Process for preparing heterophasic polypropylene composition

By using a specific catalyst system and peroxide treatment in the gas phase, the problem of the multi-reactor polymerization method is solved in the prior art that the heterophasic propylene copolymer is difficult to achieve high catalyst yield and high stiffness at the same time, and efficient preparation is achieved. Heterophase propylene copolymer with excellent properties.

CN119213043APending Publication Date: 2024-12-27SABIC GLOBAL TECHNOLOGIES BV
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Patent Information

Application Number
CN202380039986.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Priority Date
2022-05-13
Filing Date
2023-05-05
Publication Date
2024-12-27

AI Technical Summary

Technical Problem

The prior art is difficult to prepare heterophase propylene copolymers with high stiffness at high catalyst yields, and the properties of the polymer are interrelated, and improving some properties can lead to a decrease in other properties.

Method used

The multi-reactor polymerization method is used to produce heterophase propylene copolymers in the gas phase using a specific catalyst system, including the main catalyst prepared from contact with a magnesium-containing support with a halogen-containing titanium compound and an internal electron donor, combined with peroxide for reduction Viscocracking treatment, optimize the ratio of propylene homopolymer and ethylene-propylene copolymer.

Benefits of technology

A heterophase propylene copolymer with high catalyst yield and high stiffness is achieved. By optimizing the catalyst and polymerization conditions, the melt flow rate and structural properties of the composition are improved, and the requirements of high stiffness and high yield are met.

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Abstract

The present invention relates to a process for preparing a polypropylene composition comprising a heterophasic propylene copolymer wherein the heterophasic propylene copolymer consists of a propylene homopolymer matrix in an amount of 71 to 92 wt.%, preferably 78 to 89 wt.%, more preferably 83 to 87 wt.%, based on the heterophasic propylene copolymer, and an ethylene-propylene copolymer in an amount of 70 to 90 wt.%, preferably 78 to 89 wt.%, more preferably 83 to 87 wt.%, based on the heterophasic propylene copolymer, the ethylene-propylene copolymer comprises units derived from ethylene in an amount of 8 to 29 wt%, preferably 11 to 22 wt%, more preferably 13 to 17 wt%, based on the heterophasic propylene copolymer, and wherein the amount of units derived from ethylene is 40 to 60 wt%, preferably 42 to 55 wt%, more preferably 43 to 51 wt%, based on the ethylene-propylene copolymer; and wherein the polypropylene composition has a melt flow rate determined according to ISO 1133: 2011 using 2.16 kg at 230 DEG C of from 0.5 to 120, preferably from 0.5 to 95, more preferably from 0.5 to 85, even more preferably from 0.5 to 80 dg / min, wherein the heterophasic propylene copolymer is produced in a sequential multi-reactor polymerization process in the gas phase in the presence of a catalyst to obtain the heterophasic propylene copolymer, wherein the catalyst comprises a procatalyst, a co-catalyst and optionally an external electron donor, and wherein the procatalyst is obtainable by a process comprising contacting a magnesium-containing support with a halogen-containing titanium compound and an internal electron donor according to formula I, wherein R1 is a secondary alkyl group and R2 is a non-secondary alkyl group having at least 5 carbon atoms, preferably R2 is a non-secondary alkyl group having at least 5 carbon atoms and branched in position 3 or another position; the procatalyst is prepared according to the following steps: i) contacting a compound R < 4 > z Mg X < 4-z > with an alkoxy or aryloxy-containing silane compound to produce a first intermediate reaction product, namely solid Mg (ORa) xX < 12-x >, wherein: Ra is a linear, branched or cyclic hydrocarbyl group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups and combinations of one or more thereof; wherein the hydrocarbyl group may be substituted or unsubstituted, may contain one or more heteroatoms, and preferably have from 1 to 20 carbon atoms; wherein R4 is a linear, branched or cyclic hydrocarbyl group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups and combinations of one or more thereof; wherein the hydrocarbyl group may be substituted or unsubstituted, may contain one or more heteroatoms and preferably have 1 to 20 carbon atoms, preferably R4 is butyl; wherein X4 and X1 are each independently selected from the group consisting of fluorine ion (F-), chloride ion (Cl-), bromide ion (Br-) or iodide ion (I-), preferably chloride ion; z is in a range greater than 0 and less than 2, i.e. 0 lt; zlt, zlt; x is an integer from 0 to 2; ii) optionally contacting the solid Mg (ORa) xX12-x obtained in step i) with at least one activating compound selected from the group consisting of an activating electron donor and a metal alkoxide compound of formula M1 (ORb) v-w (OR3) w or M2 (ORb) v-w (R3) w to obtain a second intermediate product; wherein: M1 is a metal selected from the group consisting of Ti, Zr, Hf, Al or Si; v is the valence of M1; m2 is metal Si; v is the valence of M2; each of Rb and R3 is a linear, branched or cyclic hydrocarbyl group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups and combinations of one or more thereof; wherein the hydrocarbyl group may be substituted or unsubstituted, may contain one or more heteroatoms, and preferably have from 1 to 20 carbon atoms; wherein w is less than v, preferably v is 3 or 4; iii) bringing the first intermediate reaction product or the second intermediate reaction product respectively obtained in step i) or ii) into contact with a halogen-containing Ti compound and the compound represented by formula I as an internal electron donor. # imgabs0 #
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Description

Technical Field

[0001] The present invention relates to a process for the preparation of a heterophasic polypropylene composition.

[0002] In addition, the present invention also relates to an article comprising the polypropylene composition of the present invention, preferably to an article, wherein the article is prepared by injection molding and / or wherein the article is a household article, a packaging article, a health care article or an automotive interior article. In addition, the present invention relates to the use of the polypropylene composition and to a method for preparing the article. Background Art

[0003] Polymers, such as polypropylene, are increasingly being used in applications with different requirements. At the same time, tailor-made polymers that meet the requirements of these applications are constantly sought. The requirements can be challenging because many polymer properties are directly or indirectly interconnected, i.e. improving a specific property can only be achieved at the expense of another property. An example of interconnected properties in polypropylene is impact strength and stiffness.

[0004] There is a need in the art for a process for producing a polypropylene composition comprising a heterophasic propylene copolymer having high stiffness at high catalyst productivity. Summary of the invention

[0005] Accordingly, it is an object of the present invention to provide a process for the preparation of a polypropylene composition comprising a heterophasic propylene copolymer having high stiffness with high catalyst productivity.

