Heterophasic propylene ethylene copolymer composition with excellent optical and sealing properties

Abstract

Heterophasic ethylene propylene copolymer composition with excellent optical and sealing properties. Heterophasic ethylene propylene copolymer composition having an mfr2 of 1.0 to 5.0 g / 10 min, a c2 content of 0.8 to 6.0 mol% and a tm of 153.0 to 159.0 °C, comprising: a) a crystalline matrix (m) which is a propylene homopolymer or copolymer, preferably a homopolymer; and b) an amorphous ethylene propylene elastomer (e); wherein the heterophasic ethylene propylene copolymer composition is characterized with respect to the soluble fraction (sf) and crystalline fraction (cf), as determined by crystex qc analysis: i) 85.0 to 90.0% by weight of a crystalline fraction (cf) having an iv(cf) of 2.00 to 3.00 dl / g, a c2(cf) of 0.0 to 1.5% by mol; and ii) 10.0 to 15.0% by weight of a soluble fraction (sf) having an iv(sf) of 1.30 to 2.50 dl / g and a c2(sf) of 25.0 to 40.0% by mol.

Description

1 / 36 “HETEROPHASIC ETHYLENE PROPYLENE COPOLYMER COMPOSITION WITH EXCELLENT OPTICAL AND SEALING PROPERTIES” Field of Invention

[0001] The present invention relates to a heterophasic ethylene propylene copolymer composition with excellent optical and sealing properties and to films produced therefrom. Background of the Invention

[0002] Heterophasic propylene copolymer films are used in a wide variety of areas, for example, food packaging, as packaging films and containers. These films are known for their well-balanced properties such as strength, stiffness, transparency and impact resistance, among others. Metallized films are also used as packaging material, for example, in the form of a layered polypropylene film / aluminum foil structure.

[0003] Although these films have demonstrated well-balanced properties, optimizing the balance of mechanical, optical, and sealing properties remains a refined technique, requiring compromises in some properties to achieve improvements in others.

[0004] To obtain a good balance of mechanical properties, Ziegler-Natta catalyzed polypropylene-based compositions are frequently used; however, these compositions can often have less ideal sealing and optical properties, especially after steam sterilization. Petition 870230108362, dated 08 / 12 / 2023, page 9 / 137 2 / 36

[0005] Document WO 2018 / 077663 A1 describes heterophasic polypropylene compositions that possess optimized optical and mechanical properties, as well as a low amount of extractables. These compositions can be obtained through the use of Ziegler-Natta catalysis. The heterophasic polypropylene compositions are processed into films, which are considered useful for food packaging applications.

[0006] WO 2020 / 011825 A1 describes a metallocene-based heterophasic polypropylene composition that has high stiffness, high toughness, and high transparency, wherein the beneficial properties are obtained by blending metallocene-based heterophasic polypropylene with a smaller amount of Ziegler-Natta-based heterophasic polypropylene. The metallocene-based heterophasic polypropylene copolymer component in the composition has relatively low ethylene content and soluble fraction content.

[0007] Despite developments in this field, there remains a need to provide a simple heterophasic polypropylene composition that has enhanced optical and sealing properties without sacrificing mechanical performance, particularly for materials that are easy to produce and process, in particular those that do not require extra processing steps or additional polymeric components to achieve the desired properties. Summary of the Invention

[0008] The present invention is based on the finding that a heterophasic ethylene propylene copolymer composition has specific properties, including Petition 870230108362, dated 08 / 12 / 2023, page 10 / 137 3 / 36 melting temperature and crystalline / soluble fraction content according to CRYSTEX QC analysis and the individual properties of each fraction, has enhanced sealing and optical properties both before and after steam sterilization.

[0009] The present invention is directed to a heterophasic ethylene propylene copolymer (HECO) composition having a melt flow rate (MFR2) measured according to ISO 1133 at 230 °C and 2.16 kg in the range of 1.0 to 5.0 g / 10 min, a total ethylene C(C2) content, as determined by quantitative IR spectroscopy, in the range of 0.8 to 6.0 mol%, and a melting temperature (Tm) measured by differential scanning calorimetry (DSC) in the range of 153.0 to 159.0 °C, comprising: a) a crystalline matrix (M) that is a propylene homopolymer or copolymer, preferably a homopolymer; and b) an amorphous propylene-ethylene elastomer (E); where the heterophasic ethylene propylene copolymer composition is characterized with respect to its soluble fraction (SF) and crystalline fraction (CF), as determined by CRYSTEX QC analysis: i) 85.0 to 90.0% by weight, based on the total weight of the heterophasic ethylene propylene copolymer composition, of a crystalline fraction (CF) having an intrinsic viscosity iV(CF) measured according to DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C) in the range of 2.00 to 3.00 dl / g, an ethylene C2(CF) content, as determined by quantitative IR spectroscopy, in the range of 0.0 to 1.5 mol%; and ii) 10.0 to 15.0% by weight, based on the total weight of the Petition 870230108362, dated 08 / 12 / 2023, page 11 / 137 4 / 36 composition of heterophasic ethylene propylene copolymer, of a soluble fraction (SF) having an intrinsic viscosity iV(SF) measured according to DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C) in the range of 1.30 to 2.50 dl / g and an ethylene content C2(SF), as determined by quantitative IR spectroscopy, in the range of 25.0 to 40.0 mol%.

[0010] In another aspect, the present invention is directed to a film, preferably a cast film, comprising at least 90% by weight of the inventive heterophasic ethylene propylene copolymer (HECO) composition. Definitions

[0011] A heterophasic polypropylene copolymer is a propylene-based copolymer with a crystalline matrix phase, which may be a propylene homopolymer or a random copolymer of propylene and at least one alpha-olefin comonomer, and an elastomeric phase dispersed therein. In the case of a random heterophasic propylene copolymer, said crystalline matrix phase is a random copolymer of propylene and at least one alpha-olefin comonomer. The polymers according to the present invention have this morphology.

[0012] The elastomeric phase can be a propylene copolymer with a high comonomer content that is not randomly distributed in the polymer chain, but is distributed in a comonomer-rich block structure and a propylene-rich block structure. A heterophasic polypropylene copolymer usually differs from a monophasic propylene copolymer by having two distinct glass transition temperatures Tg which are Petition 870230108362, dated 08 / 12 / 2023, page 12 / 137 5 / 36 attributed to the matrix phase and the elastomeric phase.

[0013] A propylene homopolymer is a polymer consisting essentially of propylene monomer units. Due to impurities, especially during commercial polymerization processes, a propylene homopolymer may comprise up to 0.1 mol% of comonomer units, preferably up to 0.05 mol% of comonomer units, and most preferably up to 0.01 mol% of comonomer units. A propylene random copolymer is a copolymer of propylene monomer and comonomer units, preferably selected from ethylene and C4-C12 alpha-olefins, in which the comonomer units are randomly distributed in the polymer chain. The propylene random copolymer may comprise comonomer units of one or more comonomers differing in their carbon atom quantities. The quantities below are given as a percentage by weight (% by wt), unless otherwise stated. Detailed Description of the Invention The heterophasic ethylene propylene copolymer (HECO) composition

[0014] In a heterophasic propylene copolymer, the matrix and elastomeric phases cannot be separated and measured, since the elastomeric phase is dispersed within the crystalline matrix. In order to characterize the matrix and elastomeric phases of a heterophasic propylene copolymer, several methods are known. One method consists of xylene extraction of a fraction that contains mostly the elastomeric phase, thus separating a cold-soluble xylene fraction (XCS) from a fraction of Petition 870230108362, dated 08 / 12 / 2023, page 13 / 137 6 / 36 cold insoluble in xylene (XCI). The XCS fraction contains mostly the elastomeric phase and only a small part of the matrix phase, while the XCI fraction contains mostly the matrix phase and only a small part of the elastomeric phase.

