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WO2015070360A1 - Composition de polypropylène à résistance aux rayures améliorée et propriétés mécaniques équilibrées - Google Patents

Composition de polypropylène à résistance aux rayures améliorée et propriétés mécaniques équilibrées Download PDF

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Publication number
WO2015070360A1
WO2015070360A1 PCT/CN2013/001383 CN2013001383W WO2015070360A1 WO 2015070360 A1 WO2015070360 A1 WO 2015070360A1 CN 2013001383 W CN2013001383 W CN 2013001383W WO 2015070360 A1 WO2015070360 A1 WO 2015070360A1
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Prior art keywords
polypropylene composition
heco
iso
propylene copolymer
heterophasic propylene
Prior art date
Application number
PCT/CN2013/001383
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English (en)
Inventor
Jianglei ZHU
Weili QIANG
Shih Ping CHEN
Original Assignee
Borouge Compounding Shanghai Co., Ltd.
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Publication date
Application filed by Borouge Compounding Shanghai Co., Ltd. filed Critical Borouge Compounding Shanghai Co., Ltd.
Priority to PCT/CN2013/001383 priority Critical patent/WO2015070360A1/fr
Priority to CN201380080827.1A priority patent/CN105705573B/zh
Publication of WO2015070360A1 publication Critical patent/WO2015070360A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/14—Copolymers of propene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
    • C08F10/04—Monomers containing three or four carbon atoms
    • C08F10/06—Propene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/013—Fillers, pigments or reinforcing additives

Definitions

  • This invention is directed to a polypropylene composition (PP), an article comprising said polypropylene composition (PP) as well as the use of said polypropylene composition for the preparation of a moulded article.
  • polypropylene is the polymer of choice in many applications for which it can be tailored to a diversity of different purposes.
  • One main field of application of polypropylenes is in the automotive industry where a variety of automobile parts like bumpers, door panels, dashboards or door claddings are made of polypropylenes.
  • heterophasic propylene copolymers are very attractive materials in this field as they are able to provide the highly desired combination of mechanical stiffness and good impact behavior.
  • Heterophasic propylene copolymers are well known in the art and comprise a matrix being either a polypropylene homopolymer or a random polypropylene copolymer in which an elastomeric copolymer is dispersed.
  • the polypropylene matrix contains (finely) dispersed inclusions being not part of the matrix and said inclusions contain the elastomer.
  • inclusion indicates that the matrix and the inclusion form different phases within the heterophasic propylene copolymer, said inclusions are for instance visible by high resolution microscopy, like electron microscopy or scanning force microscopy. Even though the polypropylenes already on the market achieve a very good balance between stiffness and impact, even more advanced performance characteristics are required in many cases.
  • fillers to polypropylenes is known to improve stiffness while impact strength may be negatively affected with increasing amounts of inorganic filler material.
  • the general mechanical properties of such polypropylenes like for instance the stiffness of the corresponding materials are insufficient for many industrially important applications.
  • the object of the present invention is to provide a polypropylene composition exhibiting high stiffness and impact strength further combined with good scratch resistance.
  • the specific finding of the present invention is to provide a polypropylene composition (PP) comprising the following components,
  • HECO heterophasic propylene copolymer
  • HDPE high density polyethylene
  • the heterophasic propylene copolymer (HECO) has a) a xylene cold soluble (XCS) fraction measured according to ISO 16152 (25 °C) of from 15.0 to 50.0 wt.-%, based on the total weight of the heterophasic propylene copolymer (HECO), and/or b) an ethylene content of ⁇ 20.0 wt.-%, based on the total weight of the heterophasic propylene copolymer (HECO).
  • XCS xylene cold soluble
  • xylene cold soluble (XCS) fraction of the heterophasic propylene copolymer (HECO) has
  • HECO heterophasic propylene copolymer
  • the polypropylene composition (PP) comprises
  • the propylene homopolymer (homo-PP) has a melt flow rate MFR 2 (230 °C, 2.16 kg) measured according to ISO 1133 of from 5.0 to 48.0 g/lO min.