[0006] This object is achieved by a process for the preparation of a polypropylene composition comprising a heterophasic propylene copolymer, wherein the heterophasic propylene copolymer consists of:

[0007] a propylene homopolymer matrix in an amount of 71 to 92 wt.-%, preferably 78 to 89 wt.-%, more preferably 83 to 87 wt.-%, based on the heterophasic propylene copolymer, and

[0008] - ethylene-propylene copolymer in an amount of 8 to 29 wt.%, preferably 11 to 22 wt.%, more preferably 13 to 17 wt.%, based on the heterophasic propylene copolymer,

[0009] ● wherein the amount of units derived from ethylene, based on the ethylene-propylene copolymer, is from 40 to 60% by weight, preferably from 42 to 55% by weight, more preferably from 43 to 51% by weight, and

[0010] The polypropylene composition has

[0011] a melt flow rate of 0.5 to 120, preferably 0.5 to 95, more preferably 0.5 to 85, even more preferably 0.5 to 80 dg / min, as determined according to ISO 1133:2011 using 2.16 kg at 230°C, and

[0012] Wherein the multiphase propylene copolymer is produced in the gas phase in the presence of a catalyst in a sequential multi-reactor polymerization process to obtain a multiphase propylene copolymer, wherein the catalyst comprises a procatalyst, a cocatalyst, and an optional external electron donor, and wherein the procatalyst can be obtained by a process comprising the following steps:

[0013] Contacting a magnesium-containing support with a halogen-containing titanium compound and an internal electron donor according to formula I:

[0014]

[0015] Wherein, R 1 is a secondary alkyl group and R 2 is a non-secondary alkyl group having at least 5 carbon atoms, preferably R 2 is a non-secondary alkyl group having at least 5 carbon atoms and branched at the 3-position or another position;

[0016] The procatalyst is prepared according to the following steps:

[0017] i) Contacting the compound R 4 z MgX 4 2-z with a silane compound containing an alkoxy or aryloxy group to produce a first intermediate reaction product, namely solid Mg(OR a ) x X 1 2-x , wherein: R a is a straight-chain, branched, or cyclic hydrocarbon group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl, or alkylaryl groups and one or more combinations thereof; wherein the hydrocarbon group may be substituted or unsubstituted, may contain one or more heteroatoms, and preferably has 1 to 20 carbon atoms; wherein R 4 is a straight-chain, branched, or cyclic hydrocarbon group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl, or alkylaryl groups and one or more combinations thereof; wherein the hydrocarbon group may be substituted or unsubstituted, may contain one or more heteroatoms, and preferably has 1 to 20 carbon atoms, preferably R 4 is butyl; wherein X 4 and X 1 are each independently selected from the group consisting of fluoride ion (F-), chloride ion (Cl-), bromide ion (Br-), or iodide ion (I-), preferably chloride ion; z is in the range greater than 0 and less than 2, i.e., 0 < z < 2, and x is an integer from 0 to 2;

[0018] ii) Optionally, the solid Mg(OR a ) obtained in step i)x X 1 2-x and an activated electron donor selected from the group consisting of 1 (OR b ) v-w (OR 3 ) w or M 2 (OR b ) v-w (R 3 ) w to obtain a second intermediate product; wherein: M 1 is a metal selected from the group consisting of Ti, Zr, Hf, Al or Si; v is M 1 The valence of 2 is metal Si; v is M 2 The valence of b and R 3 Each is a straight chain, branched or cyclic hydrocarbon group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups and one or more combinations thereof; wherein the hydrocarbon group may be substituted or unsubstituted, may contain one or more heteroatoms and preferably has 1 to 20 carbon atoms; wherein w is less than v, preferably v is 3 or 4;

[0019] iii) contacting the first intermediate reaction product or the second intermediate reaction product obtained in step i) or ii) respectively with a halogen-containing Ti compound and the compound represented by formula I as an internal electron donor.

[0020] The present invention also provides a polypropylene composition obtainable or obtainable by the process according to the present invention.

[0021] The present invention also provides a polypropylene composition comprising a heterophasic propylene copolymer, wherein the heterophasic propylene copolymer consists of:

[0022] a propylene homopolymer matrix in an amount of 71 to 92 wt.-%, preferably 78 to 89 wt.-%, more preferably 83 to 87 wt.-%, based on the heterophasic propylene copolymer, and

[0023] - ethylene-propylene copolymer in an amount of 8 to 29 wt.%, preferably 11 to 22 wt.%, more preferably 13 to 17 wt.%, based on the heterophasic propylene copolymer,

[0024] ● wherein the amount of units derived from ethylene, based on the ethylene-propylene copolymer, is from 40 to 60% by weight, preferably from 42 to 55% by weight, more preferably from 43 to 51% by weight, and

[0025] The polypropylene composition has

[0026] • A melt flow rate of 0.5 to 120, preferably 0.5 to 95, more preferably 0.5 to 85, even more preferably 0.5 to 80 dg / min, measured according to ISO 1133:2011 using 2.16 kg at 230°C.

[0027] According to the present invention it has surprisingly been found that the use of a specific catalyst in the process for the preparation of a heterophasic propylene copolymer leads to a combination of high catalyst productivity and high stiffness of the composition (caused by the high stiffness of the homopolymer matrix of the heterophasic propylene copolymer). DETAILED DESCRIPTION

[0028] Heterophasic propylene copolymer

[0029] The polypropylene composition according to the present invention comprises a heterophasic propylene copolymer. The heterophasic propylene copolymer consists of:

[0030] a propylene homopolymer matrix in an amount of 71 to 92 wt.-%, preferably 78 to 89 wt.-%, more preferably 83 to 87 wt.-%, based on the heterophasic propylene copolymer, and

[0031] - ethylene-propylene copolymer in an amount of 8 to 29 wt.%, preferably 11 to 22 wt.%, more preferably 13 to 17 wt.%, based on the heterophasic propylene copolymer,

[0032] The amount of units derived from ethylene, based on the ethylene-propylene copolymer, is from 40 to 60% by weight, preferably from 42 to 55% by weight, more preferably from 43 to 51% by weight, and

[0033] The amount of propylene homopolymer matrix and ethylene-propylene copolymer is 100 wt.%, based on the heterophasic propylene copolymer. The amount of ethylene-propylene copolymer relative to the heterophasic propylene copolymer (sometimes referred to herein as RC) and the amount of units derived from ethylene relative to the amount of ethylene-propylene copolymer in the heterophasic propylene copolymer (sometimes referred to herein as RCC2) can be determined by 13 The results were determined by C-NMR spectroscopy.

[0034] Preferably, the heterophasic propylene copolymer has a CXS in the range of 8 to 29 wt.-%, preferably 10 to 28, more preferably 11 to 22 wt.-%, even more preferably 11 to 16 wt.-%, wherein the CXS is measured by the method described in the "CRYSTEX method for heterophasic propylene copolymers" section of the Test Methods section of the present application.

[0035] Preferably the heterophasic propylene copolymer has a melt flow rate (MFR) in the range of 0.50 to 110 dg / min, wherein the melt flow rate is determined using ISO 1133-1:2011 using 2.16 kg at 230 °C.

[0036] In some preferred embodiments, the heterophasic propylene copolymer has an MFR of 0.50 to 30 dg / min, determined using ISO 1133-1:2011 using 2.16 kg at 230 °C. In some other preferred embodiments, the heterophasic propylene copolymer has an MFR of 30 to 110 dg / min, determined using ISO 1133-1:2011 using 2.16 kg at 230 °C.

[0037] In some embodiments the heterophasic propylene copolymer within the polypropylene composition is prepared by visbreaking an intermediate heterophasic propylene copolymer having an initial melt flow rate (MFRinitial) as determined according to ISO 1133-1:2011 at 230 °C of 0.5 to 50 dg / min, preferably 0.5 to 40 dg / min, more preferably 4.0 to 40 dg / min, as determined according to ISO 1133-1:2011 at 230 °C using 2.16 kg, by contacting the intermediate heterophasic propylene copolymer with a peroxide during melt mixing in an amount such that a composition comprising a heterophasic propylene copolymer having a desired final melt flow rate (MFRfinal) as determined according to ISO 1133-1:2011 at 230 °C of 0.5 to 120, preferably 0.5 to 80, more preferably 5.0 to 80, even more preferably 3 to 45 dg / min is obtained.

[0038] The term "visbreaking" is well known in the field of the present invention. For example, methods for visbreaking polypropylene are disclosed in US 4,282,076 and EP0063654.

