples:
[0239] As FTIR is a secondary method, several calibration standards were compounded to cover the targeted analysis range, typically from:
[0240] • 0.2 wt% to 2.5 wt% for PA
[0241] • 0.1 wt% to 5 wt% for PS
[0242] • 0.2 wt% to 2.5 wt% for PET
[0243] • 0.1 wt% to 4 wt% for PVC
[0244] The following commercial materials were used for the compounds: Borealis HC600TF as iPP, Borealis FB3450 as HDPE and for the targeted polymers such RAMAPET N1 S (Indorama Polymer) for PET, Ultramid® B36LN (BASF) for Polyamide 6, Styrolution PS 486N (Ineos) for High Impact Polystyrene (HIPS), and for PVC Inovyn PVC 263B (under powder form). All compounds are made at small scale in a Haake kneader at a temperature below 265°C and less than 10 minutes to avoid degradation.
[0245] Additional antioxidant such as Irgafos 168 (3000 ppm) is added to minimize the degradation.
[0246] Calibration:
[0247] The FTIR calibration principal is the same for all the components: the intensity of a specific FTIR band divided by the plate thickness is correlated to the amount of component determined by 1 H or 13C solution state NMR on the same plate.
[0248] Each specific FTIR absorption band is chosen due to its intensity increase with the amount of the component concentration and due to its isolation from the rest of the peaks, whatever the composition of the calibration standard and real samples.
[0249] This methodology is described in the publication from Signoret and al. “Alterations of plastic spectra in MIR and the potential impacts on identification towards recycling”, Resources, conservation and Recycling journal, 2020, volume 161 , article 104980.
[0250] The wavelength for each calibration band is:
[0251] • 3300 cm’1for PA,
[0252] • 1601 cnrr1for PS,
[0253] • 1410 cm’1for PET,
[0254] • 615 cnr1for PVC,
[0255] • 1167 cm1for iPP.
[0256] For each polymer component i, a linear calibration (based on linearity of Beer-Lambert law) is constructed. A typical linear correlation used for such calibrations is given below: where Xi is the fraction amount of the polymer component i (in wt%)
[0257] Ei is the absorbance intensity of the specific band related to the polymer component i (in a.u. absorbance unit). These specific bands are, 3300 cnr1for PA, 1601 cm1for PS, 1410 cm-1for PET, 615 cm1for PVC, 1167 cm-1for iPP d is the thickness of the sample plate A and Bi are two coefficients of correlation determined for each calibration curve
[0258] No specific isolated band can be found for C2 rich fraction and as a consequence the C2 rich fraction is estimated indirectly, xC2 rich=100—(XiPP +XPA +XPS+ XPET+ XEVA+ XPVC+ Xchaik+ Xtajc)
[0259] The EVA, Chalk and Talc contents are estimated “semi-quantitatively”. Hence, this renders the C2 rich content “semi-quantitative".
[0260] The following bands are used to estimate the EVA, Chalk and Talc contents:
[0261] EVA: band centred at 607 crrr1
[0262] Chalk : band centred at 1798 cm-1
[0263] Talc : band centred at 3676 crrr1
[0264] In addition, the presence of titanium di-oxide, TiOz and Carbon Black are reported. Their quantifications are not feasible with FTIR.
[0265] For each calibration standard, wherever available, the amount of each component is determined by either1H or13C solution state NMR, as primary method (except for PA). The NMR measurements are performed on the exact same FTIR plates used for the construction of the FTIR calibration curves.
[0266] Crystex analysis
[0267] The crystalline (CF) and soluble fractions (SF) of the polypropylene (PP) compositions as well as the comonomer content and intrinsic viscosities of the respective fractions were analyzed by use of the Crystex (crystallisation extraction) method. Potential instruments that can be used are Crystex QC or Crystex 42 (Polymer Char; Valencia, Spain). Details of the technique and the method can be found in literature (Ljiljana Jeremie, Andreas Albrecht, Martina Sandholzer & Markus Gahleitner (2020): Rapid characterization of high-impact ethylenepropylene copolymer composition by crystallization extraction separation: comparability to standard separation methods, International Journal of Polymer Analysis and Characterization, 25:8, 581 -596) The crystalline and amorphous fractions are separated through temperature cycles of dissolution at 160°C, crystallization at 40°C and re-dissolution in 1 ,2,4-trichlorobenzene at 160°C. Quantification of SF and CF and determination of ethylene content (C2) are achieved by means of an integrated infrared detector (IR4) and for the determination of the intrinsic viscosity (IV) an online 2-capillary viscometer is used.
[0268] IR4 detector is a multiple wavelength detector measuring IR absorbance at two different bands (CH3 stretching vibration (centred at app. 2960 cm-1) and the CH stretching vibration (2700- 3000 cm-1) that are serving for the determination of the concentration and the Ethylene content in Ethylene-Propylene copolymers. IR4 detector is calibrated with series of 8 EP copolymers with known Ethylene content in the range of 2 wt.-% to 69 wt.-% (determined by 13C-NMR) and each at various concentrations, in the range of 2 and 13mg / ml. To encounter for both features, concentration and ethylene content at the same time for various polymer concentration expected during Crystex analyses the following calibration equations were applied:
[0269] Cone = a + b*Abs(CH) + c*(Abs(CH))2+ d*Abs(CH3) + e*(Abs(CH3)2+ f*Abs(CH)*Abs(CH3) (Equation 1)
[0270] CH3 / 1000TC = a + b*Abs(CH) + c* Abs(CH3) + d * (Abs(CH3) / Abs(CH)) + e * (Abs(CH3) / Abs(CH))2(Equation 2)
[0271] The constants a to f for equation 1 and a to e for equation 2 were determined by using least square regression analysis.
[0272] The CH3 / 1000TC (total C Atoms) is converted to the ethylene content in wt.-% using following relationship:
[0273] Wt.-% (Ethylene in EP Copolymers) = 100 - CH3 / 1000TC * 0.3 (Equation 3)
[0274] Amount of Soluble fraction (SF) and Crystalline Fraction (CF) are correlated through the XS calibration to the “Xylene Cold Soluble” (XCS) quantity and respectively Xylene Cold Insoluble (XCI) fractions, determined according to standard gravimetric method as per ISO16152. XS calibration is achieved by testing various EP copolymers with XS content in the range 2-31 Wt%. A linear calibration curve is used: Wt.-% XS = a * Wt.-% SF (Equation 4)
[0275] Intrinsic viscosity (IV) of the parent EP copolymer and its soluble and crystalline fractions are determined with a use of an online 2-capillary viscometer and are correlated to corresponding IV’s determined by standard method in decalin according to ISO 1628-3. Calibration is achieved with various EP copolymers and PP polymers with IV = 2-4 dL / g. The determined calibration curve is linear.