  • the high density polyethylene has a melt flow rate MFR 2 (190 °C, 2.16 kg) measured according to ISO 1133 of from 5.0 to 20.0 g/10 min.
  • the inorganic filler (F) a) is selected from the group consisting of talc, mica, calcium carbonate, diatomaceous, wollastonite and kaolin,
  • b) has a median particle size ⁇ 3 ⁇ 4 ⁇ of from 0.2 to 10 ⁇ .
  • the polypropylene composition has a melt flow rate MFR 2 (230 °C, 2.16 kg) measured according to ISO 1133 of from 8.0 to 30.0 g/10 min.
  • the polypropylene composition (PP) has a flexural modulus measured according to ISO 178 of at least 1 ,580 MPa.
  • the polypropylene composition (PP) has tensile strength of more than 19 MPa according to ISO 527-2. In another preferred embodiment of the present invention, the polypropylene composition (PP) has elongation@break of at least 70% according to ISO 527-2.
  • the polypropylene composition (PP) has Charpy Notched impact strength of at least 30 kJ/m 2 (23°C) according to ISO 179-1/leA / DIN 53453.
  • the polypropylene composition (PP) has anti-scratch properties defined by a value of not higher than 1.1.
  • the composition comprises additionally a polysiloxane (PS), preferably said polysiloxane (PS)
  • a) is present in an amount of from 1.0 to 4.0 wt.-% based on the total weight of the polypropylene composition (PP),
  • the present invention is directed to an article comprising, preferably consisting of, a polypropylene composition (PP) according to the present invention.
  • the article is a moulded article, preferably an injection moulded article.
  • the present invention is directed to the use of a polypropylene composition (PP) according to the present invention for the preparation of a moulded article, preferably an injection moulded article.
  • PP polypropylene composition
  • the polypropylene composition (PP) according to this invention exhibits excellent scratch resistance while the stiffness and the impact strength of the polypropylenes according to the present invention are also excellent.
  • inventive polypropylene composition (PP) it is to be understood that these preferred embodiments or technical details also refer to the inventive article comprising the polypropylene composition (PP). It should be understood that for the purposes of the present invention, the following terms have the following meanings:
  • heterophenasic indicates that an elastomeric copolymer is (finely) dispersed in a matrix.
  • the elastomeric propylene copolymer forms inclusions in the matrix.
  • the matrix contains (finely) dispersed inclusions being not part of the matrix and said inclusions contain the elastomeric propylene copolymer.
  • inclusion shall preferably indicate that the matrix and the inclusion form different phases within the heterophasic propylene copolymer, said inclusions are for instance visible by high resolution microscopy, like electron microscopy or scanning force microscopy.
  • the final composition is probably of a complex structure.
  • the matrix of the heterophasic propylene copolymer may form a continuous phase being the matrix of the composition wherein the elastomeric copolymers and optional additives form together or individually inclusions dispersed therein.
  • a polypropylene composition (PP) according to this invention comprises a heterophasic propylene copolymer (HECO).
  • HECO heterophasic propylene copolymer
  • the heterophasic propylene copolymer (HECO) ensures a high impact and other basic mechanical property, such as tensile strength and flexural modulus.
  • the heterophasic propylene copolymer (HECO) has a melt flow rate MFR 2 (230 °C, 2.16 kg) measured according to ISO 1133 of from 3.0 to 30.0 g/10 min.
  • the amount of the heterophasic propylene copolymer (HECO) based on the total amount of the polypropylene composition (PP) is in the range of from 40 to 75 wt.-%, preferably 45.0 to 70.0 wt.- %, and more preferably of from 50 to 65 wt.-%.
  • the heterophasic propylene copolymer (HECO) has preferably a melt flow rate MFR 2 (230 °C) in the range of 3.0 to 30.0 g/lOmin, more preferably in the range of 7.0 to 25.0 g/lOmin, still more preferably in the range of 9.0 to 20.0 g/lOmin.