[0039] Several different types of well-known chemical reactions can be used to visbreak the propylene polymer. One example is pyrolysis, which is achieved by exposing the polymer to high temperatures, for example above 350° C. in an extruder. Another method is exposure to strong oxidizing agents. Another method is exposure to ionizing radiation. However, it is preferred to use peroxides for visbreaking. Such materials initiate free radical chain reactions at elevated temperatures, resulting in β-fracture of the polypropylene molecules. Visbreaking can be carried out directly after polymerization and removal of unreacted monomers and before pelletization (during extrusion in an extruder, where shifting of the intermediate heterophasic propylene copolymer occurs). However, the present invention is not limited to such an embodiment, and visbreaking can also be carried out on already pelletized polypropylene, which usually contains stabilizers to prevent degradation.

[0040] Examples of suitable peroxides include organic peroxides having a decomposition half-life of less than 1 minute at the average process temperature during the visbreaking step. Suitable organic peroxides include, but are not limited to, dialkyl peroxides such as dicumyl peroxide, peroxyketals, peroxycarbonates, diacyl peroxides, peroxyesters, and peroxydicarbonates. Specific examples of these include benzoyl peroxide, dichlorobenzoyl peroxide, diisopropyl peroxide, di-tert-butyl peroxide, 2,5-dimethyl-2,5-di(peroxybenzoyl)-3-hexene, 1,4-bis(tert-butylperoxyisopropyl)benzene, lauroyl peroxide, tert-butyl peracetate, a,a'-bis(tert-butylperoxy)diisopropylbenzene ( 802), 2,5-dimethyl-2,5-di(tert-butylperoxy)-3-hexene, 2,5-dimethyl-2,5-di(tert-butylperoxy)-hexane, tert-butyl perbenzoate, tert-butyl perphenylacetate, tert-butyl persecanoate, tert-butyl peroxypivalate, isopropyl peroxypivalate, isopropyl hydroperoxide, diisopropyl hydroperoxide, 1,3-bis(tert-butylperoxyisopropyl)benzene, diisopropyl peroxide, tert-butyl peroxyisopropyl carbonate and any combination thereof. Preferably, dialkyl peroxide is used in the method according to the present invention. More preferably, the peroxide is a,a'-bis-(tert-butylperoxy)diisopropylbenzene, 2,5-dimethyl-2,5-di(tert-butylperoxy)-hexane or 3,6,9-triethyl-3,6,9-trimethyl-1,4,7-triperoxynonane. Preferably, the peroxide is selected from the group of non-aromatic peroxides.

[0041] A person skilled in the art can easily determine by routine experimentation how much peroxide should be used to obtain a composition with a desired melt flow rate. This also depends on the half-life of the peroxide and on the conditions used for melt mixing, which in turn depends on the exact composition.

[0042] Preferably, the propylene homopolymer matrix has a pentad isotacticity of at least 96 wt.-%, preferably at least 97 wt.-% before any visbreaking step, wherein 13 C NMR to determine the pentad isotacticity, and / or preferably, the propylene homopolymer matrix before any visbreaking step has a melt flow rate (MFR 500 wt %) measured according to ISO 1133-1:2011 using 2.16 kg at 230° C. in the range of 0.5 to 95, preferably 0.5 to 85, more preferably 5 to 85 dg / min. Hopol ).

[0043] Preferably, the propylene homopolymer matrix has a cold xylene soluble content (CXS) of 1.0 to 4.0 wt%, preferably 1.0 to 3.0 wt%, measured by the method described in the "CRYSTEX Method for Propylene Homopolymers" section of the Test Methods section of this application.

[0044] Preferably, the melt flow rate (MFR) of the ethylene-propylene copolymer is 橡胶 ) is in the range of 0.03 to 3.0 dg / min, preferably in the range of 0.04 to 2.5 dg / min, for example in the range of 0.05 to 2.0 dg / min, wherein MFR is calculated according to the following formula 橡胶 :

[0045] MFR rubber = 10^((Log MFR multiphase - matrix content * Log MFR Hopol ) / (Rubber content))

[0046] in

[0047] MFR Heterophasic is the MFR (dg / min) of the heterophasic propylene copolymer measured according to ISO 1133-1:2011 (2.16 kg / 230°C),

[0048] MFR Hopol is the MFR (dg / min) of the propylene homopolymer matrix measured according to ISO 1133-1:2011 (2.16 kg / 230°C),

[0049] The matrix content is the fraction of the propylene homopolymer matrix in the heterophasic propylene copolymer,

[0050] The rubber content is the fraction of ethylene-propylene copolymer in the heterophasic propylene copolymer. For the avoidance of any doubt, Log in the formula means log10.

[0051] Preferably, the propylene homopolymer matrix has a molecular weight distribution (Mw / Mn) in the range of 1.0 to 11.0, more preferably in the range of 4.0 to 9.0, wherein Mw denotes the weight average molecular weight and Mn denotes the number average molecular weight, and wherein Mw and Mn are measured according to ISO 16014-1 (4):2003.

[0052] Process for the preparation of heterophasic propylene copolymers

[0053] According to the present invention the heterophasic propylene copolymer is produced in a sequential multi-reactor polymerization process in the gas phase in the presence of a catalyst to obtain the heterophasic propylene copolymer.

[0054] The heterophasic propylene copolymer can be prepared by a process comprising the following steps:

[0055] - polymerizing propylene in the presence of a catalyst to obtain a propylene-based substrate, and

[0056] - Subsequently polymerizing ethylene with α-olefins in a propylene-based matrix in the presence of a catalyst to obtain a heterophasic propylene copolymer. These steps are preferably carried out in different reactors. The catalysts of the first and second steps may be different, but are preferably the same.

[0057] catalyst

[0058] The catalyst used for preparing the polypropylene composition according to the present invention is a catalyst described in detail in WO2021 / 063930, which is incorporated herein by reference. The catalyst comprises a main catalyst, a cocatalyst and optionally an external electron donor.

[0059] The procatalyst can be obtained by a process comprising contacting a magnesium-containing support with a halogen-containing titanium compound and an internal electron donor according to formula I:

[0060]

[0061] Where R 1 is a secondary alkyl group and R 2 is a non-secondary alkyl group having at least 5 carbon atoms, preferably R 2 is a non-secondary alkyl group having at least 5 carbon atoms and branched at the 3-position or another position.

[0062] The method for providing the procatalyst comprises the following steps:

[0063] i) making the compound R 4 z MgX 4 2-z contacting with an alkoxy- or aryloxy-containing silane compound to produce a first intermediate reaction product, namely solid Mg(OR a ) x X 1 2-x , where: R a is a straight chain, branched or cyclic hydrocarbon group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups and one or more combinations thereof; wherein the hydrocarbon group may be substituted or unsubstituted, may contain one or more heteroatoms and preferably has 1 to 20 carbon atoms; wherein R 4 is a straight chain, branched or cyclic hydrocarbon group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups and one or more combinations thereof; wherein the hydrocarbon group may be substituted or unsubstituted, may contain one or more heteroatoms and preferably has 1 to 20 carbon atoms, preferably R 4 is butyl; wherein X4 and X 1 are each independently selected from the group consisting of fluoride ion (F-), chloride ion (Cl-), bromide ion (Br-), or iodide ion (I-), preferably chloride ion; z is in the range greater than 0 and less than 2, i.e., 0 < z < 2, and x is an integer from 0 to 2;

[0064] ii) Optionally, contacting the solid Mg(OR a ) x X 1 2-x obtained in step i) with at least one activating compound selected from the group consisting of an activating electron donor and a metal alkoxide compound of the formula M 1 (OR b ) v-w (OR 3 ) w or M 2 (OR b ) v-w (R 3 ) w to obtain a second intermediate product; wherein: M 1 is a metal selected from the group consisting of Ti, Zr, Hf, Al, or Si; v is the valence of M 1 ; M 2 is the metal Si; v is the valence of M 2 ; R b and R 3 are each independently a straight-chain, branched, or cyclic hydrocarbon group selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl, or alkylaryl groups and one or more combinations thereof; wherein the hydrocarbon group may be substituted or unsubstituted, may contain one or more heteroatoms, and preferably has 1 to 20 carbon atoms; wherein w is less than v, and preferably v is 3 or 4;

[0065] iii) Contacting the first intermediate reaction product or the second intermediate reaction product obtained in step i) or ii) respectively with a halogen-containing Ti compound and the compound of formula I as an internal electron donor.