[0015] As an alternative method, the separation of a crystalline fraction and a soluble fraction using the CRYSTEX QC method with trichlorobenzene (TCB) as solvent. This method is described below in the determination methods section. The crystalline fraction (CF) contains mostly the matrix phase and only a small part of the elastomeric phase, and the soluble fraction (SF) contains mostly the elastomeric phase and only a small part of the matrix phase. In some cases, this method results in more useful data, since the crystalline fraction (CF) and the soluble fraction (SF) correspond more accurately to the matrix and elastomeric phases, respectively. Due to the differences in the xylene extraction and CRYSTEX QC separation methods, the properties of the XCS / XCI fractions, on the one hand, and the crystalline / soluble fractions (CF / SF), on the other, are not exactly the same, meaning that the amounts of the matrix phase and the elastomeric phase may differ, as well as their properties. Crystalline fraction from CRYSTEX QC measurement

[0016] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention has a crystalline fraction (CF) content within the range of 85.0 to 90.0% by weight, more preferably 86.0 to 89.0% by weight, based on the total weight of the heterophasic ethylene propylene copolymer composition. Petition 870230108362, dated 08 / 12 / 2023, page 14 / 137 7 / 36

[0017] The crystalline fraction (CF) of the heterophasic ethylene propylene copolymer (HECO) composition of the present invention has an intrinsic viscosity iV(CF) measured in accordance with DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C) in the range of 2.00 to 3.00 dl / g, more preferably in the range of 2.20 to 2.80 dl / g, with maximum preference in the range of 2.30 to 2.60 dl / g.

[0018] The crystalline fraction (CF) of the heterophasic ethylene propylene copolymer (HECO) composition of the present invention has an ethylene C2(CF) content, as determined by quantitative IR spectroscopy, in the range of 0.0 to 1.5 mol%, more preferably in the range of 0.0 to 1.0 mol%, most preferably in the range of 0.0 to 0.5 mol%. Soluble fraction of the CRYSTEX QC measurement

[0019] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention has a soluble fraction (SF) content within the range of 10.0 to 15.0% by weight, more preferably 11.0 to 14.0% by weight, based on the total weight of the heterophasic ethylene propylene copolymer composition.

[0020] The soluble fraction (SF) of the heterophasic ethylene propylene copolymer (HECO) composition of the present invention has an intrinsic viscosity iV(SF) measured in accordance with DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C) in the range of 1.30 to 2.50 dl / g, more preferably in the range of 1.50 to 2.40 dl / g, with maximum preference in the range of 1.80 to 2.30 dl / g.

[0021] The soluble fraction (SF) of the heterophasic ethylene propylene copolymer (HECO) composition of the present Petition 870230108362, dated 08 / 12 / 2023, p. 15 / 137 8 / 36 The invention has an ethylene C2(SF) content, as determined by quantitative IR spectroscopy, in the range of 25.0 to 40.0 mol%, more preferably in the range of 25.0 to 36.0 mol%, with maximum preference in the range of 25.0 to 33.0 mol%.

[0022] According to the present invention, the ratio of the intrinsic viscosities of the two fractions, iV(SF) / iV(CF), is preferably in the range of 0.50 to 1.00, more preferably in the range of 0.65 to 0.95, with maximum preference in the range of 0.75 to 0.90.

[0023] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention has a melt flow rate (MFR2) measured in accordance with ISO 1133 at 230 °C and 2.16 kg in the range of 1.0 to 5.0 g / 10 min, more preferably from 1.5 to 4.0 g / 10 min, with maximum preference in the range of 1.5 to 3.0 g / 10 min.

[0024] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention has an ethylene C(C2) content, as determined by quantitative IR spectroscopy, preferably in the range of 0.8 to 6.0 mol%, more preferably in the range of 1.0 to 4.0 mol%, most preferably in the range of 1.5 to 3.0 mol%.

[0025] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention preferably has an intrinsic viscosity (iV) measured in accordance with DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C) in the range of 2.00 to 3.00 dl / g, more preferably from 2.10 to 2.70 dl / g, with maximum preference in the range of 2.20 to 2.50 dl / g.

[0026] The crystalline matrix component (M) of Petition 870230108362, dated 08 / 12 / 2023, p. 16 / 137 9 / 36 heterophasic ethylene propylene copolymer (HECO) composition preferably has a melt flow rate (MFR2), measured in accordance with ISO 1133 at 230 °C and 2.16 kg in the range of 1.0 to 100 g / 10 min, more preferably 1.0 to 10.0 g / 10 min, even more preferably 1.5 to 6.0 g / 10 min, with a maximum preference of 2.0 to 4.0 g / 10 min.

[0027] It is preferred that the crystalline matrix component (M) of the heterophasic ethylene propylene copolymer (HECO) composition of the present invention be a propylene homopolymer.

[0028] When the crystalline matrix component (M) of the heterophasic ethylene propylene copolymer (HECO) composition is a propylene homopolymer, it preferably has an isotactic pentad concentration [mmmm] as determined by 13C-NMR spectroscopy greater than 97.0% and a 2.1 regiodefect content in the range of 0.1 to 1.4 mol%. These values ​​are indicative of heterophasic ethylene propylene copolymers that were produced in the presence of a single-site catalyst.

[0029] In many similar heterophasic propylene copolymers, it is necessary to adjust the rheological and mechanical properties of the final composition by treating the crude heterophasic propylene copolymer with a radical initiator, often in the extrusion step. This process may be known as viscoreduction. The properties of the heterophasic ethylene propylene copolymer (HECO) composition of the present invention are suitably desirable and therefore no viscoreduction (or similar treatment) is required to obtain superior properties. It is therefore preferable that the propylene copolymer composition Petition 870230108362, dated 08 / 12 / 2023, page 17 / 137 10 / 36 heterophasic ethylene (HECO) is free of radical initiators and their decomposition products, more preferably the heterophasic ethylene propylene copolymer (HECO) composition has not been viscoreduced.

[0030] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention preferably has a glass transition temperature associated with the amorphous propylene-ethylene elastomer (Tg(E)), measured in accordance with ISO 6721-7, in the range of -50 to -40 °C, more preferably in the range of -48 to -41 °C, with maximum preference in the range of -46 to -42 °C.

[0031] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention preferably has a glass transition temperature associated with the crystalline matrix (Tg(M)), measured in accordance with ISO 67217, in the range of -5 to 5 °C, more preferably in the range of -3 to 2 °C, with a maximum preference in the range of -2 to 0 °C.

[0032] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention preferably has a melting temperature (Tm) measured by differential scanning calorimetry (DSC) in the range of 153.0 to 159.0 °C, more preferably in the range of 154.0 to 158.5 °C, most preferably in the range of 155.0 to 158.0 °C. These values ​​are indicative of heterophasic propylene ethylene copolymers that were produced in the presence of a single-site catalyst.

[0033] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention preferably has a crystallization temperature (Tc) measured by differential scanning calorimetry (DSC) in the range of Petition 870230108362, dated 08 / 12 / 2023, page 18 / 137 11 / 36 120.0 to 127.0 °C, more preferably in the range of 121.0 to 126.0 °C, more preferably in the range of 122.0 to 125.0 °C.