[0276] IV (dl / g) = a * Vsp / c (Equation 5)
[0277] The constant a for equation 4 and 5 was determined by using least square regression analysis respectively.
[0278] The samples to be analyzed are weighed out in concentrations of 10 mg / ml to 20mg / ml.
[0279] After automated filling of the vial with 1 ,2,4-TCB containing 250 mg / l 2,6-tert-butyl-4- methylphenol (BHT) as antioxidant, the sample is dissolved at 170°C until complete dissolution is achieved with either constant stirring or gentle shaking. To avoid sample degradation, polymer solution is blanketed with the N2 atmosphere during dissolution.
[0280] For PP composition containing inorganic fillers or pigments or any other non-TCB soluble polymeric substances removal of these is required. This can be done by hot filtration prior to injection.
[0281] A defined volume of the polymer solution is injected into the column filled with inert support where the crystallization of the sample and separation of the soluble fraction from the crystalline fraction is taking place. This process is repeated two times. During the first injection the whole sample is measured at high temperature, determining the I V[dl / g] and the C2[wt%] of the PP composition. During the second injection the soluble fraction SF (at low temperature) and the crystalline fraction CF (at high temperature) with the crystallization cycle are measured (SF[wt%], C2(SF)[wt%], IV(SF)[dl / g], C2(CF)[wt%], IV(CF)[dl / g]).
[0282] Quantification of microstructure by NMR spectroscopy (for CRYSTEX calibration) Quantitative nuclear-magnetic resonance (NMR) spectroscopy was used for calibration.
[0283] Quantitative 13C{ 1 H} NMR spectra were recorded in the solution-state using a Bruker Avance Neo 400 NMR spectrometer operating at 400.15 and 100.62 MHz for 1 H and 13C respectively. All spectra were recorded using a 13C optimized 10 mm extended temperature probe head at 125°C using nitrogen gas for all pneumatics. Approximately 200 mg of material was dissolved in approximately 3 ml of 1 ,1 ,2,2-tetrachloroethane-d2 (TCE-d2) along with approximately 3 mg BHT (2,6-di-tert-butyl-4-methylphenol CAS 128-37-0) and chromium-(lll)-acetylacetonate (Cr(acac)3) resulting in a 60 mM solution of relaxation agent in solvent as described in G. Singh, A. Kothari, V. Gupta, Polymer Testing 2009, 28(5), 475.
[0284] To ensure a homogenous solution, after initial sample preparation in a heat block, the NMR tube was further heated in a rotatory oven for at least 1 hour. Upon insertion into the magnet the tube was spun at 10 Hz. This setup was chosen primarily for the high resolution and quantitatively needed for accurate ethylene content quantification. Standard single-pulse excitation was employed without NOE, using an optimised tip angle, 1 s recycle delay and a bi-level 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 acquired per spectra.
[0285] Quantitative 13C{1 H} NMR spectra were processed, integrated and relevant quantitative properties determined from the integrals. All chemical shifts were indirectly referenced to the central methylene group of the ethylene block (EEE) at 30.00 ppm using the chemical shift of the solvent. This approach allowed comparable referencing even when this structural unit was not present.
[0286] Characteristic signals corresponding to the incorporation of ethylene were observed (as described in Cheng, H. N., Macromolecules 1984, 17, 1950) and the comonomer fraction calculated as the fraction of ethylene in the polymer with respect to all monomer in the polymer: fE = ( E / ( P + E )
[0287] The comonomer fraction was quantified using the method of W-J. Wang and S. Zhu, Macromolecules 2000, 33 1157, through integration of multiple signals across the whole spectral region in the 13C{1 H} spectra. Integral regions were slightly adjusted to increase applicability across the whole range of encountered comonomer contents.
[0288] The mole percent comonomer incorporation was calculated from the mole fraction:
[0289] E [mol%] = 100 * fE
[0290] The weight percent comonomer incorporation was calculated from the mole fraction:
[0291] E [wt%] = 100 * ( fE * 28.06 ) / ( (fE * 28.06) + ((1 -fE) * 42.08) ). DMTA torsional
[0292] The characterization of polymers in the solid state under oscillatory deformation in torsional mode complies with ISO standards 6721 -1 , 6721 -7 and 6721 -11. The measurements were performed on Anton Paar MCR702 on rectangular samples with length of around 10 mm, width of around 2 mm and thickness of around 1 mm, which were cut from compression-moulded plates. The samples are held with grips under a normal force of 0.6 N. The frequency is set to 1 Hz (6.28 rad / s), and the strain amplitude is set within the linear viscoelastic regime about 0.2%.
[0293] The temperature was controlled using liquid nitrogen (N2), increased from initial temperature of Ti=-130°C, to final temperature of Tfaround 160°C, when the E’ is lower than 1 MPa, by heating rate of 2 K / min.
[0294] The storage, and loss moduli (E’, and E”) as well as phase shift Tan6 (Tan(delta)) are recorded over temperature ramp. The values of E’ at certain temperatures (for instance -150, -50, -30, 23, 60, 90, 120 °C) as well as the temperatures of peaks and shoulders for E” and Tan6 (Tan(delta)) are tracked for comparison.
[0295] Frequency sweep (FS)
[0296] 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. Measurements were undertaken on compression moulded plates using nitrogen atmosphere and setting a strain within the linear viscoelastic regime. The oscillatory shear tests were done at 200°C applying a frequency range between 0.01 and 600 rad / s and setting a gap of 1.3 mm.
[0297] In a dynamic shear experiment the probe is subjected to a homogeneous deformation at a sinusoidal varying shear strain or shear stress (strain and stress controlled mode, respectively). On a controlled strain experiment, the probe is subjected to a sinusoidal strain that can be expressed by y(t) = Yo sin(wt) (1 )
[0298] If the applied strain is within the linear viscoelastic regime, the resulting sinusoidal stress response can be given by o(t) = Oo sin(wt +5) (2) where a0, and Yo are the stress and strain amplitudes, respectively; w is the angular frequency; 5 is the phase shift (loss angle between applied strain and stress response); t is the time.