  • the heterophasic propylene copolymer (HECO) according to this invention preferably comprises
  • the propylene content in the heterophasic propylene copolymer (HECO) is 75.0 to 92.0 wt.-%, more preferably 80.0 to 90.0 wt.-%, based on the total heterophasic propylene copolymer (HECO), more preferably based on amount of the polymer components of the heterophasic propylene copolymer (HECO), yet more preferably based on the amount of the matrix (M) and the elastomeric copolymer (E) together.
  • the remaining part constitute the comonomers different from propylene (ethylene and/or C 4 to C 12 a-olefin), preferably constitutes ethylene.
  • heterophasic propylene copolymer comprises comonomers, preferably ethylene and/or C 4 to C 12 a-olefin, more preferably ethylene, in the range of 8.0 to 25.0 wt.-%, still more preferably in the range of 8.0 to equal or below 20.0 wt.-%, yet more preferably in the range of 10.0 to 18.0 wt.- %.
  • a heterophasic propylene copolymer comprises as polymer components only the polypropylene matrix (M) and the elastomeric copolymer (E).
  • the heterophasic propylene copolymer (HECO) may contain further additives but no other polymer in an amount exceeding 5 wt-%, more preferably exceeding 3 wt.-%, like exceeding 1 wt.-%, based on the total heterophasic propylene copolymer (HECO), more preferably based on the polymers present in the heterophasic propylene copolymer (HECO).
  • a heterophasic propylene copolymer as defined in the instant invention contains only a polypropylene matrix (M), an elastomeric copolymer (E) and optionally a polyethylene in amounts as mentioned in this paragraph.
  • the xylene cold insoluble (XCI) fraction of the heterophasic propylene copolymer (HECO) represents the matrix (M) and optionally the polyethylene whereas the xylene cold soluble (XCS) fraction represents the elastomeric part of the heterophasic propylene copolymer (HECO), i.e. the elastomeric copolymer (E).
  • matrix (M) content i.e. the xylene cold insoluble (XCI) content
  • heterophasic propylene copolymer is preferably in the range of 50.0 to 78.0 wt.-%, more preferably in the range of 55.0 to 75.0 wt.-%.
  • the values for the matrix (M) content but not for the xylene cold insoluble (XCI) content may be a bit decreased.
  • the elastomeric copolymer (E) content i.e. the xylene cold soluble (XCS) content
  • the heterophasic propylene copolymer (HECO) is preferably in the range of 15.0 to 50.0 wt.-%, more preferably in the range of 22.0 to 50.0 wt.-%, still more preferably in the range of 25.0 to 45.0 wt.-% and most preferably in the range of 26.0 to 38.0 wt.%.
  • the polypropylene matrix (M) is preferably a random propylene copolymer ( ) or a propylene homopolymer (H), the latter especially preferred.
  • the co-monomer content of the polypropylene matrix (M) is equal or below 1.0 wt.-%, yet more preferably not more than 0.8 wt.-%, still more preferably not more than 0.5 wt.-%, like not more than 0.2 wt.-%.
  • polypropylene matrix (M) is preferably a propylene homopolymer (H).
  • propylene homopolymer used in the instant invention relates to a polypropylene that consists substantially, i.e. of more than 99.7 wt.-%, still more preferably of at least 99.8 wt.-%, of propylene units. In a preferred embodiment only propylene units in the propylene homopolymer are detectable.
  • the random propylene copolymer (R) comprises monomers co-polymerizable with propylene, for example co-monomers such as ethylene and/or C 4 to C 12 a-olefins, in particular ethylene and/or C 4 to C 8 a-olefins, e.g. 1-butene and/or 1-hexene.
  • the random propylene copolymer (R) according to this invention comprises, especially consists of, monomers co-polymerizable with propylene from the group consisting of ethylene, 1-butene and 1-hexene.
  • the random propylene copolymer (R) of this invention comprises - apart from propylene - units derivable from ethylene and/or 1 -butene.
  • the random propylene copolymer (R) comprises units derivable from ethylene and propylene only.
  • the random propylene copolymer (R) has preferably a co- monomer content in the range of more than 0.3 to 1.0 wt.-%, more preferably in the range of more than 0.3 to 0.8 wt.-%, yet more preferably in the range of 0.3 to 0.7 wt.-%.