[0034] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention preferably has a flexural modulus measured in accordance with ISO 178 in the range of 1100 to 1500 MPa, more preferably in the range of 1200 to 1450 MPa, with maximum preference in the range of 1250 MPa to 1400 MPa.

[0035] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention preferably has a Notched Charpy Impact Resistance (NIS) measured in accordance with ISO 179-1 eA at 23 °C in the range of 25.0 to 100 kJ / m2, more preferably in the range of 30.0 to kJ / m2, with maximum preference in the range of 35.0 to 60 kJ / m2.

[0036] The heterophasic ethylene propylene copolymer (HECO) composition of the present invention preferably has a Notched Charpy Impact Resistance (NIS) measured in accordance with ISO 179-1 eA at -20 °C in the range of 1.0 to 20 kJ / m2, more preferably in the range of 1.4 to 10.0 kJ / m2, with maximum preference in the range of 1.8 to 6.0 kJ / m2.

[0037] In addition to the fractions discussed above, the heterophasic ethylene propylene copolymer composition of the present invention may comprise additives.

[0038] Preferably, the heterophasic ethylene propylene copolymer (HECO) composition comprises 0.01 to 5.0% by weight, more preferably 0.03 to 3.0% by weight, even more preferably 0.06 to 2.0% by weight, most preferably 0.08 to 1.0% by weight of additives, based on the weight of the ethylene propylene copolymer composition. Petition 870230108362, dated 08 / 12 / 2023, page 19 / 137 12 / 36 heterophasic (HECO).

[0039] These additives are commercially available and, for example, described in “Plastic Additives Handbook”, 6th edition, 2009 by Hans Zweifel (pages 1141 to 1190). Process for the polymerization of heterophasic propylene copolymer (HECO)

[0040] The heterophasic propylene copolymer (HECO) of the present invention can be polymerized by sequential polymerization in the presence of a single-site catalyst system, wherein (a) A first fraction of polypropylene consisting of a propylene homopolymer or a propylene random copolymer, preferably having a comonomer content of 0.0 to 1.5 mol%, is prepared in a bulk phase reactor in a first polymerization stage. b) optionally, transfer said first polypropylene fraction to the second polymerization stage, wherein a second polypropylene fraction consisting of a propylene homopolymer or a propylene-ethylene random copolymer, preferably having a comonomer content of 0.0 to 1.5 mol%, is prepared in a gas phase reactor (GPR1), c) transfer the first polypropylene fraction (a) or the mixture comprising said first and second polypropylene fractions together (b) to a second (optionally third) polymerization stage in which the amorphous propylene-ethylene elastomer having a comonomer content (C2 of SF) of 25.0 to 40.0 mol%, such as 25.0 to 36.0 mol%, or 25.0 to 33.0 mol% is prepared in a gas phase reactor, d) a mixture of the said two, optionally three Petition 870230108362, dated 08 / 12 / 2023, page 20 / 137 13 / 36 polymers, which optionally undergo a deactivation and purification step followed by compounding and pelleting.

[0041] In a preferred embodiment, the polymerization process is carried out in the presence of a single-site catalyst system, as presented in this document.

[0042] The heterophasic polypropylene composition of the present invention is typically and preferably made in a multi-stage process well known in the art. A multi-stage process is a gas-phase cycle process, as developed by Borealis A / S, Denmark (known as BORSTAR® technology) described, for example, in the patent literature, such as in document EP-A0887379 or in document WO 92 / 12182. An alternative multi-stage process is the Spheripol process from LyondellBasell, USA.

[0043] The invention preferably relates to the copolymerization of propylene, ethylene and optionally and additionally comonomers as defined above and below, in at least one, at least two, optionally three step processes so as to form the heterophasic polypropylene composition. Preferably, propylene and ethylene are the only monomers used.

[0044] Ideally, the invention process employs two, preferably three, main reactors: a first reactor operating in large quantities, a first gas-phase reactor, and optionally a second gas-phase reactor.

[0045] The process can also use a prepolymerization step, which takes place in a separate reactor before the Petition 870230108362, dated 08 / 12 / 2023, page 21 / 137 14 / 36 three main reactors.

[0046] The crystalline matrix may preferably be present in the range of 80 to 93% by weight, more preferably in the range of 81 to 90% by weight, most preferably in the range of 83 to 89% by weight, based on the total weight of the heterophasic polypropylene composition.

[0047] The elastomeric phase comprised in the heterophasic polypropylene composition and dispersed in the aforementioned matrix may preferably be present in the range of 7 to 20% by weight, more preferably in the range of 10 to 19% by weight, with maximum preference in the range of 11 to 17% by weight, based on the total weight of the heterophasic polypropylene composition.

[0048] The comonomer content, C(C2) (total), of the inventive polymer may be in the range of 0.8 to 6.0 mol%, more preferably in the range of 1.0 to 4.0 mol%, with maximum preference in the range of 1.5 to 3.0 mol%. Unimodal matrix

[0049] The crystalline matrix, which is a homo- or copolymer of propylene, is produced in a bulk stage, then transferred to the second stage where the amorphous ethylene propylene elastomer is produced in a first gas phase reactor (GPR1) in the presence of the first polypropylene fraction.

[0050] The comonomer content of the crystalline matrix may be in the range of 0.0 to 1.5 mol%, preferably in the range of 0.0 to 1.2 mol%, more preferably in the range of 0.0 to 1.0 mol%.

[0051] It is particularly preferred that the crystalline matrix (a) be a propylene homopolymer and comprise Petition 870230108362, dated 08 / 12 / 2023, page 22 / 137 15 / 36 0.0% by weight of comonomer.

[0052] The MFR of the crystalline matrix can be in the range of 1.0 to 10.0 g / 10 min, more preferably in the range of 1.5 to 6.0 g / 10 min, most preferably in the range of 2.0 to 4.0 g / 10 min. This applies regardless of the (bi)modality of the crystalline matrix. Bimodal matrix

[0053] In this case, the crystalline matrix is ​​bimodal, so the first polypropylene fraction is produced in a bulk stage, then transferred to the second stage where the second polypropylene fraction is prepared in a first gas phase reactor (GPR1) in the presence of the first polypropylene fraction. This mixture, which is the crystalline matrix and which comprises the said first and second polypropylene fractions together, is transferred to the third stage where the amorphous propylene-ethylene elastomer is prepared in a gas phase reactor (GPR2) in the presence of the crystalline matrix.

[0054] The MFR2 of the polymer produced in the first stage, which consists of the first polypropylene fraction, may be in the range of 1.0 to 10.0 g / 10 min, more preferably in the range of 1.5 to 6.0 g / 10 min, with maximum preference in the range of 2.0 to 4.0 g / 10 min.

[0055] The MFR2 of the polymer produced in the second stage, which consists of the second polypropylene fraction, may be in the range of 1.0 to 10.0 g / 10 min, more preferably in the range of 1.5 to 6.0 g / 10 min, with maximum preference in the range of 2.0 to 4.0 g / 10 min.

[0056] Since the second polypropylene fraction is produced in the presence of the first polypropylene fraction, Petition 870230108362, dated 08 / 12 / 2023, page 23 / 137 16 / 36 It is understood that its properties cannot be analyzed as such, but must be determined based on the properties of the first polypropylene fraction and the properties of the crystalline fraction.

[0057] In a preferred embodiment, the heterophasic polypropylene composition comprises a1) 40–60% by weight, preferably in the range of 42–57% by weight, more preferably in the range of 45–55% by weight of a first polypropylene fraction having an MFR2 of 1.0–10.0 g / 10 min, a2) 28–40% by weight, preferably in the range of 29–38% by weight, more preferably in the range of 30–36% by weight of a second polypropylene fraction having an MFR2 of 1.0–10.0 g / 10 min, b) 7 to 20% by weight of amorphous ethylene propylene elastomer, preferably in the range of 10 to 19% by weight, more preferably in the range of 11 to 17% by weight.