[0299] Dynamic test results are typically expressed by means of several different rheological functions, namely the shear storage modulus, G’, the shear loss modulus, G”, the complex shear modulus, G*, the complex shear viscosity, q*, the dynamic shear viscosity, q', the out- of-phase component of the complex shear viscosity, q" and the loss tangent, tan q, which can be expressed as follows:
[0300] The determination of so-called Shear Thinning Index, which correlates with MWD and is independent of Mw, is done as described in equation 9.
[0301] For example, the SHI(2.7 / 2io) is defined by the value of the complex viscosity, in Pa s, determined for a value of G* equal to 2.7 kPa, divided by the value of the complex viscosity, in Pa s, determined for a value of G* equal to 210 kPa.
[0302] The SHI(i / ioo) is accordingly defined by the value of the complex viscosity, in Pa s, determined for a value of G* equal to 1 kPa, divided by the value of the complex viscosity, in Pa s, determined for a value of G* equal to 100 kPa.
[0303] The values of storage modulus (G')> loss modulus (G"), complex modulus (G*) and complex viscosity (q*) were obtained as a function of frequency (co).
[0304] Thereby, e.g. q*3oorad / s (eta*3oorad / s or Eta at 300 rad / s) is used as abbreviation for the complex viscosity at the frequency of 300 rad / s and q*o.o5rad / s (eta*o.osrad / s or Eta at 0.05 rad / s) is used as abbreviation for the complex viscosity at the frequency of 0.05 rad / s.
[0305] The loss tangent tan (delta) is defined as the ratio of the loss modulus (G") and the storage modulus (G') at a given frequency. Thereby, e.g. tan0.05 is used as abbreviation for the ratio of the loss modulus (G") and the storage modulus (G') at 0.05 rad / s and tan3oo is used as abbreviation for the ratio of the loss modulus (G") and the storage modulus (G') at 300 rad / s.
[0306] The elasticity balance tano.o5 / tan3oo is defined as the ratio of the loss tangent tan0.05 and the loss tangent tan3oo.
[0307] Besides the above mentioned rheological functions one can also determine other rheological parameters such as the so-called elasticity index El(x). The elasticity index Ei(x) is the value of the storage modulus, G’ determined for a value of the loss modulus, G” of x kPa and can be described by equation 10.
[0308] EI x) = G' for (G" = x kPa) [Pa] (10)
[0309] For example, the EI(5kPa) is the defined by the value of the storage modulus G’, determined for a value of G” equal to 5 kPa, the EI(2kPa) is the defined by the value of the storage modulus G’, determined for a value of G” equal to 2 kPa and the EI(0.5kPa) is the defined by the value of the storage modulus G’, determined for a value of G” equal to 0.5 kPa.
[0310] The rheological polydispersity index, PI, is defined by equation 11 . where COCOP is the cross-over angular frequency, determined as the angular frequency for which the storage modulus, G', equals the loss modulus, G".
[0311] The values are determined by means of a single point interpolation procedure, as defined by Rheoplus software. In situations for which a given G* value is not experimentally reached, the value is determined by means of an extrapolation, using the same procedure as before. In both cases (interpolation or extrapolation), the option from Rheoplus "Interpolate y-values to x- values from parameter" and the "logarithmic interpolation type" were applied.
[0312] The so-called Zero Shear Viscosity (ZSV) is the plateau viscosity at low enough shear rate (angular frequency). It is determined by fitting the Garreau-Yasuda model on the complex viscosity versus angular frequency. The Garreau-Yasuda equation describes the viscosity curve of a material with Newtonian regions at low shear rates and a shear thinning (power law) region at medium shear rates. Fitting is done by Rheoplus or Rheocompass software by equation 12. w angular frequency in rad / s h * complex viscosity in Pa s h0zero shear viscosity in Pa-s a Garreau constant n shear thinning exponent
[0313] 2. relaxation time in s
[0314] As the ZSV (in low frequency regions) is not always fully reached within applied experimental conditions, the determination of the ZSV shall be done with special care to avoid extreme extrapolations, for example and thus, high errors.
[0315] For example, if the last experimental data point for the complex viscosity (e.g. at 0.01 rad / s) is about 70% of the calculated Zero Shear Viscosity ( / i0) value by fitting of Carreau-Yasuda model, then the calculated h0can be accepted. For cases in which the deviation is higher (last experimental complex viscosity < 70% of calculated h0), the h0should not be reported. The estimation of the rheological behaviour at low frequencies, can be alternatively done, by providing the complex viscosity at an angular frequency of 0.05 rad / s (eta @0.05 rad / s).
[0316] References:
[0317]
[0001] “Rheological characterization of polyethylene fractions", Heino, E.L., Lehtinen, A., Tanner J., Seppala, J., Neste Oy, Porvoo, Finland, Theor. Appl. Rheol., Proc. Int. Congr. Rheol, 11th (1992), 1 , 360-362.
[0318] [2] “The influence of molecular structure on some rheological properties of polyethylene", Heino, E.L., Borealis Polymers Oy, Porvoo, Finland, Annual Transactions of the Nordic Rheology Society, 1995.
[0319] [3] “Definition of terms relating to the non-ultimate mechanical properties of polymers”, Pure & Appl. Chem., Vol. 70, No. 3, pp. 701 -754, 1998.
[0320] DSC
[0321] A TA Instruments Q200 Differential Scanning Calorimeter calibrated with Indium, Zinc, and Tin and operating under 50 mL / min of nitrogen flow was used. The employed thermal program consisted of a first heating step from 0 to 225°C to erase the previous thermal history and a cooling step at 10 °C / min. The melting behavior was obtained by performing a second heating scan from 0 to 225 °C at 10 °C / min. The crystallization and melting temperatures were taken as the peak values from the cooling and second heating scan respectively. The DSC trace was integrated from 50°C to the end of the melting peak to evaluate the melting enthalpy (fusion heat) or crystallization enthalpy.
[0322] OCS (reflection mode) The cast film samples were produced and optically examined on a small-scale laboratory cast film line with installed camera detection from Optical Control Systems GmbH.