  • the term "random" indicates that the co-monomers of the random propylene copolymers (R) and (R) are randomly distributed within the propylene copolymers.
  • the term random is understood according to IUPAC (Glossary of basic terms in polymer science; IUPAC recommendations 1996).
  • the heterophasic propylene copolymer as well as its individual components can be produced by blending different polymer types. However, it is preferred that the heterophasic propylene copolymer as well as its individual components (matrix and elastomeric copolymer) are produced in a sequential step process, using reactors in serial configuration and operating at different reaction conditions.
  • the polypropylene matrix (M) of the heterophasic propylene copolymer (HECO) has a moderate melt flow MFR 2 (230 °C).
  • MFR 2 (230 °C) of the polypropylene matrix (M) equates with the melt flow rate MFR 2 (230 °C) of the xylene cold insoluble (XCI) fraction of the heterophasic propylene copolymer (HECO).
  • the xylene cold insoluble (XCI) fraction of the heterophasic propylene copolymer (HECO) has a melt flow rate MFR 2 (230 °C) measured according to ISO 1133 of 30.0 to 150.0 g/lOmin, more preferably of 35.0 to 110 g/lOmin, still more preferably of 40.0 to 100 g/10 min, still more preferably of 50.0 to 90 g/10 min.
  • MFR 2 230 °C
  • the polypropylene matrix (M) is isotactic. Accordingly it is appreciated that the polypropylene matrix (M) has a rather high pentad concentration, i.e.
  • the second component of the heterophasic propylene copolymer (HECO) is the elastomeric copolymer (E).
  • the elastomeric copolymer (E) comprises, preferably consists of, units derivable from (i) propylene and (ii) ethylene and/or at least another C 4 to C 12 a-olefin, like C 4 to C 10 a-olefin, more preferably units derivable from (i) propylene and (ii) ethylene and/or at least another ⁇ -olefin selected form the group consisting of 1-butene, 1-pentene, 1-hexene, 1-heptene and 1-octene.
  • the elastomeric copolymer (E) may additionally contain units derived from a conjugated diene, like butadiene, or a non-conjugated diene, however it is preferred that the elastomeric copolymer (E) consists of units derivable from (i) propylene and (ii) ethylene and/or C 4 to Cj 2 a-olefins only.
  • Suitable non- conjugated dienes include straight-chain and branched-chain acyclic dienes, such as 1,4- hexadiene, 1,5-hexadiene, 1 ,6-octadiene, 5-methyl-l, 4-hexadiene, 3,7-dimethyl-l,6-octadiene, 3,7- dimethyl- 1,7-octadiene, and the mixed isomers of dihydromyrcene and dihydro-ocimene, and single ring alicyclic dienes such as 1 ,4-cyclohexadiene, 1 ,5-cyclooctadiene, 1,5-cyclododecadiene, 4-vinyl cyclohexene, l-allyl-4-isopropylidene cyclohexane, 3-allyl cyclopentene, 4-cyclohexene and 1- isopropenyl-4-(4-butenyl) cyclo
  • the elastomeric copolymer (E) comprises at least units derivable from propylene and ethylene and may comprise other units derivable from a further ⁇ -olefin as defined in the previous paragraph.
  • elastomeric copolymer (E) comprises units only derivable from propylene and ethylene and optionally a conjugated diene, like butadiene, or a non-conjugated diene as defined in the previous paragraph, like 1, 4-hexadiene.
  • EPDM ethylene propylene non-conjugated diene monomer polymer
  • EPR ethylene propylene rubber
  • the content of units derivable from propylene in the elastomeric copolymer (EP) equates with the content of propylene detectable in the xylene cold soluble (XCS) fraction.
  • the propylene detectable in the xylene cold soluble (XCS) fraction ranges from 50.0 to 75.0 wt.-%, more preferably from 55.0 to 70.0 wt.-%, and still more preferably from 58.0 to 67.0 wt%.