[0058] Preferably, the amount of the first polypropylene fraction is equal to or greater than the amount of the second polypropylene fraction based on the total weight of the crystalline matrix.

[0059] The amount of the first polypropylene fraction may be in the range of 50 to 75% by weight, preferably 55 to 70% by weight, more preferably in the range of 60 to 65% by weight based on the total weight of the crystalline matrix.

[0060] The amount of the second polypropylene fraction may be in the range of 25 to 50% by weight, preferably 30 to 45% by weight, more preferably in the range of 35 to 40% by weight based on the total weight of the crystalline matrix.

[0061] The ratio between the quantity of the first and the second Petition 870230108362, dated 08 / 12 / 2023, page 24 / 137 17 / 36 fractions of polypropylene may be in the range of 50:50 to 75:25, such as 55:45 to 70:30, preferably 60:40 to 65:35.

[0062] For large-scale gas-phase copolymerization reactions, the reaction temperature used is generally in the range of 60 to 115 °C (e.g., 70 to 110 °C), the reactor pressure will generally be in the range of 1 to 4 MPa (10 to 40 bar) for bulk polymerization gas-phase reactions operating at slightly higher pressures. The residence time will generally be 0.25 to 8 hours (e.g., 0.3 to 3 hours).

[0063] The comonomer content of the first and second polypropylene fractions may be the same or different and independently chosen from each other.

[0064] The comonomer content of the polymer produced in the first stage, that is, the first polypropylene fraction, may be in the range of 0.0 to 1.5 mol%, preferably in the range of 0.0 to 1.2 mol%, more preferably in the range of 0.0 to 1.0 mol%.

[0065] It is particularly preferred that the first polypropylene fraction be a propylene homopolymer and comprise 0.0% by weight of comonomer.

[0066] The comonomer content of the polymer produced in the second stage, that is, the second polypropylene fraction, may be in the range of 0.0 to 1.5 mol%, preferably in the range of 0.0 to 1.2 mol%, more preferably in the range of 0.0 to 1.0 mol%.

[0067] It is particularly preferred that the second polypropylene fraction be a propylene homopolymer and comprise 0.0% by weight of comonomer.

[0068] In this request, it is understood that the comonomer content Petition 870230108362, dated 08 / 12 / 2023, page 25 / 137 18 / 36 of the crystalline matrix, when available as a sample of different material, is determined by quantitative FT-IR spectroscopy calibrated by 13C NMR spectroscopy. When the comonomer content of the matrix and the dispersed fraction are to be evaluated from the final polymer (comprising both the matrix and the dispersed fraction), then the matrix (and its properties) is reflected by the crystalline fraction (CF) determined according to CRYSTEX QC analysis. Consequently, the dispersed amorphous ethylene propylene elastomer is reflected by the soluble fraction (SF) determined according to CRYSTEX QC analysis. Catalytic converter system

[0069] The heterophasic polypropylene composition according to the invention is preferably obtainable by a catalyst system comprising a single-site catalyst, more preferably obtainable by a metallocene catalyst complex and cocatalysts.

[0070] Preferred complexes of the metallocene catalyst include: rac-dimethylsilanodi-ilbis[2-methyl-4(3',5'-dimethylphenyl)-5-methoxy-6-tert-butylinden-1yl]zirconium dichloreth, dichlorite of rac-anti-dimethylsilanodi-yl[2-methyl-4(4'-tert-butylphenyl)-inden-1-yl][2-methyl-4-(4'tertbutylphenyl)-5-methoxy-6-tert-butylinden-1-yl]zirconium, dichloreth de rac-anti-dimethylsilanodi-yl[2-methyl-4(4'-terc-butylphenyl)-inden-1-yl][2-methyl-4-phenyl-5-methoxy6-terc-butylinden-1-yl]zirconium, dichloreth of rac-anti-dimethylsilanodi-yl[2-methyl-4(3',5'-tert-butylphenyl)-1,5,6,7-tetra-hydro-syndacene-1 Petition 870230108362, dated 08 / 12 / 2023, p. 26 / 137 19 / 36 il][2-methyl-4-(3',5'-dimethyl-phenyl)-5-methoxy-6-tercbutylinden-1-yl]zirconium, dichloreth de rac-anti-dimethylsilanodi-yl[2-methyl-4,8bis-(4′-terc-butylphenyl)-1,5,6,7-tetra-hydro-syndacene-1yl][2-methyl-4-(3′,5′-dimethyl-phenyl)-5-methoxy-6-tercbutylidene,chloronizine-1 rac-anti-dimethylsilanodi-yl[2-methyl-4,8bis(3,,5'-dimethylphenyl)-1,5,6,7-tetra-hydro-s-indacen-1-yl] [2-methyl-4-(3',5'-dimethylphenyl)-5-methoxy-6-tercônyl-butylindene rac-anti-dimethylsilanodi-yl[2-methyl-4,8bis-(3',5'-dimethylphenyl)-1,5,6,7-tetra-hydro-s-indacen-1yl][2-methyl-4-(3',5'-5 diterc-butyl-phenyl)-5-methoxybutyl-zin-6-terc

[0071] Or rac-anti-dimethylsilanodi-yl[2methyl-4,8-bis(3',5'-dimethylphenyl)-1,5,6,7-tetra-hydro-syndacene-1-yl] dichlorate [2-methyl-4-(3',5'-dimethylphenyl-butyl]-n-5-c1-metho zircon is specifically preferred. Co-catalyst

[0072] In order to form an active catalytic species, it is normally necessary to employ a cocatalyst as is well known in the art.

[0073] According to the present invention, a cocatalyst system comprising a boron-containing cocatalyst and an aluminoxane cocatalyst is used in combination with the metallocene catalyst complex defined above.

[0074] The aluminoxane cocatalyst may be one of formula (I): Petition 870230108362, dated 08 / 12 / 2023, page 27 / 137 20 / 36 - R --Al---O-nL J(I) where n is from 6 to 20 and R has the meaning below.

[0075] Aluminoxanes are formed by partial hydrolysis of organoaluminum compounds, for example, those of formula AlR3, AlR2Y and Al2R3Y3 wherein R may be, for example, C1-C10 alkyl, preferably C1-C5 alkyl, or C3C10 cycloalkyl, arylalkyl or alkylaryl and / or C7C12 phenyl or naphthyl, and wherein Y may be hydrogen, halogen, preferably chlorine or bromine, or C1-C10 alkoxy, preferably methoxy or ethoxy. The resulting oxygen-containing aluminoxanes are not, in general, pure compounds, but mixtures of oligomers of formula (I).

[0076] The preferred aluminoxane is methylaluminoxane (MAO). Since the aluminoxanes used according to the invention as cocatalysts are not, due to their method of preparation, pure compounds, the molarity of aluminoxane solutions hereinafter in this document is based on their aluminum content.

[0077] A boron-containing cocatalyst is also used in combination with the aluminoxane cocatalyst.

[0078] The catalyst complex ideally comprises a cocatalyst, with certain boron-containing cocatalysts being preferred. Borates particularly preferred for use in the invention therefore comprise the trityl ion, i.e., triphenylcarbenium. Thus, the use of Ph3CB(PhF5)4 and analogues is therefore particularly favoured.