[0066] In one embodiment, during step ii), as the activating compound, an alcohol is used as the activating electron donor and a tetraalkyl titanate is used as the metal alkoxide compound.

[0067] In one embodiment, an activator is present. In one embodiment, the activator is ethyl benzoate. In one embodiment, the activator is a benzamide according to formula X:

[0068]

[0069] wherein R70 and R 71 are each independently selected from hydrogen or alkyl, and R 72 , R 73 , R 74 , R 75 , R 76 Each is independently selected from hydrogen, a heteroatom or a hydrocarbon group, which is preferably selected from an alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl group and one or more combinations thereof, more preferably wherein R 70 and R 71 are all methyl and R 72 , R 73 , R 74 and R 75 All are hydrogen, namely N,N'-dimethylbenzamide (Ba-2Me).

[0070] In some preferred embodiments, the activating compound is NN-dimethylbenzamide.

[0071] Preferably, the internal electron donor used is according to formula I:

[0072]

[0073] Where R 1 is a secondary alkyl group having at least three carbon atoms (C3) and R 2 is a non-secondary alkyl group having at least 5 carbon atoms, preferably R 1 and R 2 having up to seven carbon atoms (C7), preferably up to six carbon atoms (C6), preferably isopropyl, isobutyl, isopentyl, cyclopentyl, n-pentyl and isohexyl, preferably R 2 Branching at position 3 or another position.

[0074] In another embodiment, the internal electron donor is 3,3-bis(methoxymethyl)-2,6-dimethylheptane, according to Formula I, wherein R1 is isopropyl, i.e., a secondary alkyl group, and R2 is isopentyl, i.e., a non-secondary alkyl group and having a branch on the third carbon atom (abbreviated as iPiPen, where iP represents isopropyl and iPen represents isopentyl, also known as 3-methyl-butyl). The compound iPiPen has C 13 H 28 O 2 Chemical formula; exact mass of 216.21 and molecular weight of 216.37. In a more preferred embodiment of the present invention, iPiPen is used as internal donor and preferably N,N-dimethylbenzamide is used as activating agent.

[0075]

[0076] In another embodiment, the internal electron donor is (1-methoxy-2-(methoxymethyl)-5-methylhexan-2-yl)cyclopentane, according to Formula I, wherein R 1 is a secondary alkyl cyclopentyl and R 2 is a secondary cyclopentyl group (abbreviated as CPiPen, where CP represents cyclopentyl and iPen represents isopentyl, also known as 3-methyl-butyl). 15 H 30 O 2 Chemical formula; exact mass of 242.22 and molecular weight of 242.40. In a more specific embodiment, CPiPen is used as internal donor and N,N-dimethylbenzamide is preferably used as activator.

[0077]

[0078] In another embodiment, the internal electron donor is 3,3-bis(methoxymethyl)-2,7-dimethyloctane, according to Formula I, wherein R 1 isopropyl secondary alkyl and R 2 is a non-secondary isohexyl radical with a branch on the fourth carbon atom (abbreviated as iPiHex, where iP represents isopropyl and iHex represents isohexyl, also known as 4-methyl-pentyl). The compound iPiHex has C 14 H 30 O 2 ; exact mass of 230.22 and molecular weight of 230.39. In a more specific embodiment, iPiHex is used as an internal donor and N,N-dimethylbenzamide is preferably used as an activating agent.

[0079]

[0080] In another embodiment, the internal electron donor is 3,3-bis(methoxymethyl)-2-methyloctane, according to Formula I, wherein R 1 isopropyl secondary alkyl and R 2 is a non-secondary non-branched n-pentyl group (abbreviated as iPnPen, wherein iP represents isopropyl and nPen represents n-pentyl). The compound iPnPen has C 13 H 28 O 2 ; exact mass of 216.21 and molecular weight of 216.37. In a more specific embodiment, iPnPen is used as internal donor and N,N-dimethylbenzamide is preferably used as activator.

[0081]

[0082] In another embodiment, the internal electron donor is 3,3-bis(methoxymethyl)-2,6-dimethyloctane, according to Formula I, wherein R 1 isopropyl secondary alkyl and R 2 It is a non-secondary branched hexyl group with a branch at the third carbon atom (abbreviated as iP3Hex, wherein iP represents an isopropyl group and wherein 3Hex represents a hexyl group with a branch at the third carbon atom, also known as 3-methyl-pentyl). The compound iP3Hex has C 14 H 32 O 2 Chemical formula; exact mass of 230.22 and molecular weight of 230.39. In a more preferred embodiment, iP3Hex is used as internal donor and / or N,N-dimethylbenzamide is preferably used as activating agent.

[0083]

[0084] In one embodiment, the substituent R 1 is isopropyl or cyclopentyl. In one embodiment, the substituent R 2 The following table shows the above embodiments together with their abbreviations and R 1 and R 2 groups, whether these groups are secondary and whether they are branched.

[0085] According to the present invention, it is also preferred that R 1 is a secondary alkyl group and R 2 is a non-secondary alkyl group branched at the 3-position or another position.

[0086]

[0087] In some preferred embodiments, the cocatalyst is selected from the group consisting of trimethylaluminum, triethylaluminum, triisobutylaluminum, trihexylaluminum, diisobutylaluminum hydride, trioctylaluminum, dihexylaluminum hydride, and mixtures thereof.

[0088] Preferably, the external electron donor is selected from the group of compounds having the structure according to:

[0089] -Formula III: (R 90 ) 2 N—Si(OR 91 ) 3 ,

[0090] -Formula IV: (R 92 )Si(OR 93 ) 3 ,

[0091] -Formula V:Si(OR a )4-n R b n ,and

[0092] - mixtures thereof,

[0093] Among them, R 90 , R 91 , R 92 and R 93 Each of the groups is independently a linear, branched or cyclic, substituted or unsubstituted alkyl group having 1 to 10 carbon atoms, preferably wherein R 90 , R 91 , R 92 and R 93 The groups are each independently a straight-chain unsubstituted alkyl group having 1 to 8 carbon atoms,

[0094] Where n can be 0 to 2, and R a and R b Each of independently represents an alkyl or aryl group, optionally containing one or more heteroatoms, such as O, N, S or P, having, for example, 1 to 20 carbon atoms.

[0095] For example, the external electron donor can be ethyl, methyl or n-propyl, such as diethylaminotriethoxysilane (DEATES), n-propyltriethoxysilane (nPTES), n-propyltrimethoxysilane (nPTMS), diisobutyldimethoxysilane (DiBDMS), tert-butylisopropyldimethoxysilane (tBuPDMS), cyclohexylmethyldimethoxysilane (CHMDMS), dicyclopentyldimethoxysilane (DCPDMS) or diisopropyldimethoxysilane (DiPDMS). More preferably, the external electron donor is selected from di(isopropyl)dimethoxysilane (DiPDMS) or diisobutyldimethoxysilane (DiBDMS).