  • the elastomeric copolymer (E), i.e. the xylene cold soluble (XCS) fraction comprises from 25.0 to 50.0 wt.-%, more preferably 30.0 to 45.0 wt.-%, and even more preferably 33.0 to 42.0 wt.-% units derivable from ethylene and/or at least another C 4 to C 12 a-olefin.
  • the elastomeric copolymer (E) is an ethylene propylene non-conjugated diene monomer polymer (EPDM) or an ethylene propylene rubber (EPR), the latter especially preferred, with a propylene and/or ethylene content as defined in this paragraph.
  • EPDM ethylene propylene non-conjugated diene monomer polymer
  • EPR ethylene propylene rubber
  • a further preferred requirement of the present invention is that the intrinsic viscosity (IV) of the xylene cold soluble (XCS) fraction of the heterophasic propylene copolymer (HECO) is rather high. Rather high values of intrinsic viscosity (IV) improve the impact strength. Accordingly it is appreciated that the intrinsic viscosity of the xylene cold soluble (XCS) fraction of the heterophasic propylene copolymer (HECO) is above 1.8 dl/g, more preferably at least 2.0 dl/g. On the other hand the intrinsic viscosity (IV) should be not too high otherwise the flowability is decreased.
  • the intrinsic viscosity of the xylene cold soluble (XCS) fraction of the heterophasic propylene copolymer (HECO) is preferably in the range of 2.0 to 4.5 dl/g, more preferably in the range 2.0 to 3.5 dl/g and even more preferably in the range of 2.0 to 2.8 dl/g.
  • One further essential component of the instant polypropylene composition is a propylene homopolymer (homo-PP).
  • the propylene homopolymer (homo-PP) is chemically different from the propylene homopolymer (H) used in the matrix (M) of the heterophasic propylene copolymer (HECO).
  • the polypropylene composition (PP) comprises the propylene homopolymer (homo-PP) in an amount from 5.0 to 40.0 wt.-%, based on the total weight of the composition, contributing to a good stiffness (modulus and strength) of the composition.
  • the propylene composition (PP) comprises the propylene homopolymer (homo-PP) in an amount from 5.0 to 30.0 wt.-%, based on the total weight of the propylene composition (PP).
  • the propylene composition (PP) comprises the propylene homopolymer (homo-PP) in an amount from 7.0 to 20.0 wt.-%, more preferably from 8.0 to 17.0 wt.-%, based on the total weight of the composition. It comes appereant from the wording that the propylene homopolymer (homo-PP) is not a heterophasic system, i.e. a system comprising a crystalline matrix phase in which an elastomeric phase is dispersed. Accordingly, it is preferred that the propylene homopolymer (homo-PP) is monophasic, i.e. in DMTA no multiphase structure can be identified as there exists just one glass transition temperature.
  • the propylene homopolymer preferably has a melting temperature of more than 158 °C, i.e. of more than 158 to 166 °C, more preferably of at least 159 °C, i.e. in the range of 159 to 165 °C, still more preferably in the range of 160 to 164 °C.
  • a further characteristic of the propylene homopolymer is the low amount of misinsertions of propylene within the polymer chain, which indicates that the propylene
  • the homopolymer (homo-PP) is produced in the presence of a Ziegler-Natta catalyst. Accordingly the propylene homopolymer (homo-PP) is preferably featured by low amount of 2,1 erythro regio- defects, i.e. of equal or below 0.4 mol.-%, more preferably of equal or below than 0.2 mol.-%, like of not more than 0.1 mol.-%, determined by C-NMR spectroscopy. In an especially preferred embodiment no 2,1 erythro regio-defects are detectable.
  • the propylene homopolymer preferably has a melt flow rate MFR 2 (230°C) measured according to ISO 1133 in the range of 5.0 to 50g/10min, preferably in the range of 5.0 to
  • the propylene homopolymer (homo-PP) has a melt flow rate MFR 2 (230°C) measured according to ISO 1133 in the range of 5.0 to 25 g/lOmin, more preferably in the range of 7.0 to 20.0 g/lOmin.