[0079] The catalyst system of the invention is used in Petition 870230108362, dated 08 / 12 / 2023, page 28 / 137 21 / 36 Support form. The particulate support material used is silica or a mixed oxide such as silica-alumina, in particular silica. The use of a silica support is preferred. The skilled practitioner is aware of the procedures necessary to support a metallocene catalyst.

[0080] In a preferred embodiment, the catalyst system corresponds to ICS3 of WO 2020 / 239598 A1. Article

[0081] The present invention is further directed to a film comprising at least 90% by weight of heterophasic ethylene propylene copolymer (HECO) composition, as described in the preceding sections.

[0082] Preferably, the film is a cast film.

[0083] The film, more preferably the cast film, comprises at least 90% by weight, more preferably at least 93% by weight, even more preferably at least 95% by weight, even more preferably at least 98% by weight, of the heterophasic ethylene propylene copolymer (HECO) composition.

[0084] Other polymeric components besides the heterophasic ethylene propylene copolymer composition may be present in the film, most preferably the molten film; however, it is preferable that the heterophasic ethylene propylene copolymer (HECO) composition be the only polymeric component in the film, most preferably the molten film.

[0085] In a particularly preferred embodiment, the film, more preferably the cast film, consists of a heterophasic ethylene propylene copolymer composition. Petition 870230108362, dated 08 / 12 / 2023, page 29 / 137 22 / 36 (HECO).

[0086] It is preferable that the film, more preferably the cast film, has a thickness in the range of 5 to 100 pm, more preferably in the range of 10 to 80 pm, more preferably in the range of 20 to 70 pm.

[0087] The film, more preferably the cast film, comprising the composition of heterophasic ethylene propylene copolymer (HECO), preferably has a sealing strength, measured according to the method described in this document, in the range of 8.0 to 40 N, more preferably in the range of 10.0 to 35 N, most preferably in the range of 15.0 to 30 N.

[0088] It is preferable that the film, more preferably the cast film, have an opacity value before steam sterilization, measured in accordance with ASTM D1003, of less than 7.0%, more preferably less than 6.0%, most preferably less than 5.0%.

[0089] It is preferable that the film, more preferably the cast film, has an opacity value after steam sterilization, measured in accordance with ASTM D1003, less than 9.0%, more preferably less than 7.0%, most preferably less than 5.0%.

[0090] It is preferable that the film, more preferably the cast film, has a tensile modulus in the machine direction (MD), measured in accordance with ISO 527-3, in the range of 1000 to 1500 MPa, more preferably in the range of 1100 to 1400 MPa, most preferably in the range of 1150 to 1300 MPa.

[0091] It is preferable that the film, more preferably the cast film, have a traction modulus in the direction Petition 870230108362, dated 08 / 12 / 2023, page 30 / 137 23 / 36 transverse (TD), measured in accordance with ISO 527-3, in the range of 900 to 1500 MPa, more preferably in the range of 1000 to 1400 MPa, more preferably in the range of 1100 to 1250 MPa.

[0092] The film, more preferably the cast film, may be a single-layer film. Alternatively, the film, more preferably the cast film, may be present as a single layer in a multi-layer film.

[0093] When the film is present as a single layer in a multilayer film, the film can be produced by any means known in the art. It is preferred that multilayer films be prepared by means of fused film coextrusion. EXAMPLES I. Definitions / Methods of Determination: Melt Flow Rate

[0094] The melt flow rate (MFR) is determined according to ISO 1133 and is indicated in g / 10 min. The MFR is an indication of the flowability and therefore the processability of the polymer. The higher the melt flow rate, the lower the viscosity of the polymer. The MFR2 of polypropylene is determined at a temperature of 230 °C and a load of 2.16 kg. Differential scanning calorimetry (DSC)

[0095] Differential scanning calorimetry (DSC) analysis, melting temperature (Tm) and enthalpy of molten material (Hm), crystallization temperature (Tc) and heat of crystallization (Hc, HCR) are measured with a differential scanning calorimetry (DSC) using a TA Instrument Q200 on samples of 5 to 7 mg. DSC operates according to ISO 11357. Petition 870230108362, dated 08 / 12 / 2023, page 31 / 137 24 / 36 / part 3 / method C2 in a heat / cold / heat cycle with a scan rate of 10 °C / min in the temperature range of -30 to +225 °C. The crystallization temperature (Tc) and heat of crystallization (Hc) are determined from the cooling stage, while the melting temperature (Tm) and enthalpy of molten material (Hm) are determined from the second heating stage. Quantification of PP matrix microstructure by NMR spectroscopy

[0096] Quantitative nuclear magnetic resonance (NMR) spectroscopy was used to quantify stereoregularity (tacticity) and regioregularity of the polymer crystal matrix.

[0097] Quantitative 13C{1H}NMR spectra were recorded in solution state using a Bruker Advance III 400 NMR spectrometer operating at 400.15 and 100.62 MHz for 1H and 13C, respectively. All spectra were recorded using a 10 mm extended temperature probe head optimized for 13C at 125 °C with the use of nitrogen gas for all pneumatics.

[0098] For polypropylene homopolymers, approximately 200 mg of material were dissolved in 1,2-tetrachloroethane-d2 (TCE-d2). To ensure a homogeneous solution, after initial sample preparation in a heating block, the NMR tube was further heated in a rotary oven for at least 1 hour. By inserting the magnet, the tube was rotated at 10 Hz. This configuration was chosen primarily for the high resolution required for quantification of tacticity distribution (Busico, V., Cipullo, R., Prog. Polym. Sci. 26 (2001) 443; Busico, V.; Petition 870230108362, dated 08 / 12 / 2023, page 32 / 137 25 / 36 Cipullo, R., Monaco, G., Vacatello, M., Segre, AL, Macromolecules 30 (1997) 6251). Standard single-pulse excitation was employed using NOE and a WALTZ16 dual-level decoupling scheme (Zhou, Z., Kuemmerle, R., Qiu, X., Redwine, D., Cong, R., Taha, A., Baugh, D. Winniford, B., J. Mag. Reson. 187 (2007) 225; Busico, V., Carbonniere, P., Cipullo, R., Pellecchia, R., Severn, J., Talarico, G., Macromol. Rapid Commun. 2007, 28, 11289). A total of 8192 (8k) variables were acquired by spectra.

[0099] Quantitative 13C{1H} NMR spectra were processed, integrated, and relevant quantitative properties determined from the integrals using specific computer programs. For polypropylene homopolymers, all chemical shifts are internally referenced to the methyl isotactic pentad (mmmm) at 21.85 ppm. The tacticity distribution was quantified by integrating the methyl region between 23.6-19.7 ppm with correction for any sites unrelated to the stereo sequences of interest (Busico, V., Cipullo, R., Prog. Polym. Sci. 26 (2001) 443; Busico, V., Cipullo, R., Monaco, G., Vacatello, M., Segre, A.L., Macromoleucles 30 (1997) 6251).

[0100] Specifically, the influence of regiodefects and comonomer on the quantification of the tacticity distribution was corrected by subtracting representative regiodefect and comonomer integrals from the specific integral regions of the stereo sequences. Isotacticity was determined at the pentad level and reported as the percentage of isotactic pentad sequences (mmmm) relative to all pentad sequences: Petition 870230108362, dated 08 / 12 / 2023, page 33 / 137 26 / 36 [mmmm] % = 100 * (mmmm / sum of all pentads)

[0101] The presence of 2,1 erythro regiodefects was indicated by the presence of the two methyl sites at 17.7 and 17.2 ppm and confirmed by other characteristic sites.