[0323] The line consists of an extruder with a 0 25 mm screw with an L / D ratio of 25. The extruder temperature was set at 200-220-230-240-240 °C in five zones, the melt temperature was 230- 240 °C. The extruder is followed by a die with a width of 150 mm and a fixed die gap of 0.5 mm. The film were produced by extrusion at a screw speed of 30 rpm with a thickness of 100 pm. During the extrusion the chill-roll temperature was set at 50-80 °C. The gels and contaminations of the film were detected and counted on 5 m2of the film during the extrusion process with reflected light and a 4096 pixel camera. During the measurement a LED light source was used. The resolution of the camera is x / y 25 pm on film. The defects, i.e., gels, contaminations and others, were divided into 4 size-classes (100-299 pm; 300-599 pm; 600- 1000 pm; >1000 pm), and the results are presented as the number of defects per square meter (1 / m2).
[0324] If the ratio between length and width of the detected spots is not more than 4.5, the spots are categorized as “gels” (having pixels with grey value of not more than 50% but more than 10% of the average grey value) or “contaminations” (having pixels with grey value of not more than 10% of the average grey value). If the ratio between length and width of the detected spots is greater than 4.5 and their pixels have grey value of not more than 50% of the average grey value, the spots are categorized as “Others”.
[0325] The “gel index” is calculated by multiplying the amount of gels in each size class by factors for the size classes (0.1 ; 1 ; 5; 10) and adding these values together.
[0326] MFR2
[0327] The melt flow rate (MFR) was determined at a temperature of 230 °C and a load of 2.16 kg. according to ISO 1133 - Determination of the melt mass-flow rate (MFR) and melt volume-flow rate (MVR) of thermoplastics - Part 1 : Standard method and is indicated in g / 10 min. The MFR is an indication of the flowability, and hence the processability, of the polymer. The higher the melt flow rate, the lower the viscosity of the polymer.
[0328] Oven ash content
[0329] The ash content was measured at 950°C by an oven method according to ISO 3451 -1 (1997).
[0330] Mechanical testing Specimen preparation for mechanical testing
[0331] Test specimens for measurements of Charpy notched impact strength, tensile properties, were injection moulded (IM) according to ISO 294-1 and ISO 19069-2 on the injection moulding machine Engel VC 200 / 60 tech with a screw diameter of 22 mm.
[0332] Charpy notched impact strength of injection moulded specimens
[0333] Charpy notched impact strength was determined according to ISO 179-1 / 1 eA on notched specimen of 80 mm x10 mm x 4 mm (specimen according to ISO 179-1 / 1 eA). Testing temperature was 23±2° C or -20±2° C. Injection moulding was carried out to prepare the specimens according to “specimen preparation for mechanical testing”.
[0334] Tensile testing of injection moulded specimens
[0335] The tensile properties, including tensile modulus, tensile stress at break, tensile strain at break, were determined according to ISO 527-2 method B on 1A ISO 527-2 dogbone specimens. Following the standard, a test speed of 1 mm / min was used for tensile modulus and 50mm / min for all other properties. The testing temperature was 23±2° C. Injection moulding was carried out to prepare the specimens according to “specimen preparation for mechanical testing”.
[0336] Application testing
[0337] Ring stiffness
[0338] Ring stiffness tests were performed according to ISO 9969 at +23 °C on pipe specimens.
[0339] The test pipe specimens had a wall thickness of 4 mm, an outer diameter of 110 mm and a length of 300 mm. The diameter and wall thickness of the pipe were measured at one pipe end (a cutting end).
[0340] Impact resistance evaluated by external blow test
[0341] External blow test was conducted according to ISO 11173: 2018.
[0342] The test pipe specimens had a wall thickness of 4mm, outside diameter of 110 mm and a length of 20mm. The testing conditions used were: striker type d90, weight of 4 kg and a testing temperature of -10 °C. Drop height for 50 % failure (H5o) was reported to evaluate the impact resistance. The maximum drop height is 3000 mm that can be measured.
[0343] Internal pressure testing (IPT)
[0344] Internal pressure testing was conducted according to ISO 1167-1 :2006 standard. The pipes were extruded with a wall thickness of 4 mm, an outer diameter of 110 mm and cut to test specimens with a length of 650 mm by a band saw. The medium was water inside and water outside environment according to ISO 1167-1 : 2006. The testing conditions used were: temperature 80°C, hoop stress 4.2 MPa; temperature 95°C, hoop stress 2.5 MPa. 3 pipe specimens were tested for each material in each condition sets.
[0345] End caps of type A were used and the time of failure was determined in hours.
[0346] Material / process description
[0347] Manufacturing of HECO-1
[0348] HECO-1 was prepared according to EP2145923, in the presence of a Ziegler-Natta catalyst which had been prepared as described for example in WO 00 / 68315. The matrix is made of a propylene homopolymer which was prepared in a loop reactor and a gas phase reactor (GPR1). Further information about the propylene homopolymer constituting the matrix is shown in Table 1 .Subsequently, the propylene homopolymer was transferred to a second gas phase reactor (GPR2) where the elastomeric polypropylene was prepared. Grindsted PS 432 (a glycerol ester compound) was added to the second gas phase reactor at a feed rate of 3.3 g / h. Further information about the process parameters is provided in Table 1.
[0349] Table 1 : Polymerization conditions for HECO-1
[0350] C2 ethylene
[0351] H2 / C3 ratio hydrogen I propylene ratio
[0352] C2 / C3 ratio ethylene / propylene ratio
[0353] Manufacturing of HECO-2
[0354] Preparation of the catalyst
[0355] First, 0.1 mol of MgCI2x 3 EtOH was suspended under inert conditions in 250 ml of decane in a reactor at atmospheric pressure. The solution was cooled to the temperature of -15°C and 300 ml of cold TiCl4 was added while maintaining the temperature at said level. Then, the temperature of the slurry was increased slowly to 20 °C. At this temperature, 0.02 mol of diethylhexylphthalate (DOP) was added to the slurry. After the addition of the phthalate, the temperature was raised to 135 °C during 90 minutes and the slurry was allowed to stand for 60 minutes. Then, another 300 ml of TiCl4 was added and the temperature was kept at 135 °C for 120 minutes. After this, the catalyst was filtered from the liquid and washed six times with 300 ml heptane at 80 °C. Then, the solid catalyst component was filtered and dried. Catalyst and its preparation concept is described in general e.g. in patent publications EP 491 566, EP 591 224 and EP 586 390.
[0356] For the preparation of the HECO-2 as indicated below triethylaluminium (TEAL), dicyclopentyldimethoxysilane (D-donor), catalyst as produced above and vinyl cyclohexane (VCH) were added into oil, like mineral oil, e.g. Technol 68 (kinematic viscosity at 40 °C 62-74 cSt), in amounts so that TEAL / Ti was 125 mol / mol, TEAL / D donor was 5 mol / mol, and weight ratio of VCH / solid catalyst was 1 :1. The mixture was heated to 60 - 65 °C and allowed to react until the content of the unreacted vinylcyclohexane in the reaction mixture was ~ 150 ppm. Catalyst concentration in the final oil- catalyst slurry was 10 - 20 wt-%.