  • the propylene homopolymer (homo-PP) has a melt flow rate MFR 2 (230°C) measured according to ISO 1133 in the range of 25.0 to 50 g/lOmin, more preferably in the range of 30.0 to 48.0 g/lOmin, like in the range of 35.0 to 48.0 g/lOmin.
  • the propylene homopolymer (homo-PP) preferably has a melt flow rate MFR 2 (230°C) measured according to ISO 1133 which is at least 5.0 g/lOmin lower, preferably at least 8.0 g/lOmin lower, and even more preferably at least 10.0 g/lOmin lower than the polypropylene matrix (M) of the heterophasic propylene copolymer (HECO).
  • MFR 2 230°C
  • the propylene homopolymer has a relatively high flexural modulus, such as, at least 2,000 MPa, preferably at least 2,050 MPa, so as to impart the composition with a high modulus.
  • the propylene homopolymer (homo-PP) is known in the art and is prepared preferably with a catalyst of Ziegler-Natta.
  • the polypropylene composition (PP) of the instant invention also comprises a high density polyethylene (HDPE) next to the heterophasic propylene copolymer (HECO) and the propylene homopolymer (homo-PP) in order to improve the anti-scratch properties of the surface of the article moulded from the instant polypropylene composition (PP).
  • the high density polyethylene (HDPE) is (chemically) different to the elastomeric propylene copolymer (E) of the heterophasic propylene copolymer (HECO).
  • the high density polyethylene (HDPE) used according to the invention is well known in the art and commercially available.
  • the high density polyethylene preferably has a melt flow rate MFR 2 (190 °C, 2.16 kg) of from 0.2 to 15.0 g/lOmin, preferably from 0.5 to 10.0 g/10 min, more preferably from
  • the high density polyethylene (HDPE) typically has a density of at least 930 kg/m 3 , preferably from 930 to 970 kg/m 3 and more preferably from 940 to 970 kg/m 3 .
  • the polypropylene composition (PP) comprises the high density polyethylene (HDPE) in an amount of from 4.0 to 12.0 wt.-%, based on the total weight of the polypropylene composition (PP).
  • the polypropylene composition (PP) preferably comprises the high density polyethylene (HDPE) in an amount of from 5.0 to 11.0 wt.-%, based on the total weight of the polypropylene composition (PP) or, even more preferably in an amount of 6.0 to 10.0 wt.-%.
  • the polypropylene composition (PP) of the invention may further preferably comprise an anti- scratch agent.
  • An especially preferred anti-scratch agent is a polysiloxane (PS).
  • the polysiloxane (PS) preferably is an ultra-high molecular weight polysiloxane.
  • the weight average molecular weight (Mw) of the polysiloxane (PS), like the polydialkylsiloxane, e.g. polydimethylsiloxane, is preferably of at least 1,000,000 g/mol, preferably 1,200,000 g/mol or even more preferably 1,500,000 g/mol.
  • the polysiloxane (PS) may be used as pure materials or mixed via extrusion with various thermoplastics.
  • the polysiloxane (PS), like the polydialkylsiloxane, e.g. polydimethylsiloxane is provided as a masterbatch and thus is mixed with a polyolefin, such as polyethylene, polypropylene or a combination thereof.
  • the polyolefin is a propylene homopolymer, for instance a propylene homopolymer with a melt flow rate MFR 2 (230°C) in the range of 8 to 18 g/1 Omin.
  • MFR 2 melt flow rate
  • the amount of polysiloxane (PS) present in such masterbatches is at least 25 wt.-%, more preferably 25 to 60 wt.-%, like 40 to 60 wt.-%, still more preferably 45 to 55 wt.-%, like 50 to 52 wt.-%.
  • PS polysiloxane
  • DOW CORNING MB50 series Masterbatches such as DOW CORNING MB50-001, MB50-002, MB50-313, MB50-314 and MB50-321, especially MB50-001, all of which are available from Dow Corning Corporation, Midland, MI.
  • the polypropylene composition (PP) comprises an anti-scratch agent, like a polysiloxane, in an amount of ⁇ 3.0 wt.-%, preferably from 1.0 to 2.5 wt.-% and more preferably in an amount of about 1.0 to 2.0 wt.-%, based on the total weight of the polypropylene composition (PP).