[0096] Preferably, the external donor comprises or consists of a compound selected from the list comprising organosilicon compounds, silanes, alkoxysilanes, alkylsilanes, alkylalkoxysilanes and aliphatic / aromatic esters, for example dicyclopentyldimethoxysilane, di-tert-butyldimethoxysilane, methylcyclohexyldimethoxysilane, ethylcyclohexyldimethoxysilane, diphenyldimethoxysilane, diisopropyldimethoxysilane, di-n-propyldimethoxysilane, diisobutyldimethoxysilane, di-n-butyldimethoxysilane, cyclopentyltrimethoxysilane, isopropyltrimethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, ethyltriethoxysilane, tetramethoxysilane, tetraethoxysilane, cyclopentylpyrrolidinodimethoxysilane, bis(pyrrolidino)dimethoxysilane, and mixtures thereof, preferably di(isopropyl)dimethoxysilane (DiPDMS).

[0097] The compounds mentioned above as examples of external electron donors are sometimes referred to as selectivity control agents (SCA). The external electron donor may consist of SCA. Alternatively, in addition to SCA, the external electron donor may additionally include a compound referred to as an activity limiting agent (ALA). Preferably, the activity limiting agent (ALA) is selected from the group consisting of ethyl acetate, ethyl benzoate, ethyl p-ethoxybenzoate, methyl trimethylacetate, isopropyl myristate, di-n-butyl sebacate, (poly)(alkylene glycol) mono- or diacetate, (poly)(alkylene glycol) mono- or dimyristate, (poly)(alkylene glycol) mono- or dilaurate, (poly)(alkylene glycol) mono- or dioleate, triacetin, a mixed glyceride of linoleic acid, oleic acid, palmitic acid and stearic acid, and a mixture thereof. More preferably, the activity limiting agent (ALA) is isopropyl myristate.

[0098] The ratio of selectivity control agent (SCA) to activity limiting agent (ALA) is not critical in principle, with best results being obtained with a SCA / ALA ratio in the range of 0.010 to 100, more preferably in the range of 0.10 to 20.

[0099] The molar ratio of Al in the promoter to Si in the external electron donor may be, for example, 1 to 120.

[0100] In a preferred embodiment, the molar ratio of Al in the co-catalyst to Si in the external electron donor is from 1 to 25, preferably from 1 to 15, preferably from 3 to 10, more preferably from 3.5 to 8. A relatively low molar ratio of Al / Si results in a higher rigidity of the composition. In some preferred embodiments, the molar ratio of Al in the co-catalyst to Si in the external electron donor is greater than 15 and at most 120 or greater than 25 and at most 120. A relatively high molar ratio of Al / Si results in a higher catalyst productivity.

[0101] In some embodiments, the preferred molar ratio of Si in the external electron donor to Ti in the primary catalyst is 10 to 50.

[0102] In some embodiments, the preferred molar ratio of Al in the co-catalyst to Ti in the main catalyst is 125-250.

[0103] Catalyst productivity (CY) Ti*Productivity / Mass retention:

[0104] Preferably, the process has a CY Ti (KgPP / g catalyst)*productivity (Kg / h) / mass hold-up (Kg) of at least 25, more preferably at least 30, more preferably at least 35, more preferably at least 40, wherein CY Ti (KgPP / g catalyst) is calculated according to equation (1):

[0105]

[0106] The Ti content in the catalyst and the Ti content in the obtained polymer were measured by inductively coupled plasma mass spectrometry (ICP-MS).

[0107] Composition

[0108] The polypropylene composition has a melt flow rate (MFR) in the range of 0.50 to 110 dg / min, wherein the melt flow rate is determined using ISO 1133-1:2011 using 2.16 kg at 230°C. In some preferred embodiments, the MFR of the polypropylene composition measured using ISO 1133-1:2011 using 2.16 kg at 230°C is from 0.50 to 30 dg / min. In some preferred embodiments, the MFR of the polypropylene composition measured using ISO 1133-1:2011 using 2.16 kg at 230°C is from 30 to 110 dg / min.

[0109] Preferably the amount of heterophasic propylene copolymer is at least 95 wt.-%, based on the polypropylene composition.

[0110] Inorganic fillers

[0111] The composition according to the present invention may contain an inorganic filler. Suitable examples of inorganic fillers include talc, calcium carbonate, wollastonite, barium sulfate, kaolin, glass flakes, layered silicates (bentonite, montmorillonite, montmorillonite) and mica. For example, the inorganic filler is selected from talc, calcium carbonate, wollastonite, mica and mixtures thereof. More preferably, the inorganic filler is talc.

[0112] Preferably, the inorganic filler has a median diameter d50, determined according to ISO 13320-1:2020, of 5 to 20 μm, preferably 3 to 15 μm.

[0113] The composition according to the invention may be free or substantially free of inorganic fillers. For example, the composition according to the invention may comprise less than 1.0 wt%, less than 0.1 wt% or less than 0.01 wt% of inorganic fillers.

[0114] additive

[0115] In some embodiments, the polypropylene composition additionally comprises additives, e.g. in an amount of 0.10 to 1.0 wt.-%, based on the polypropylene composition.

[0116] Suitable additives include, but are not limited to, stabilizers. The stabilizer may, for example, be selected from a heat stabilizer, an antioxidant and / or a UV stabilizer. Examples include conventional stabilizers such as Irgafos 168, Irganox 1010 and / or Irganox B225.

[0117] Additives may further include nucleating agents, colorants such as pigments and dyes; clarifying agents; surface tension adjusting agents; lubricants; flame retardants; mold release agents; flow improvers; plasticizers; antistatic agents; foaming agents; and slip agents.

[0118] In one aspect, the present invention provides an article comprising a polypropylene composition of the present invention. Preferably, based on the article, the amount of the polypropylene composition is at least 95% by weight. Preferably, the article is prepared by injection molding. Preferably, the article is a household article, such as a vacuum cleaner housing, household chemicals and paint, or a packaged article, such as a container, a crate, a box, a battery shell, a bucket, a flower pot, a food container / package, an ice cream container, a thin-walled package, a lid and a closure, a health care package, or a health care article, such as a drug delivery article, a laboratory ware, a medical device, a medical diagnostic article, or an automotive interior article, such as a dashboard bracket, a door panel, an instrument panel, an instrument panel bracket, a door cladding, a door fixture, an armrest, a pillar cladding, a seat cladding, a trunk cladding, an interior decoration, and applications in heating, ventilation, and air conditioning (HVAC) applications.

[0119] In one aspect, the present invention provides the use of the polypropylene composition of the present invention for preparing articles. Preferably, based on the article, the amount of the polypropylene composition is at least 95% by weight. Preferably, the article is prepared by injection molding. Preferably, the article is a household article, such as a vacuum cleaner housing, household chemicals and paint, or a packaged article, such as a container, a crate, a box, a battery shell, a bucket, a flower pot, a food container / package, an ice cream container, a thin-walled package, a lid and a closure, a health care package, or a health care article, such as a drug delivery article, a laboratory ware, a medical device, a medical diagnostic article, or an automotive interior article, such as a dashboard bracket, a door panel, an instrument panel, an instrument panel bracket, a door cladding, a door fixture, an armrest, a pillar cladding, a seat cladding, a trunk cladding, an interior decoration, and applications in heating, ventilation, and air conditioning (HVAC) applications.