[0357] Table 2 : Polymerization conditions for HECO-2
[0358] C2 ethylene
[0359] IV intrinsic viscosity
[0360] XCS xylene cold soluble fraction
[0361] H2 / C3 ratio hydrogen I propylene ratio C2 / C3 ratio ethylene I propylene ratio
[0362] Loop Loop reactor
[0363] GPR 1 / 2 gas phase reactor 1 / 2 Dosina aaent
[0364] HA001 A-B1 is a commercial propylene homopolymer of Borealis having a melt flow rate MFR2 (230 °C) of 0.6 g / 10 min.
[0365] The following additives were used: Acid scavenger: AS1 (Ceasit AV / T), Antioxidants: AO1 (lrganox1010FF), AO2 (Kinox-68G), AO3 (Songnox DSTDP SB).
[0366] In Table 3 several examples (comparative-CE; inventive-IE) are summarized. The amounts of additives / dosing agent are those added during the melt blending, not including the ones resulting from virgin polymer(s) or recycled polymer(s).
[0367] The recyclate Blends A-1 and A-2 used are characterized by the properties as illustrated in Table 3. Blends A-1 and A-2 are obtained from consumer waste feedstock.
[0368] Recyclate Blend A-3 used as a comparative example is characterized by the properties as illustrated in Table 3. Blend A-3 is obtained from packaging waste for example from Systec Plastics GmbH (Germany).
[0369] Table 3 refers to a polyolefin composition comprising a) (CE1 ) heterophasic polypropylene copolymer (HECO-1 ) b) (CE2) heterophasic polypropylene copolymer (HECO-2) c) (CE3) Blend A-3 of recyclate material, d) (CE4) Blend A-1 of recyclate material, e) (CE5) Blend A-2 of recyclate material, f) (CE6) heterophasic polypropylene copolymer (HECO-1 ), Blend A-3 and additives (AS1 , AO1 , AO2, AO3); g) (IE1 ) heterophasic polypropylene copolymer (HECO-1 ), Blend A-1 and additives (AS1 , AO1 , AO2, AO3), h) (IE2) heterophasic polypropylene copolymer (HECO-2), Blend A-2 and additives (AS1 , AO1 , AO2, AO3),
[0370] I) (IE3) heterophasic polypropylene copolymer (HECO-2), Blend A-2 and additives (AS1 , AO1 , AO2, AO3), j) (IE4) heterophasic polypropylene copolymer (HECO-1), heterophasic polypropylene copolymer (HECO-2), Blend A-2 and additives (AS1 , AO1 , AO2, AO3), k) (IE5) heterophasic polypropylene copolymer (HECO-1), heterophasic polypropylene copolymer (HECO-2), Blend A-2 and additives (AS1 , AO1 , AO2, AO3), As can be seen in Table 3, in comparison to CE6, IE1 has higher ring stiffness, similar impact resistance, and longer failure time in pipe pressure testing than CE6. It also has smoother pipe inner surface than CE6 ( not shown). IE2-IE5 show a high pipe impact resistance.
[0371] The rPP used for IE1 and IE2-IE5, i.e. Blend A-1 (CE4) and Blend A-2 (CE5), has lower MFR2, lower gel content, and lower Crystex SF content than Blend A-3 (CE3) used for CE6. In addition, it does not have a peak / shoulder on the DMTA curve of tan6 vs temperature between -65 and -50°C (not shown).
[0372] ble 3
[0373]
[0374] .: not determinable i.e. lower than limit of detection and / or lower than limit of quantification;
Claims
Claims1 . Polyolefin composition comprising a) 40 to 90 wt% (based on the overall weight of the polyolefin composition) of at least one heterophasic propylene copolymer (HECO) having a total ethylene (C2) content (as determined according to Crystex analysis described in the method section) in the range from 0.5 to 6.0 wt.-% (based on the total weight of the heterophasic propylene copolymer), a soluble fraction (SF) determined according to Crystex analysis described in the method section in the range from 2.0 to 15.0 wt% (based on the total weight of the heterophasic propylene copolymer), and a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C, ) in the range of from 0.1 to 1 .0 g / 10 min; b) 10 to 60 wt% (based on the overall weight of the polyolefin composition) of a mixed-plastics polypropylene blend of recycled material ( Blend A) having a soluble fraction (SF) determined according to Crystex analysis as described in the method section in the range from 2.0 to 8.0 wt% (based on the total weight of the mixed-plastic polypropylene blend of recycled material) a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C, ) in the range from 1 .0 to 15.0 g / 10 min, and one or more, preferably all, of the following properties determined with camera detection from Optical Control Systems (OCS): an OCS gel index (determined as described in the method section) of less than 65000,OCS others (> 1000 pm, determined as described in the method section) of less than 1500 1 / m2,OCS contaminations (>1000 pm, determined as described in the method section) of less than 85 1 / m2, and / orOCS gel (>1000 pm, determined as described in the method section) of less than 300 1 / m2;c) optionally further additives (based on the overall weight of the polyolefin composition), wherein the sum of all ingredients always adds up to 100 wt%.
2. Polyolefin composition according to claim 1 , which comprises a) in the range of from 42 to 87 wt%, preferably from 45 to 85 wt%, more preferably from 47 to 80 wt%, even more preferably from 65 to 77 wt.-%, still more preferably from 68 to 76 wt% (based on the overall weight of the polyolefin composition) of at least one heterophasic propylene copolymer (HECO) with a total ethylene (C2) content (as determined according to Crystex analysis as described in the method section) in the range from 0.5 to 6.0 wt.-% (based on the total weight of the heterophasic propylene copolymer), soluble fraction (SF) (determined according to Crystex analysis as described in the method section) in the range from 2.0 to 15.0 wt% (based on the total weight of the heterophasic propylene copolymer), and a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C) in the range from 0.1 to 1 g / 10 min; b) in the range from 13 to 58 wt%, preferably from 15 to 55 wt%, more preferably from 20 to 53 wt%, even more preferably from 23 to 35 wt%, still more preferably from 24 to 32 wt% (based on the overall weight of the polyolefin composition) of a mixed- plastics polypropylene blend of recycled material (Blend A) having a soluble fraction (SF) determined according to Crystex analysis described in the method section in the range from 2.0 to 8.0 wt%, (based on the total weight of the mixed-plastic polypropylene blend of recycled material), a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C) in the range from 1 .0 to 15 g / 10 min, and one or more, preferably all of the following properties: an OCS gel index (determined as described in the method section) of less than 65000, OCS others (> 1000 pm, determined as described in the method section) of less than 1500 1 / m2, OCS contaminations (>1000 pm, determined as described in the method section) of less than 85 1 / m2, and / or OCS gel (>1000 pm, determined as described in the method section) of less than 300 1 / m2, and c) optionally further additives (based on the overall weight of the polyolefin composition), wherein the sum of all ingredients always adds up to 100 wt%.