[0102] The characteristic signs corresponding to other types of regiodefects were not observed (Resconi, L., Cavallo, L., Fait, A., Piemontesi, F., Chem. Rev. 2000, 100, 1253). The amount of 2.1 erythro regiodefects was quantified using the integral mean of the two characteristic methyl sites at 17.7 and 17.2 ppm: P21e = ( Ie6 + Ie8 ) / 2

[0103] The amount of primary 1,2-propene inserted was quantified based on the methyl region, with corrections made for sites included in this region unrelated to primary insertion and for primary insertion sites excluded from this region: P12 = Ich3 + P12e

[0104] The total amount of propene was quantified as the sum of primary propene inserted and all other regiodefects present: Ptotal = P12 + P21e

[0105] The mole percentage of 2,1-erythro regiodefects was quantified relative to the whole propene: [21e] % in mol = 100 * (P21e / Ptotal) Dynamic Mechanical Thermal Analysis (DMTA)

[0106] The glass transition temperature Tg is determined by dynamic mechanical thermal analysis (DMTA) according to ISO 6721-7. Measurements are made in torsion mode on compression-molded samples (40x10x1 mm3) between -100 °C and +150 °C with a heating rate of 2 °C / min and a Petition 870230108362, dated 08 / 12 / 2023, page 34 / 137 27 / 36 frequency of 1 Hz. The storage module G' is determined at +23 °C according to ISO 6721-7:1996. Measurements are made in torsion mode on compression-molded samples (40x10x1 mm3) between -150 °C and +150 °C with a heating rate of 2 °C / min and a frequency of 1 Hz. Bending Modulus

[0107] The bending modulus was determined in 3-point bending at 23 °C according to ISO 178 on 80 x 10 x 4 mm3 injection molded test bars in line with EN ISO 1873-2. Notched impact resistance (NIS)

[0108] The Charpy impact resistance with notch was measured in accordance with ISO 179 1eA at +23 °C or -20 °C using 80x10x4 mm3 injection molded bar test specimens prepared in accordance with EN ISO 1873-2. Crystex Analysis Crystalline and soluble fractions method

[0109] The crystalline (CF) and soluble (SF) fractions of the polypropylene (PP) compositions, as well as the comonomer content and intrinsic viscosities of the respective fractions, were analyzed by CRYSTEX QC, Polymer Char (Valencia, Spain).

[0110] A schematic representation of the CRYSTEX QC instrument is shown in Fig. 1a. The crystalline and amorphous fractions are separated through temperature cycles of dissolution at 160 °C, crystallization at 40 °C, and redissolution in 1,2,4-trichlorobenzene (1,2,4-TCB) at 160 °C, as shown in Fig. 1b. Quantification of SF and CF and determination of ethylene content (C2) are obtained using an infrared detector (IR4) and a 2-capillary viscometer in Petition 870230108362, dated 08 / 12 / 2023, page 35 / 137 28 / 36 line, which is used for the determination of intrinsic viscosity (IV).

[0111] The IR4 detector is a multi-wavelength detector that detects IR absorbance in two different bands (CH3 and CH2) for the determination of ethylene concentration and content in ethylene-propylene copolymers. The IR4 detector is calibrated with series of 8 EP copolymers with known ethylene content in the range of 2% by weight to 69% by weight (determined by 13C-NMR spectroscopy) and various concentrations between 2 and 13 mg / ml for each EP copolymer used for calibration.

[0112] The amount of Soluble Fraction (SF) and Fraction Crystalline (CF) fractions are correlated through XS calibration with the amount of "Cold Soluble in Xylene" (XCS) and, respectively, Cold Insoluble in Xylene (XCI) fractions, determined according to the standard gravimetric method as per ISO16152. XS calibration is obtained by testing various EP copolymers with XS content in the range of 2-31% by weight.

[0113] The intrinsic viscosity (iV) of the parent EP copolymer and its soluble and crystalline fractions are determined using a 2-capillary in-line viscometer and are correlated with the corresponding iVs determined by the standard decalin method according to ISO 1628. Calibration is obtained with several EP PP copolymers with iV = 2-4 dl / g.

[0114] A sample of the PP composition to be analyzed is weighed at concentrations of 10 mg / ml to 20 mg / ml. After automated filling of the ampoule with 1,2,4-TCB containing 250 mg / l of 2,6-tert-butyl-4-methylphenol (BHT) as Petition 870230108362, dated 08 / 12 / 2023, page 36 / 137 29 / 36 antioxidant, the sample is dissolved at 160 °C until complete dissolution is achieved, typically for 60 min, with constant stirring at 800 rpm.

[0115] As shown in Figures 1a 1b, a defined volume of the sample solution is injected into the column packed with inert support where sample crystallization and separation of the soluble fraction from the crystalline part is occurring. This process is repeated twice. During the first injection, the entire sample is measured at high temperature, determining the iv[dl / g] and C2[% by weight] of the PP composition. During the second injection, the soluble fraction (at low temperature) and the crystalline fraction (at high temperature) with the crystallization cycle are measured (% by weight of SF, % by weight of C2, iV).

[0116] EP stands for ethylene propylene copolymer.

[0117] PP means polypropylene. Intrinsic viscosity

[0118] Intrinsic viscosity is measured according to DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C). Opacity

[0119] Opacity was determined in accordance with ASTM. D1003-00 in 60x60x1 mm3 injection molded plates according to EN ISO 1873-2 or directly on 50 µm cast film produced in the experimental section. Sealing resistance

[0120] Thermal sealing experiments were performed on at least 3 film samples 85 mm wide by 200 mm long cut in the machine direction. Teflon-coated steel heating rods 5 mm x 150 mm were set to a temperature Petition 870230108362, dated 08 / 12 / 2023, page 37 / 137 30 / 36 of 110 °C. Two films were sealed by positioning, one on top of the other, using a sealing time of 0.5 se pressure of 0.67 N / mm2. The resulting sealed area was 85 mm x 5 mm. The samples were then conditioned for 7 days (± 24 h) at 23 °C (± 2 °C) / 50% RH (± 10%). 10 samples of 15 mm width were cut and tested in tensile mode at 23 °C (± 2 °C) / 50% RH (± 10%) on a Universal Testing Machine (Zwick Z005). The clamping distance used was 100 mm and the test speed was 200 mm / min. The yield strength and maximum strength were measured for each test specimen.

[0121] Basic sealing: • Film width: 85 mm • Film length: > 200 mm • Sealed seam width: 5 mm • Sealing temperature: 110 °C • Sealing pressure: 0.67 N / mm2 • Sealing time: 0.5 s • Sealing jaws: Teflon coated

[0122] Conditioning • Conditioning time: 7 days (± 24 h) at 23 °C (± °C) / 50% RH (± 10%)

[0123] Thermal sealing resistance: • Test temperature: 23 °C (± 2 °C) / 50% RH (± 10%) • Specimen width: 15 mm • Grip distance: 100 mm • Test speed: 200 mm / min • Test device: Universal testing machine Traction module

[0124] The traction module in the machine and in the steering Petition 870230108362, dated 08 / 12 / 2023, page 38 / 137 31 / 36 cross-sectional area was determined according to ISO 527-3 at 23 °C in 50 μm thick melt films produced on a single-layer melt film line with a melt temperature of 220 °C and a cooled roll temperature of °C. The test was performed at a pull speed of mm / min. Steam sterilization

[0125] Steam sterilization was performed on a Systec D series machine (Systec Inc., USA). Samples were heated at a rate of 5 °C / min starting at 23 °C. After being held for 30 min at At 121 °C, they were immediately removed from the steam sterilizer and stored at room temperature until further processing. Experimental: 2.1 Polymerization of the inventive HECO (IE1) Catalyst Synthesis