  • an anti-scratch agent like a polysiloxane
  • the polypropylene composition (PP) of the invention preferably comprises inorganic filler (F) in a selected amount. Accordingly, the polypropylene composition (PP) according to the present invention preferably comprises inorganic filler (F) in an amount of from 10.0 to 30.0 wt.-%, based on the total weight of the polypropylene composition
  • the polypropylene composition (PP) according to the present invention preferably comprises inorganic filler (F) in an amount of from 10.0 to 20.0 wt.-%, based on the total weight of the polypropylene composition (PP) while it is even more preferable to have inorganic filler (F) in an amount of 12.0-18.0 wt.-% based on the total weight of the polypropylene composition (PP).
  • the inorganic filler (F) is selected from the group consisting of talc, mica, calcium carbonate, diatomaceous, wollastonite and kaolin.
  • the inorganic filler (F) is talc.
  • the inorganic filler (F) preferably has a median particle size d 50 calculated from the particle size distribution in mass percent and measured by laser diffraction in the range of 0.2 to 10.0 ⁇ , more preferably in the range of 0.3 to 15.0 ⁇ , still more preferably in the range of 0.4 to 10.0 ⁇ .
  • the most preferred median particle size d 50 is in the range of 0.60 to 7.0 ⁇ .
  • the inorganic filler (F) has a specific surface area BET in the range from 1.0 to 50.0 m /g, more preferably in the range from 5.0 to 40.0 m /g, still more preferably in the range from 10.0 to 30.0 m 2 /g and even more preferably in the range of 10.0 to 20.0 m 2 /g.
  • the polypropylene composition (PP) preferably comprises talc as inorganic filler (F).
  • the inorganic filler (F) is present in a specific weight ratio compared to the heterophasic propylene copolymer (HECO) and/or the polypropylene homopolymer (homo-PP) in the polypropylene composition (PP).
  • the weight ratio of heterophasic propylene copolymer (HECO) to the inorganic filler (F) [HECO/F] is from 5.0:1.0 to 1.0:1.0.
  • the weight ratio of heterophasic propylene copolymer (HECO) to the inorganic filler (F) [HECO/F] is from 4.5:1.0 to 2.0:1.0 and more preferably from 4.0:1.0 to 3.0:1.0.
  • the weight ratio of polypropylene homopolymer (homo-PP) to the inorganic filler (F) [homo-PP/F] is from 1.0:1.0 to 1.0:7.0.
  • the weight ratio of polypropylene homopolymer (homo-PP) to the inorganic filler (F) [homo-PP/F] is from 1.0:1.0 to 1.0:6.0, and more preferably from 1.0:1.0 to 1.0:5.0.
  • the weight ratio of heterophasic propylene copolymer (HECO) and polypropylene homopolymer (homo-PP) to the inorganic filler (F) [HECO+homo-PP/F] is below 5.5.
  • the weight ratio of heterophasic propylene copolymer (HECO) and polypropylene homopolymer (homo-PP) to the inorganic filler (F) [HECO+homo-PP/F] is from 5.5:1.0 to 2.0:1.0 and more preferably from 5.0:1.0 to 3.0:1.0.
  • the polypropylene composition (PP) is preferably featured by a high stiffness, i.e. a flexural modulus of at least 1,580 MPa, preferably of at least 1,600 MPa according to ISO 178.
  • the polypropylene composition (PP) has a tensile strength according to ISO 527-2 of > 19 MPa, more preferably of > 20 MPa and most preferably of from 19 to 30 MPa.
  • the polypropylene composition (PP) has an
  • the impact strength should be rather high.
  • the polypropylene composition (PP) is preferably featured by a Charpy Notched impact strength (23 °C) of at least 30 kJ/m , more preferably of at least 35 kJ/m .
  • the polypropylene composition (PP) is preferably featured by a Charpy notched impact strength (23°C) in the range of from 30 to 45 kJ/m 2 or from 35 to 45 kJ/m 2 .