3. Polyolefin composition according to one of the preceding claims, having a ring stiffness (determined as described in the method section) of at least 7.0 kN / m2, preferably of atleast 7.5 kN / m2, more preferably of at least 8.0 kN / m2, even more preferably of at least 9.2 kN / m2, still more preferably of at least 9.5 kN / m2, as in the range from 7.0 kN / m2to 20.0 kN / m2, preferably in the range from 7.5 kN / m2to 15.0 kN / m2, more preferably in the range from 8.0 kN / m2to 12.0 kN / m2.
4. Polyolefin composition according to one of the preceding claims, having a failure time in pipe internal pressures testing (at +95°C, 2.5 MPa, determined as described in the method section) of at least 1800 hours, preferably at least 1900 hours, more preferably of at least 2000 hours, such as in the range from 1800 hours to 6000 hours, preferably in the range from 1900 hours to 5000 hours, more preferably in the range from 2000 hours to 4000 hours.
5. Polyolefin composition according to one of the preceding claims, having an impact strength (ISO179-1 , Charpy notched 1 eA -20°C, measured as described in the method section) of at least 1 .0 kJ / m2, preferably of at least 1 .3 kJ / m2, still more preferably of at least 1.5 kJ / m2, in particular in a range from 1.0 to 15.0 kJ / m2, more particular in a range from 1 .3 to 10.0 kJ / m2, even more particular in a range from 1 .5 to 5.0 kJ / m2.
6. Polyolefin composition according to one of the preceding claims having one or more, preferably all of the following properties: an OCS gel index (determined as described in the method section) of less than 2.000, preferably of less than 1800, more preferably of less than 1500, even more preferably of less than 1200, still more preferably of less than 1000, an OCS others (> 1000 pm, determined as described in the method section) of less than 10.0 1 / m2, preferably of less than 8.0 1 / m2, more preferably of less than 5.0 1 / m2, even more preferably of less than 2.0 1 / m2, an OCS contaminations (>1000 pm, determined as described in the method section) of less than 3.5 1 / m2, preferably of less than 3.0 1 / m2, more preferably of less than 2.5 1 / m2, even more preferably of less than 2.0 1 / m2, still more preferably of less than 1.0 1 / m2’, and / oran OCS gel (>1000 pm, determined as described in the method section) of less than 15.0 1 / m2, preferably of less than 10.0 1 / m2, more preferably of less than 5.0 1 / m2, even more preferably of less than 2.0 1 / m2’ still more preferably of less than 1 .0 1 / m2.
7. Polyolefin composition according to any one of the preceding claims, wherein the at least one heterophasic propylene copolymer (HECO) has a total ethylene (C2) content in the range of 0.5 to less than 5.5 wt.-%, preferably from 0.8 to 5.3 wt%, more preferably from 1 .0 to 5.2 wt%, even more preferably from 1 .0 to less than 4.5 wt.-%, preferably from 1 .0 to 4.3 wt%, more preferably from 1 .3 to 4.2 wt% (based on the total weight of the heterophasic propylene copolymer),8. Polyolefin composition according to any one of the preceding claims, wherein the at least one heterophasic propylene copolymer (HECO) has a melt flow rate MFR2(measured according to ISO 1133, 2.16 kg, 230°C) in the range from 0.1 to 0.9 g / 10 min, preferably from 0.13 to 0.7 g / 10min, more preferably from 0.15 to 0.5 g / 10min.
9. Polyolefin composition according to any one of the preceding claims, wherein the at least one heterophasic propylene copolymer (HECO-1) has in the Crystex analysis one or more, preferably all of the following properties:- a total ethylene (C2) content from 0.5 to less than 4.0 wt.-%, preferably from 1 .0 to 3.5 wt%, more preferably from 1 .2 to 3.0 wt%, such as from 1 .2 to 2.5 wt% (based on the total weight of the heterophasic propylene copolymer), and / or- an intrinsic viscosity (IV) in the range from 1.0 to 6.0 dl / g, preferably in the range from 2.0 to 5.5 dl / g, more preferably in the range from 3.0 to 5.0 dl / g, and / or- a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF)) in the range from 0.3 to 3.0 wt.-% (based on the total weight of the crystalline fraction), preferably from 0.4 to 2.0 wt%, more preferably from 0.5 to 1 .5 wt%. an intrinsic viscosity (IV(CF)) in the range from 2.0 to 6.0 dl / g, preferably in the range from 2.5 to 5.5 dl / g, more preferably in the range from 3.0 to 5.0 dl / g, and / or- a soluble fraction (SF) content in the range of 2.5 to 9.5 wt%, preferably in the range of 3.0 to 8.5 wt%, more preferably in the range of 3.5 to 7.5 wt% (based on the total weight of the heterophasic propylene copolymer)- the soluble fraction (SF) having one or more, preferably all of the following properties: an ethylene content (C2(SF)) in the range from 15.0 to 35.0 wt.-% (based on the total weight of the soluble fraction), preferably from 18.0 to 30.0 wt%, more preferably from 20.0 to 25.0 wt%. an intrinsic viscosity (IV(SF)) in the range from 1 .0 to 6.0 dl / g, preferably in the range from 1 .5 to 5.0 dl / g, more preferably in the range from 2.0 to 4.0 dl / g.