[0126] The catalyst used was Anti-dimethylsilanedi-yl[2-methyl-4,8-di(3,5-dimethylphenyl) 1,5,6,7-tetrahydro-s-indacen-1-yl][2-methyl-4-(3,5dimethylphenyl)-5-methoxy-6-tert-butylinden-1-yl]zirconium dichloride as disclosed in the WO document 2020 / 239598 A1 as ICS3. Preparation of MAO silica support

[0127] A steel reactor equipped with a mechanical stirrer and filter mesh was purged with nitrogen and the reactor temperature was set to 20 °C. Next, pre-calcined 600 °C DM-L-303 grade silica from AGC Si-Tech Co. (5.0 kg) was added from a feed drum followed by careful pressurization and depressurization with nitrogen using valves. Petition 870230108362, dated 08 / 12 / 2023, page 39 / 137 32 / 36 manuals. Then, toluene (22 kg) was added. The mixture was stirred for 15 min. Next, 30% by weight of solution of MAO in toluene (9.0 kg) from Lanxess was added via the feed line at the top of the reactor within 70 min. The reaction mixture was then heated to 90 °C and stirred at 90 °C for a further two hours. The fluid paste was allowed to settle and the mother liquor was removed by filtration. The catalyst was washed twice with toluene (22 kg) at 90 °C, followed by sedimentation and filtration. The reactor was cooled to 60 °C and the solid was washed with heptane (22.2 kg). Finally, MAO-treated SiO2 was dried at 60 °C under a nitrogen stream for 2 hours and then for 5 hours under vacuum (0.5 barg) with stirring. The MAO-treated support was collected as a free-flowing white powder found to contain 12.2% Al by weight. Catalyst preparation

[0128] 30% by weight of MAO in toluene (0.7 kg) was added to a clean nitrogen-containing steel reactor via a burette at 20 °C. Toluene (5.4 kg) was then added under stirring. The aforementioned catalyst (93 g) was added from a metal cylinder followed by washing with 1 kg of toluene. The mixture was stirred for 60 minutes at 20 °C. Trityltetrakis(pentafluorophenyl)borate (91 g) was then added from a metal cylinder followed by a purge with 1 kg of toluene. The mixture was stirred for 1 h at room temperature. The resulting solution was added to a stirred cake of silica MAO support prepared as described above for 1 hour. The cake was allowed to stand for 12 hours, followed by drying under a stream of N2 at 60 °C for 2 h. Petition 870230108362, dated 08 / 12 / 2023, p. 40 / 137 33 / 36 additionally for 5 h under vacuum (-0.5 barg) with stirring. The dry catalyst was sampled as a free-flowing pink powder containing 13.9 wt% Al and 0.11 wt% Zr.

[0129] The inventive HECO IE1 was polymerized according to the conditions in Table 1.

[0130] The resulting polymer powder was composed of 1250 ppm of cis-1,2-cyclohexanedicarboxylate calcium (Hyperform HPN-20E), supplied by Milliken, USA, and 2000 ppm of Irganox 225 (a 1:1 blend of pentaerythrityl tetrakis(3-(3',5'-dibutyl-4-hydroxytoluyl)propionate and tris(2,4-di-t-butylphenyl)phosphite), supplied by BASF.

[0131] AG, Germany, and 1000 ppm calcium stearate, supplied by Croda, United Kingdom. 2.2 Comparative HECO Polymerization (CE1)

[0132] For the comparative CE1 HECO polymerization process, a Ziegler-Natta type catalyst as used for the inventive examples of document WO 2016 / 066446 A1 and prepolymerized with vinylcyclohexane to obtain nucleation with poly(vinylcyclohexane) was used.

[0133] Nucleation by prepolymerization with vinylcyclohexane is described in detail in documents EP 2 960 256 B1 and EP 2 960 279 B1. The comparative HECO CE1 was polymerized according to the conditions in Table 1, using dicyclopentyl dimethoxysilane (donor D) as the external donor and triethyl aluminum (TEAL) as the cocatalyst. The resulting polymer powder was composed of 1250 ppm of cis-1,2-cyclohexanedicarboxylate calcium (Hyperform HPN-20E), supplied by Milliken, USA, 2000 ppm of Irganox 225 (1:1 blend of pentaerythrityl tetrakis(3-(3',5'-di-ferre-butyl4-hydroxytoluyl)propionate and tris(2,4-di-t-butylphenyl) Petition 870230108362, dated 08 / 12 / 2023, page 41 / 137 34 / 36 phosphite), supplied by BASF

[0134] AG, Germany, and 1000 ppm calcium stearate, supplied by Croda, United Kingdom. 2.3 Cast film production

[0135] The films were produced on the Barmag pilot line CAST-Coex, equipped with a 60 mm diameter extruder and an L / D ratio of 30. A hanger die with a die width of 800 mm and a die clearance of 0.5 mm was used.

[0136] 50 pm films were produced in melt mode with a production rate of 60 kg / h, a line speed of 30 m / min and a melting temperature of 239 °C.

[0137] Roller configurations: 1st roller: diameter 400 mm and °C; 2nd roller: diameter 250 mm and 25 °C.

[0138] Electrical fixation was applied via electrostatic charge.

[0139] Table 1 Polymerization conditions for inventive and comparative HECOs IE1 CE1 Pre-polymerization TEAL / Ti ratio mol / mol - 173 TEAL / Donor ratio mol / mol - 8.0 Temperature °C 20 30 Dwell time min 22 15 Cycle Temperature °C 70 80 Division % by weight 52 39 H2 / C3 feed mol / kmol 0.07 0.40 MFR2 g / 10 min 2.2 2.4 First GPR Petition 870230108362, dated 08 / 12 / 2023, page 42 / 137 35 / 36 IE1 CE1 Temperature °C 80 80 Division % by weight 33 50 H2 / C3 mol / kmol 1.3 7.0 MFR2 g / 10 min 2.2 2.4 Second GPR Temperature °C 70 75 C2 / C3 mol / kmol 768 223 H2 / C2 mol / kmol 2.9 551 Division % by weight 15 11 MFR2 g / 10 min 2.3 3.0 Pellet Tm °C 157 167 Tg(E) °C -43.6 -43.0 Tg(M) °C -0.3 0.7 SF % by weight 11.9 13.9 CF % by weight 88.2 86.2 C2(total) % by mol 2.88 6.56 C2(SF) % by mol 26.8 36.9 C2(CF) mol% 0 3.23 iV(total) dl / g 2.38 2.60 iV(SF) dl / g 2.05 1.67 iV(CF) dl / g 2.41 2.70 G' MPa 672 723 Flexural Modulus MPa 1265 1400 NIS Charpy (23 °C) kJ / m2 41.3 40.0 NIS Charpy (-20 °C) kJ / m2 1.97 1.80 Opacity % 47 54 50 pm film Petition 870230108362, dated 08 / 12 / 2023, page 43 / 137 36 / 36 IE1 CE1 Tensile Modulus (MD) MPa 1177 1292 Tensile Modulus (TD) MPa 1108 1154 Sealing Strength N 17.8 6.9 Opacity (before sterilization) % 4.4 4.7 Opacity (after sterilization) % 4.8 5.3

[0140] As can be seen in Table 1, the inventive HECO (IE1) has comparable mechanical properties (Flexural Modulus, Tensile Modulus and Impact Resistance), although it has improved optical properties (opacity) and significantly improved sealing resistance, compared to the comparator HECO (CE1). Petition 870230108362, dated 08 / 12 / 2023, page 44 / 137