[0120] In one aspect, the present invention provides a method for preparing an article, comprising the steps of:

[0121] a. Provide a polypropylene composition of the present invention, and

[0122] b. Converting the polypropylene composition into an article, for example by using extrusion or injection molding methods.

[0123] It is further noted that the present invention relates to any possible combination of features described herein, including all possible combinations of embodiments described herein, preferably in particular those combinations of features or embodiments presented in the claims. Thus, it will be appreciated that all combinations of features or embodiments relating to compositions according to the invention; all combinations of features or embodiments relating to methods according to the invention; and all combinations of features or embodiments relating to compositions according to the invention with features or embodiments relating to methods according to the invention are described herein.

[0124] It is also noted that the term "comprising / including / containing" does not exclude the presence of other elements. However, it is also understood that a description of a product / composition comprising certain components also discloses a product / composition consisting of these components. A product / composition consisting of these components may be advantageous because it provides a simpler and more economical method for preparing the product / composition. Similarly, it is also understood that a description of a method comprising certain steps also discloses a method consisting of these steps. A method consisting of these steps may be advantageous because it provides a simpler and more economical method.

[0125] The invention is now explained with the aid of the following examples without, however, being restricted thereto.

[0126] Example

[0127] Method for preparing primary catalyst

[0128] For Examples E1 and E2 of the present invention: the main catalyst was prepared according to the method disclosed in Example 1 of WO2021 / 063930A1;

[0129] For Comparative Examples CE1 and CE2: The procatalyst was INcat P420, commercially available from INEOS Polyolefin Catalyst, and prepared according to the manufacturer's instructions.

[0130] Process conditions of embodiments E1, E2, CE1 and CE2 of the present invention

[0131] The gas phase polymerization to prepare the heterophasic propylene copolymers E1, E2, CE1 and CE2 was carried out in a set of two horizontal cylindrical stirred bed gas phase reactors connected in series.

[0132] In the first reactor (R1) a homopolymer is formed and in the second reactor (R2) an ethylene-propylene copolymer rubber is formed to produce a heterophasic propylene copolymer. Both reactors are operated in continuous mode.

[0133] During operation, the polypropylene powder produced in the first reactor is discharged into the second reactor through the powder discharge system.

[0134] The temperature of the powder bed is measured by a series of internal thermocouples. The data from these thermocouples is used to control the quench flow to the various quench nozzles.

[0135] Hydrogen is fed to both reactors independently to control the melt flow index ratio of the homopolymer powder and the copolymer powder. In this respect, RCC2 is the amount of ethylene incorporated in the rubber fraction (wt%) and RC is the amount of rubber incorporated in the heterophasic propylene copolymer (wt%), by 13 Determined by C-NMR spectroscopy.

[0136] The propylene homopolymer from the first reactor was collected and its properties were measured.The heterophasic propylene copolymer from the second reactor and its properties were measured.

[0137] Table 1 shows the catalysts used in the polymerization process of the heterophasic propylene copolymer as well as various properties of the homopolymer obtained from the first reactor and various properties of the heterophasic propylene copolymer obtained from the second reactor.

[0138] Table 1. Polymerization reaction conditions and polymer properties

[0139]

[0140] Al / Ti is the molar ratio of co-catalyst (TEA) to main catalyst

[0141] Si / Ti is the molar ratio of external donor (DiPDMS) to main catalyst

[0142] Al / Si is the molar ratio of co-catalyst (TEA) to external donor (DiPDMS)

[0143] H2 / C3 is the molar ratio of hydrogen to propylene

[0144] It can be seen that the process of preparing E1-E2 using a catalyst comprising the main catalyst of the present invention has a higher catalyst yield (expressed by CY Ti* productivity / mass retention) than CE1-CE2 prepared using a catalyst comprising a different main catalyst, while resulting in a composition with comparable rigidity, which can be understood from the comparable values ​​of CXS and isotacticity.

[0145] Surprisingly, E1-E2 using lower Al / Si molar ratio (higher Si amount) in the catalyst than CE1-CE2 resulted in higher catalyst productivity than CE1. This shows that the type of procatalyst in the catalyst leads to differences in catalyst productivity.

[0146] Furthermore, lower amounts of Ti were detected in E1-E2 compared to CE1-CE2.

[0147] Test Method

[0148] MFR

[0149] MFRhopol, MFRinitial and MFRfinal of the heterophasic propylene copolymer composition, matrix phase and dispersed phase are measured according to ISO 1133 using 2.16 kg load at 230 °C.

[0150] RC, RCC2 and TC2

[0151] use 13 C-NMR spectroscopy was used to measure RC and RCC2. To this end, approximately 150 mg of material was dissolved in 1,1,2,2-tetrachloroethane-d2 (TCE-d2). To ensure a homogeneous solution, sample preparation was performed in a heated rotary oven. NMR measurements were performed in solution using a Bruker 500Advance III HD spectrometer running 1H and 13C at 500.16 and 125.78 MHz, respectively, and equipped with a 10 mm dual cryogenically cooled probe head running at 125 °C. 13C-NMR experiments were performed using standard single pulse excitation with NOE and two-level WALTZ16 decoupling scheme (Zhou Z. et al. J. Mag. Reson 187 (2007) 225. A total of 512 transients were acquired for each spectrum. The spectra were calibrated by setting the central signal of the triplet state of TCE at 74.2 ppm. Quantitative 13C NMR spectra were processed, integrated and relevant quantitative properties determined from the integrals using a proprietary computer program.

[0152] The total ethylene content (TC2) of the copolymer was calculated from RC and RCC2.

[0153] CRYSTEX Method

[0154] The CRYSTEX method described in WO2019179959 and herein allows the determination of the following properties of heterophasic propylene copolymers:

[0155] Amount of amorphous soluble fraction in the heterophasic propylene copolymer (CXS)

[0156] • Amount of amorphous soluble fraction in the propylene homopolymer matrix (CXS hopol).

[0157] The measurement of these properties can be carried out according to the CRYSTEX method by a CRYSTEX QC instrument of the CRYSTEX QC Polymer Char (Valencia, Spain). A schematic diagram of the CRYSTEX QC instrument is given in Del Hierro, P.; Ortin, A.; Monrabal, B.; 'Soluble Fraction Analysis in polypropylene, The Column', February 2014, pp. 18-23.

[0158] The CRYSTEX QC instrument includes an infrared detector (IR4) and an online dual capillary viscometer. Quantification is accomplished by an infrared detector that detects IR absorbance in two different bands (CH3 and CH2).

[0159] The machine was calibrated using the cold xylene soluble (CXS) fraction and the cold xylene insoluble (CXI) fraction of various propylene polymers with known CXS content determined by standard gravimetric method according to ISO16152.

[0160] CRYSTEX process for heterophasic propylene copolymers

[0161] A sample of the heterophasic propylene copolymer to be analyzed was weighed at a concentration of 5 mg / mL. After automatically filling the vial with 1,2,4-TCB containing 250 mg / L 2,6-tert-butyl-4-methylphenol (BHT) as antioxidant, the sample was dissolved at 170°C until complete dissolution was achieved, for 120 min, while continuously stirring at 800 rpm.

[0162] CRYSTEX method for propylene homopolymer matrices

[0163] A sample of the PP homopolymer to be analyzed (out of the first reactor: propylene homopolymer matrix) was weighed at a concentration of 10 mg / mL. After automatically filling the vial with 1,2,4-TCB containing 250 mg / L 2,6-tert-butyl-4-methylphenol (BHT) as an antioxidant, the sample was dissolved at 170°C until complete dissolution was achieved, for 60 min, while continuously stirring at 800 rpm.