10. Polyolefin composition according to any one of the claims 1 -8, wherein the at least one heterophasic propylene copolymer (HECO-2) has in the Crystex analysis one or more, preferably all of the following properties:- a total ethylene (C2) content from 1 .5 to less than 5.5 wt.-%, preferably from 2.0 to 5.2 wt%, more preferably from 2.5 to 5.0 wt%, such as from 3.0 to 4.8 wt% (based on the total weight of the heterophasic propylene copolymer), and / or- an intrinsic viscosity (IV) in the range from 1.0 to 6.0 dl / g, preferably in the range from 2.0 to 5.5 dl / g, more preferably in the range from 3.0 to 5.0 dl / g, and / or- a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF)) in the range from 0.5 to 5.0 wt.-% (based on the total weight of the crystalline fraction), preferably from 1 .0 to 3.0 wt%, more preferably from 1 .2 to 2.0 wt%. an intrinsic viscosity (IV(CF)) in the range from 2.0 to 6.0 dl / g, preferably in the range from 2.5 to 5.5 dl / g, more preferably in the range from 3.0 to 5.0 dl / g, and / or- a soluble fraction (SF) content in the range of 4.0 to 14.5 wt%, preferably in the range of 5.0 to 13.0 wt%, more preferably in the range of 6.0 to 11 .5 wt% (based on the total weight of the heterophasic propylene copolymer);- the soluble fraction (SF) having one or more, preferably all of the following properties: an ethylene content (C2(SF)) in the range from 20.0 to 40.0 wt.-% (based on the total weight of the soluble fraction), preferably from 25.0 to 35.0 wt%, more preferably from 30.0 to 33.0 wt%, an intrinsic viscosity (IV(SF)) in the range from 1 .0 to 6.0 dl / g, preferably in the range from 1 .5 to 5.0 dl / g, more preferably in the range from 2.0 to 4.0 dl / g.11 . Polyolefin composition according to one of the preceding claims, wherein the mixed- plastics polypropylene blend of recycled material (Blend A) comprises iPP content in the range of from 75 to 99 wt%, preferably from 80 to 98 wt%. more preferably from 85 to 95 wt% (based on the total weight of the mixed-plastics polypropylene blend of recycled material), determined according to IR method as described in the method section, which is recovered from a waste plastic material derived from post-consumer and / or post-industrial waste, preferably from post-consumer waste .
12. Polyolefin composition according to one of the preceding claims, wherein the mixed- plastics polypropylene blend of recycled material (Blend A) has a soluble fraction (SF) determined according to Crystex analysis as described in the method section in the range from 2.0 to 7.5 wt%, preferably in a range from 2.5 to 7.0 wt%, more preferably in a range from 3.0 to 7.0 wt%, even more preferably in a range from 3.3 to 6.8 wt%, such as from 3.5 to 6.5 wt% (based on the total weight of the mixed-plastic polypropylene blend of recycled material)13. Polyolefin composition according to one of the preceding claims, wherein the mixed- plastics polypropylene blend of recycled material (Blend A) has one or more, preferably all of the following properties:- DMTA (torsional)_E' +23°C (determined as described in the method section) of at least 680 MPa, preferably of at least 700 MPa, more preferably of at least 730 MPa,- DMTA (torsional)_E' +60°C (determined as described in the method section) of at least 350 MPa, preferably of at least 370 MPa, more preferably of at least 400 MPa,- DMTA (torsional)_E' +90°C (determined as described in the method section) of at least 200 MPa, preferably of at least 230 MPa, more preferably of at least 250 MPa,- DMTA (torsional)_E' -30°C (MPa) (determined as described in the method section) of at least 1600 MPa, preferably of at least 1700 MPa, more preferably of at least 1800 MPa, and / or- DMTA (torsional)_E' 0°C (MPa) (determined as described in the method section) of at least 1000 MPa, preferably of at least 1100 MPa, more preferably of at least 1200 MPa.
14. Polyolefin composition according to one of the preceding claims, wherein the mixed- plastics polypropylene blend of recycled material (Blend A) has a melt flow rate (ISO1133, 2.16kg; 230°C) in the range from 1 .0 to 12.0 g / 10 min, preferably from 1 .0 to 9.0 g / 10 min, preferably from 1.5 to 8.0 g / 10 min, more preferably from 2.0 to 7.0 g / 10min, even more preferably from 3.0 to 6.5 g / 10min, still more preferably from 4.0 to 6.4 g / 10min.
15. Polyolefin composition according to one of the preceding claims, wherein the mixed- plastics polypropylene blend of recycled material (Blend A) has one or more, preferably all of the following properties: an OCS gel index (determined as described in the method section)) of less than 50,000, preferably of less than 30,000, more preferably of less than 10,000, even more preferably of less than 5,000, an OCS others (> 1000 pm, determined as described in the method section) of less than 1000 1 / m2, preferably of less than 500 1 / m2, more preferably of less than 100 1 / m2, even more preferably of less than 50 1 / m2, an OCS contaminations (>1000 pm, determined as described in the method section) of less than 80 1 / m2, preferably of less than 75 1 / m2, more preferably of less than 70 1 / m2, even more preferably of less than 65 1 / m2, still more preferably of less than 60 1 / m2, and / or an OCS gel (> 1000 pm, determined as described in the method section) of less than 200 1 / m2, preferably of less than 100 1 / m2, more preferably of less than 50 1 / m2, even more preferably of less than 40 1 / m2.
16. Polyolefin composition according to one of the preceding claims, wherein the mixed- plastics polypropylene blend of recycled material (Blend A-1 ) has in the CRYSTEX analysis one or more, preferably all of the following properties:- a total ethylene (C2) content in the range from 1 .0 to 20.0 wt.-%, preferably from 2.0 to 15.0 wt%, more preferably from 5.0 to 13.0 wt%, even more preferably from 9.0 to 12.0 wt%, even preferably from 9.0 to 11.5 wt% (based on the total weight of the mixed-plastic polypropylene blend of recycled material), and / or- an intrinsic viscosity (IV) in the range from 1 .0 to 3.0 dl / g, preferably in the range from 1 .2 to 2.7 dl / g, more preferably in the range from 1 .5 to 2.5 dl / g; even more preferably in the range from 1 .7 to 2.2 dl / g; and / or- a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF) in the range from 1 .0 to 20.0 wt.-%, preferably from 2.0 to 15.0 wt%, more preferably from 5.0 to 13.0 wt%, even more preferably from 6.0 to 12.0 wt %; even preferably from 9.0 to 11 .5 wt% based on the total weight of the crystalline fraction); an intrinsic viscosity (IV(CF)), in the range from 1.0 to 3.0 dl / g, preferably in the range from 1 .2 to 2.7 dl / g, more preferably in the range from 1 .5 to 2.5 dl / g; even more preferably in the range from 1 .7 to 2.2 dl / g; and / or- a soluble fraction (SF) determined according to Crystex analysis as described in the method section in the range from 2.0 to 7.0 wt%, preferably in a range from 2.5 to 6.5 wt%, more preferably in a range from 3.0 to 6.0 wt%, even more preferably in a range from 3.5 to 5.5 wt%, such as from 4.0 to 5.0 wt%.(based on the total weight of the mixed-plastic polypropylene blend of recycled material)- the soluble fraction (SF) having one or more, preferably all of the following properties, if determinable: an ethylene content (C2(SF)) in the range from 0.1 to 25.0 wt.-% (based on the total weight of the soluble fraction), preferably from 4.0 to 20.0 wt%, more preferably from 5.0 to 18.0 wt%. an intrinsic viscosity (IV(SF)) in the range from 0.2 to 3.0 dl / g, preferably in the range from 0.3 to 2.5 dl / g, more preferably in the range from 0.4 to 2.0 dl / g.