Claims

1 / 5 CLAIMS 1. Heterophasic ethylene propylene copolymer (HECO) composition having a melt flow rate (MFR2) measured according to ISO 1133 at 230 °C and 2.16 kg in the range of 1.0 to 5.0 g / 10 min, a total ethylene C(C2) content, as determined by quantitative IR spectroscopy, in the range of 0.8 to 6.0 mol%, and a melt temperature (Tm) measured by differential scanning calorimetry (DSC) in the range of 153.0 to 159.0 °C, characterized by comprising: a) a crystalline matrix (M) that is a propylene homopolymer or copolymer, preferably a homopolymer; and b) an amorphous propylene-ethylene elastomer (E);wherein the heterophasic ethylene propylene copolymer composition is characterized with respect to its soluble fraction (SF) and crystalline fraction (CF), as determined by CRYSTEX QC analysis: i) 85.0 to 90.0% by weight, based on the total weight of the heterophasic ethylene propylene copolymer composition, of a crystalline fraction (CF) having an intrinsic viscosity iV(CF) measured in accordance with DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C) in the range of 2.00 to 3.00 dl / g, an ethylene C2(CF) content, as determined by quantitative IR spectroscopy, in the range of 0.0 to 1.5% by mol;and ii) from 10.0 to 15.0% by weight, based on the total weight of the heterophasic ethylene propylene copolymer composition, of a soluble fraction (SF) having an intrinsic viscosity iV(SF) measured in accordance with DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C) in Petition 870260072352, dated 21 / 07 / 2026, p. 9 / 18 2 / 5, in the range of 1.30 to 2.50 dl / g and an ethylene C2(SF) content, as determined by quantitative IR spectroscopy, in the range of 25.0 to 40.0% by mol.; 2. Heterophasic ethylene propylene copolymer (HECO) composition according to claim 1, characterized by having an intrinsic viscosity (iV) measured according to DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C) in the range of 2.00 to 3.00 dl / g.

3. Heterophasic ethylene propylene copolymer composition (HECO), according to claim 1 or 2, characterized in that the crystalline matrix (M) has a melt flow rate (MFR2) measured according to ISO 1133 at 230 °C and 2.16 kg in the range of 1.0 to 10.0 g / 10 min, more preferably in the range of 1.5 to 6.0 g / 10 min, most preferably in the range of 2.0 to 4.0 g / 10 min.

4. Heterophasic ethylene propylene copolymer (HECO) composition, according to any one of the preceding claims 1 to 3, characterized in that the ratio of the intrinsic viscosities of the soluble and crystalline fractions, iV(SF) / iV(CF), is in the range of 0.50 to 1.00, more preferably in the range of 0.65 to 0.95, most preferably in the range of 0.75 to 0.

90.

5. Heterophasic ethylene propylene copolymer composition (HECO), according to any one of the preceding claims 1 to 4, characterized in that the crystalline matrix (M) is a homopolymer with an isotactic pentad concentration [mmmm] as determined by 13C-NMR spectroscopy greater than 97.0% and a regiodefect content of 2.1 as determined by 13C-NMR spectroscopy in the range of 0.1 to 1.4 mol%.

6. Heterophasic ethylene propylene copolymer (HECO) composition, according to any of the preceding claims 1 to 5, characterized by having a crystallization temperature (Tc) measured by differential scanning calorimetry (DSC) in the range of 120.0 to 127.0 °C, more preferably in the range of 121.0 to 126.0 °C, with maximum preference in the range of 122.0 to 125.0 °C.

7. Heterophasic propylene ethylene copolymer (HECO) composition, according to any one of the preceding claims 1 to 6, characterized by having: i) a glass transition temperature associated with the amorphous propylene ethylene elastomer (Tg(E)), measured according to ISO 6721-7, in the range of -50 to -40°C, more preferably in the range of -48 to -41°C, most preferably in the range of -46 to -42°C; and / or ii) a glass transition temperature associated with the crystalline matrix (Tg(M)), measured according to ISO 6721-7, in the range of -5 to 5°C, more preferably in the range of -3 to 2°C, most preferably in the range of -2 to 0°C.

8. Heterophasic ethylene propylene copolymer (HECO) composition according to any one of the preceding claims 1 to 7, characterized by having: i) a flexural modulus measured according to ISO 178 in the range of 1100 to 1500 MPa, more preferably in the range of 1200 to 1450 MPa, with maximum preference in the range of 1250 to 1400 MPa, ii) a Charpy Notch Impact Strength (NIS) measured according to ISO 179-1 eA at 23 °C in the range of 25.0 to 100 kJ / m2, more preferably in the range of 30.0 to 80 kJ / m2, with maximum preference in the range of 35.0 to 60 kJ / m2, and / or iii) a Charpy Notch Impact Strength (NIS) measured according to ISO 179-1 eA at -20 °C in the range of 1.0 to 20 kJ / m2, more preferably in the range of 1.4 to 10.0 kJ / m2, Petition 870260072352, dated 21 / 07 / 2026, p. 11 / 18 4 / 5 with maximum preference in the range of 1.8 to 6.0 kJ / m2.

9. Heterophasic ethylene propylene copolymer (HECO) composition, according to any one of the preceding claims 1 to 8, characterized in that the ethylene content of the soluble C2(SF) fraction of CRYSTEX QC, as determined by quantitative IR spectroscopy, is in the range of 25.0 to 33.0 mol%.

10. Heterophasic ethylene propylene copolymer (HECO) composition, according to any one of the preceding claims 1 to 8, characterized in that i) the intrinsic viscosity of the soluble iV(SF) fraction of CRYSTEX QC, measured according to DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C), is in the range of 1.80 to 2.30 dl / g; and / or ii) the intrinsic viscosity of the crystalline iV(CF) fraction of CRYSTEX QC, as measured according to DIN ISO 1628 / 1, October 1999 (in Decalina at 135 °C), is in the range of 2.30 to 2.60 dl / g.

11. Film, preferably a cast film, characterized by comprising at least 90% by weight of the heterophasic ethylene propylene copolymer (HECO) composition as defined in any one of claims 1 to 10.

12. Film, preferably cast film, according to claim 11, characterized in having a thickness in the range of 5 to 100 pm, more preferably in the range of 10 to 80 pm, with maximum preference in the range of 20 to 70 pm.

13. Film, preferably cast film, according to any one of claims 11 or 12, characterized by having a sealing strength in the range of 8.0 to 40 N, more preferably in the range of 10.0 to 35 N, most preferably in the range of 15.0 to 30 N.

14. Film, preferably cast film, according to any one of claims 11 to 13, characterized by having: i) an opacity value before steam sterilization, measured in accordance with ASTM D1003, below 7.0%, more preferably below 6.0%, with maximum preference below 5.0%; and / or ii) an opacity value after steam sterilization, measured in accordance with ASTM D1003, below 9.0%, more preferably below 7.0%, with maximum preference below 5.0%.

15. Film, preferably cast film, according to any one of claims 11 to 14, characterized by having: i) a tensile modulus in the machine direction (MD), measured according to ISO 527-3, in the range of 1000 to 1500 MPa, more preferably in the range of 1100 to 1400 MPa, with maximum preference in the range of 1150 to 1300 MPa; and / or ii) a tensile modulus in the transverse direction (TD), measured according to ISO 527-3, in the range of 900 to 1500 MPa, more preferably in the range of 1000 to 1400 MPa, with maximum preference in the range of 1100 to 1250 MPa. Petition 870260072352, dated 07 / 21 / 2026, page 13 / 18

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