[0164] Isotacticity 13 C NMR

[0165] 175 mg of polypropylene pellets were dissolved in 3 ml of deuterated tetrachloroethylene (C2D2Cl4) containing 2,6-di-tert-butyl-4-methylphenol (BHT) at 130°C (5 mg BHT in 200 ml C2D2Cl). The spectra were recorded on a Bruker Avance 500 spectrometer equipped with a cryogenically cooled probe head operating at 125°C.13 C NMR spectroscopy.

[0166] The isotacticity of the mmmm pentad level is given by 13 C NMR spectroscopy, in % based on total pentad amount.

[0167] Catalyst productivity (CY) Ti (KgPP / g catalyst) * productivity (Kg / h) / mass retention (Kg)

[0168] The Ti content in the catalyst and the Ti content in the obtained polymer were measured by ICP. The ICP procedure was as follows: approximately 250 mg of each sample was digested in 6 mL of concentrated nitric acid (trace metal grade) using an Anton Paar Multiwave PRO equipped with a closed high pressure quartz digestion vessel by microwave assisted acid digestion. After the microwave digestion run, the acid analysis was transferred to a pre-cleaned plastic centrifuge tube containing 1 mL of internal standard solution and diluted to the 50 mL mark with MilliQ water. The elements in the samples were quantified using an Agilent 8900 ICP-MS system using a multi-element calibration set from Inorganic Ventures.

[0169] Then calculate CY according to equation (1)

[0170]

[0171] The production rate (Kg / h) and mass holdup (Kg) were measured.

[0172] The production rate (Kg / h) / mass hold-up (Kg) corresponds to the polymer residence time.

Claims

1. Process for the preparation of a polypropylene composition comprising a heterophasic propylene copolymer, Wherein the heterophasic propylene copolymer consists of: a propylene homopolymer matrix in an amount of 71 to 92 wt.-%, preferably 78 to 89 wt.-%, more preferably 83 to 87 wt.-%, based on the heterophasic propylene copolymer, and - ethylene-propylene copolymer in an amount of 8 to 29 wt.%, preferably 11 to 22 wt.%, more preferably 13 to 17 wt.%, based on the heterophasic propylene copolymer, ● wherein the amount of units derived from ethylene, based on the ethylene-propylene copolymer, is from 40 to 60% by weight, preferably from 42 to 55% by weight, more preferably from 43 to 51% by weight, and The polypropylene composition has a melt flow rate, measured according to ISO 1133:2011 using 2.16 kg at 230° C., of 0.5 to 120, preferably 0.5 to 95, more preferably 0.5 to 85, even more preferably 0.5 to 80 dg / min, wherein the heterophasic propylene copolymer is produced in a sequential multi-reactor polymerization process in the gas phase in the presence of a catalyst to obtain the heterophasic propylene copolymer, wherein the catalyst comprises a procatalyst, a cocatalyst and optionally an external electron donor, wherein the procatalyst is obtainable by a process comprising the steps of: The magnesium-containing support is contacted with a halogen-containing titanium compound and an internal electron donor according to formula I: Among them, R 1 is a secondary alkyl group and R 2 is a non-secondary alkyl group having at least 5 carbon atoms, preferably R 2 is a non-secondary alkyl group having at least 5 carbon atoms and branched at the 3-position or another position; The main catalyst is prepared according to the following steps: i) Contact compound R 4 z MgX 4 2-z with an alkoxy - or aryloxy - containing silane compound to produce a first intermediate reaction product, i.e., solid Mg(OR a ) x X 1 2-x , where: R a is a straight - chain, branched or cyclic hydrocarbon group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups and one or more combinations thereof; wherein the hydrocarbon group may be substituted or unsubstituted, may contain one or more heteroatoms and preferably has 1 to 20 carbon atoms; where R 4 is a straight - chain, branched or cyclic hydrocarbon group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups and one or more combinations thereof; wherein the hydrocarbon group may be substituted or unsubstituted, may contain one or more heteroatoms and preferably has 1 to 20 carbon atoms, preferably R 4 is butyl; where X 4 and X 1 are each independently selected from the group consisting of fluoride ion (F-), chloride ion (Cl-), bromide ion (Br-) or iodide ion (I-), preferably chloride ion; z is in the range greater than 0 and less than 2, i.e., 0 < z < 2, and x is an integer from 0 to 2; ii) optionally subjecting the solid Mg(OR) obtained in step i) to a ) x X 1 2-x and an activated electron donor selected from the group consisting of 1 (OR b ) v-w (OR 3 ) w or M 2 (OR b ) v-w (R 3 ) w to obtain a second intermediate product; wherein: M 1 is a metal selected from the group consisting of Ti, Zr, Hf, Al or Si; v is M 1 The valence of 2 is metal Si; v is M 2 The valence of b and R 3 Each is a straight chain, branched or cyclic hydrocarbon group independently selected from alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl groups and one or more combinations thereof; wherein the hydrocarbon group may be substituted or unsubstituted, may contain one or more heteroatoms and preferably has 1 to 20 carbon atoms; wherein w is less than v, preferably v is 3 or 4; iii) contacting the first intermediate reaction product or the second intermediate reaction product obtained in step i) or ii) respectively with a halogen-containing Ti compound and the compound represented by formula I as an internal electron donor.

2. The process according to claim 1, wherein the co-catalyst is selected from the group consisting of trimethylaluminum, triethylaluminum, triisobutylaluminum, trihexylaluminum, diisobutylaluminum hydride, trioctylaluminum, dihexylaluminum hydride and mixtures thereof.

3. The process according to any one of the preceding claims, wherein the catalyst comprises an external donor, wherein the external electron donor is a silane-containing external donor, preferably wherein the external electron donor is selected from the group of compounds having the structure according to: Formula III: (R 90 )2N—Si(OR 91 )3, Formula IV: (R 92 )Si(OR 93 )3, Formula V: Si(OR a ) 4-n R b n , and mixtures thereof, in, R 90 , R 91 , R 92 and R 93 Each of the groups is independently a linear, branched or cyclic, substituted or unsubstituted alkyl group having 1 to 10 carbon atoms, preferably wherein R 90 , R 91 , R 92 and R 93 The groups are each independently a straight-chain unsubstituted alkyl group having 1 to 8 carbon atoms, Where n can be 0 to 2, and R a and R b Each of which independently represents an alkyl or aryl group, optionally containing one or more heteroatoms, such as O, N, S or P, having, for example, 1 to 20 carbon atoms, and The molar ratio of Al in the promoter to Si in the external electron donor is 1-25, preferably 1-15, more preferably 3-10. 4 . The process according to claim 1 , wherein during step ii) as activating compound an alcohol is used as activating electron donor and a tetraalkyl titanate is used as metal alkoxide compound.

5. A method according to any one of the preceding claims, wherein: An activator is present, preferably a benzamide according to formula X: Where R 70 and R 71 are each independently selected from hydrogen or alkyl, and R 72 , R 73 , R 74 , R 75 , R 76 Each is independently selected from hydrogen, a heteroatom or a hydrocarbon group, which is preferably selected from an alkyl, alkenyl, aryl, aralkyl, alkoxycarbonyl or alkylaryl group and one or more combinations thereof, more preferably wherein R 70 and R 71 are all methyl and R 72 , R 73 , R 74 and R 75 All are hydrogen, namely N,N'-dimethylbenzamide (Ba-2Me).