17. Polyolefin composition according to one of the claims 1 -15, wherein the mixed-plastics polypropylene blend of recycled material (Blend A-2) has in the CRYSTEX analysis one or more, preferably all of the following properties:- a total ethylene (C2) content in the range from 1 .0 to 15.0 wt.-%, preferably from 2.0 to 12.0 wt%, more preferably from 2.5 to 10.0 wt%, even more preferably from 3.0 to 8.0 wt%, even preferably from 4.0 to 7.0 wt% (based on the total weight of the mixed-plastic polypropylene blend of recycled material), and / or- an intrinsic viscosity (IV) in the range from 1 .0 to 3.0 dl / g, preferably in the range from 1 .2 to 2.7 dl / g, more preferably in the range from 1 .5 to 2.5 dl / g; even more preferably in the range from 1 .5 to 2.0 dl / g; and / or- a crystalline fraction (CF) having one or more, preferably all of the following properties: an ethylene content (C2(CF) in the range from 1.0 to 15.0 wt.-%, preferably from 2.0 to 12.0 wt%, more preferably from 2.5 to 10.0 wt%, even more preferably from 3.0 to 8.0 wt %; even preferably from 4.0 to 7.0 wt% based on the total weight of the crystalline fraction); an intrinsic viscosity (IV(CF)), in the range from 1.0 to 3.0 dl / g, preferably in the range from 1 .2 to 2.7 dl / g, more preferably in the range from 1 .5 to 2.5 dl / g; even more preferably in the range from 1 .5 to 2.0 dl / g; and / or- a soluble fraction (SF) determined according to Crystex analysis as described in the method section in the range from 2.0 to 7.0 wt%, preferably in a range from 2.5 to 6.5 wt%, more preferably in a range from 3.0 to 6.0 wt%, even more preferably in a range from 3.5 to 5.5 wt%, such as from 4.0 to 5.0 wt%.(based on the total weight of the mixed-plastic polypropylene blend of recycled material)- the soluble fraction (SF) having one or more, preferably all of the following properties, if determinable: an ethylene content (C2(SF)) in the range from 0.1 to 20.0 wt.-% (based on the total weight of the soluble fraction), preferably from 1 .0 to 15.0 wt%, more preferably from 1 .5 to 5.0 wt%, even more preferably from 2.0 to 5.0 wt%. an intrinsic viscosity (IV(SF)) in the range from 0.2 to 3.0 dl / g, preferably in the range from 0.3 to 2.7 dl / g, more preferably in the range from 0.5 to 2.5 dl / g.
18. Polyolefin composition according to one of the preceding claims, wherein the polyolefin composition (PC-1 ) comprises a) in the range from 47 to 80 wt%, preferably from 65 to 77 wt.-%, more preferably from 68 to 76 wt% (based on the overall weight of the polyolefin composition) of at the least one heterophasic propylene copolymer HECO-1 ;b) in the range 20 to 53 wt%, even more preferably from 23 to 35 wt%, still more preferably from 24 to 32 wt% (based on the overall weight of the polyolefin composition) of a mixed-plastics polypropylene blend of recycled material Blend A-1 , c) optionally further additives (based on the overall weight of the polyolefin composition), wherein the sum of all ingredients always adds up to 100 wt%.
19. Polyolefin composition according to one of the preceding claims, wherein the polyolefin composition (PC-2) comprises a) in the range of from 40 to 90 wt%, preferably from 42 to 87 wt%, in particular preferably from 45 to 85 wt%, more preferably from 47 to 80 wt%, even more preferably from 49 to 76 wt.-%, (based on the overall weight of the polyolefin composition) of the at least one heterophasic propylene copolymer HECO-2; b) in the range from 10 to 60 wt%, preferably from 13 to 58 wt%, in particular preferably from 15 to 55 wt%, more preferably from 20 to 53 wt%, even more preferably from 24 to 51 wt% (based on the overall weight of the polyolefin composition) of a mixed-plastics polypropylene blend of recycled material Blend A-2, c) optionally further additives (based on the overall weight of the polyolefin composition), wherein the sum of all ingredients always adds up to 100 wt%.
20. Polyolefin composition according to one of the preceding claims, wherein the polyolefin composition (PC-3) comprises a) in the range of from 47 to 80 wt%, preferably from 65 to 77 wt.-%, more preferably from 68 to 76 wt% (based on the overall weight of the polyolefin composition) of a mixture of the at least one heterophasic propylene copolymer HECO-1 and the least one heterophasic propylene copolymer HECO-2; b) in the range from 20 to 53 wt%, even more preferably from 23 to 35 wt%, still more preferably from 24 to 32 wt% (based on the overall weight of the polyolefin composition) of a mixed-plastics polypropylene blend of recycled material Blend A-2, c) optionally further additives (based on the overall weight of the polyolefin composition), wherein the sum of all ingredients always adds up to 100 wt%.21 . A process for preparing the polyolefin composition according to one of the preceding claims, comprising the steps of- providing the at least one heterophasic propylene copolymer and the mixed- plastics polypropylene blend of recycled material,- feeding / dosing the at least one heterophasic propylene copolymer and the mixed-plastics polypropylene blend of recycled material separately or as a mixture into at least one extruder,- melting the mixture in the at least one extruder thereby providing the polyolefin composition, and- optionally pelletizing the provided polyolefin composition.
22. Use of the polyolefin composition according to one of the claims 1 -20, for manufacturing fittings and pipes, in particular pipes.
23. An article comprising the polyolefin composition according to one of the claims 1-20, in particular a pipe.