6. The process according to any one of the preceding claims, wherein the process has a CY Ti (KgPP / g catalyst) * productivity (kg / h) / mass hold-up (kg) of at least 25, more preferably at least 30, more preferably at least 35, more preferably at least 40, wherein CY Ti (kgPP / g catalyst) is calculated according to equation (1): in, The Ti content in the catalyst and the Ti content in the obtained polymer were determined by inductively coupled plasma mass spectrometry (ICP-MS).

7. The process according to any one of the preceding claims, wherein the propylene homopolymer matrix has a cold xylene soluble content (CXS) of 1.0 to 4.0 wt.-%, preferably 1.0 to 3.0 wt.-%, measured by the method described in the section "CRYSTEX Method for Propylene Homopolymers" in the Measurement Methods section of the specification.

8. Process according to anyone of the preceding claims, wherein the heterophasic propylene copolymer within the polypropylene composition is prepared by visbreaking an intermediate heterophasic propylene copolymer having an initial melt flow rate (MFRinitial) determined according to ISO 1133:2011 at 230 °C of 0.5 to 50 dg / min, preferably 0.5 to 40 dg / min, more preferably 4.0 to 40 dg / min, measured according to ISO 1133:2011 using 2.16 kg, during melt mixing with a peroxide in such an amount that a composition comprising the heterophasic propylene copolymer having a desired final melt flow rate (MFRfinal) determined according to ISO 1133:2011 at 230 °C of 0.5 to 120, preferably 0.5 to 80, more preferably 5.0 to 80, even more preferably 3 to 45 dg / min is obtained.

9. The process according to anyone of the preceding claims, wherein the polypropylene composition has a cold xylene soluble content (CXS) in the range of 8 to 29 wt.-%, preferably 10 to 28 wt.-%, more preferably 11 to 22 wt.-%, even more preferably 11 to 16 wt.-%, wherein the cold xylene soluble content (CXS) is measured by the method described in the "CRYSTEX method for heterophasic propylene copolymers" section of the Test Methods section of the specification.

10. The process according to any one of the preceding claims, wherein the propylene homopolymer matrix prior to any visbreaking step has a. at least 96% by weight, preferably at least 97% by weight, of the pentad isotacticity, wherein the use 13 C NMR to determine the isotacticity of the pentad, and / or b. Melt flow rate (MFR) measured according to ISO 1133-1:2011 using 2.16 kg at 230 ° C in the range of 0.5 to 95, preferably 0.5 to 85, more preferably 5 to 85 dg / min Hopol ).

11. The process according to any one of the preceding claims, wherein the internal donor is 3,3-bis(methoxymethyl)-2,6-dimethylheptane and / or wherein the activating compound is NN-dimethylbenzamide and / or wherein the cocatalyst is preferably selected from the group consisting of trimethylaluminum, triethylaluminum, triisobutylaluminum, trihexylaluminum, diisobutylaluminum hydride, trioctylaluminum, dihexylaluminum hydride and mixtures thereof.

12. The method according to any one of the preceding claims, wherein the external donor comprises or consists of a compound selected from the list comprising: Silicone Compounds, silanes, alkoxysilanes, alkylsilanes, alkylalkoxysilanes and aliphatic / aromatic esters, for example dicyclopentyldimethoxysilane, di-tert-butyldimethoxysilane, methylcyclohexyldimethoxysilane, ethylcyclohexyldimethoxysilane, diphenyldimethoxysilane, diisopropyldimethoxysilane, di-n-propyldimethoxysilane, diisobutyldimethoxysilane, di-n-butyldimethoxysilane, cyclopentyltrimethoxysilane, isopropyltrimethoxysilane, n-propyltrimethoxysilane, n-propyltriethoxysilane, ethyltriethoxysilane, tetramethoxysilane, tetraethoxysilane, cyclopentylpyrrolidinyldimethoxysilane, bis(pyrrolidinyl)-dimethoxysilane, and mixtures thereof, preferably di(isopropyl)dimethoxysilane (DiPDMS).

13. The method according to any of the preceding claims, wherein the external donor further comprises a compound selected from the group consisting of ethyl acetate, ethyl benzoate, ethyl p-ethoxybenzoate, methyl pivalate, isopropyl myristate, di-n-butyl sebacate, (poly)(alkylene glycol) mono- or di-acetates, (poly)(alkylene glycol) mono- or dimyristates, (poly)(alkylene glycol) mono- or di-laurates, (poly)(alkylene glycol) mono- or dioleates, triacetin, mixed glycerides of linoleic acid, oleic acid, palmitic acid and stearic acid, and mixtures thereof.

14. Polypropylene composition obtainable or obtainable by a process according to any one of the preceding claims.

15. A polypropylene composition comprising a heterophasic propylene copolymer, Wherein the heterophasic propylene copolymer consists of: a propylene homopolymer matrix in an amount of 71 to 92 wt.-%, preferably 78 to 89 wt.-%, more preferably 83 to 87 wt.-%, based on the heterophasic propylene copolymer, and - ethylene-propylene copolymer in an amount of 8 to 29 wt.%, preferably 11 to 22 wt.%, more preferably 13 to 17 wt.%, based on the heterophasic propylene copolymer, ● wherein the amount of units derived from ethylene, based on the ethylene-propylene copolymer, is from 40 to 60% by weight, preferably from 42 to 55% by weight, more preferably from 43 to 51% by weight, and The polypropylene composition has • A melt flow rate of 0.5 to 120, preferably 0.5 to 95, more preferably 0.5 to 85, even more preferably 0.5 to 80 dg / min, measured according to ISO 1133:2011 using 2.16 kg at 230°C.

16. An article comprising the polypropylene composition of claim 14 or 15, wherein the amount of the polypropylene composition is at least 95 wt.%, based on the article, and / or wherein the article is prepared by injection molding, and / or wherein the article is a household article, such as a vacuum cleaner housing, household chemicals and paints, or a packaging article, such as a container, a crate, a box, a battery housing, a bucket, a flower pot, a food container / packaging, an ice cream container, a thin wall packaging, a lid and a closure, a healthcare packaging, or a healthcare article, such as a drug delivery article, a laboratory ware, a medical device, a medical diagnostic article, or an automotive interior article, such as a dashboard tray, a door panel, an instrument panel, a dashboard tray, a door covering, a door fixture, an armrest, a pillar covering, a seat covering, a trunk covering, an interior trim, and applications in heating, ventilation, and air conditioning (HVAC) applications.

17. Use of the polypropylene composition according to claim 14 or 15 for preparing an article, wherein the amount of the polypropylene composition is at least 95 wt.%, based on the article, and / or wherein the article is prepared by injection molding, and / or wherein the article is a household article, such as a vacuum cleaner housing, household chemicals and paints, or a packaging article, such as a container, a crate, a box, a battery housing, a bucket, a flower pot, a food container / packaging, an ice cream container, a thin wall packaging, a lid and a closure, a healthcare packaging, or a healthcare article, such as a drug delivery article, a laboratory ware, a medical device, a medical diagnostic article, or an automotive interior article, such as a dashboard tray, a door panel, an instrument panel, a dashboard tray, a door covering, a door fixture, an armrest, a pillar covering, a seat covering, a trunk covering, an interior trim, and applications in heating, ventilation, and air conditioning (HVAC) applications.

18. A method for preparing an article, the method comprising the following steps a. providing a polypropylene composition as described in any one of claims 14 or 15, and b. converting the polypropylene composition into an article, for example by using extrusion or injection molding processes.