  • the polypropylene composition (PP) preferably has a flexural modulus of at least 1,580 MPa, and/or a Charpy notched impact strength (23°C) of > 30 kJ/m 2 .
  • PP polypropylene composition
  • the polypropylene composition (PP) has a flexural modulus of at least 1600 MPa, and a Charpy notched impact strength (23°C) of at least 35 kJ/m 2 .
  • the polypropylene composition (PP) has anti-scratch properties of not higher than 1.1, preferably not higher than 1.0, and, even more preferably, not higher than 0.7.
  • the polypropylene composition (PP) according to the present invention has flexural modulus of at least 1,580 MPa, Charpy notched impact strength (23°C) of at least 30 KJ/m 2 and anti-scratch properties of not higher than 1.1. More preferably, the polypropylene composition (PP) according to the present invention has flexural modulus of at least 1600 MPa, Charpy notched impact strength (23 °C) of at least 35 KJ/m 2 and anti- scratch properties of not higher than 1.0.
  • the polypropylene composition (PP) according to the present invention has flexural modulus of at least 1600 MPa, Charpy notched impact strength (23°C) of at least 35 KJ/m 2 and anti-scratch properties of not higher than 0.7.
  • the polypropylene composition (PP) has a melt flow rate MFR 2 (230 °C, 2.16 kg) measured according to ISO 1133 of from 8.0 to 30.0 g/10 min, more preferably in the range of 8.0 to 25 g/lOmin, like in the range of 9.0 to 23.0 g/lOmin.
  • the instant polypropylene composition (PP) may further comprise at least one typical additives selected from the group consisting of acid scavengers, antioxidants, colorants, pigments, light stabilizers, UV-stabilizers, slip agents, further anti-scratch agents in addition to the essential polysiloxane component, dispersing agents and colorants.
  • the polypropylene composition (PP) further comprises additives such as antioxidants, UV-stabilizers, further anti- scratch agents in addition to the essential polysiloxane component, dispersing agents and colorants.
  • the amount of these additives shall not exceed 10.0 wt.-%, like not more than 7.0 wt.-%, based on the total weight of the polypropylene composition (PP), within the instant polypropylene composition (PP).
  • the polypropylene composition (PP) comprises antioxidants, UV-stabilizers, further anti-scratch agents in addition to the polysiloxane component (PS), dispersing agents and colorants as additives in an amount from 4.0 to 7.0 wt.-% and preferably in an amount from 5.0 to 7.0 wt.-%, based on the total weight of the polypropylene composition (PP).
  • the instant polypropylene composition (PP) contains preferably an a-nucleating agent. Even more preferred the present invention is free of ⁇ -nucleating agents.
  • the nucleating agent is understood as a nucleating agent different to the inorganic filler (F).
  • the nucleating agent is preferably selected from the group consisting of
  • salts of monocarboxylic acids and polycarboxylic acids e.g. sodium benzoate or aluminum tert-butylbenzoate, and
  • dibenzylidenesorbitol e.g. 1,3 : 2,4 dibenzylidenesorbitol
  • dibenzylidenesorbitol derivatives such as methyldibenzylidenesorbitol
  • ethyldibenzylidenesorbitol or dimethyldibenzylidenesorbitol e.g. 1,3 : 2,4
  • salts of diesters of phosphoric acid e.g. sodium 2,2'-methylenebis (4, 6,-di-tert-butylphenyl) phosphate or aluminium-hydroxy-bis[2,2'-methylene-bis(4,6-di-t-butylphenyl)phosphate], and
  • the ⁇ -nucleating agent is part of the heterophasic propylene copolymer (HECO) and thus of the polypropylene composition (PP).
  • the a-nucleating agent content of the heterophasic propylene copolymer (HECO) and thus of the polypropylene composition (PP) is preferably up to 5.0 wt-%.
  • the heterophasic propylene copolymer (HECO) and thus the polypropylene composition (PP) contain(s) not more than 3000 ppm, more preferably of 1 to 2000 ppm of a ⁇ -nucleating agent, in particular selected from the group consisting of dibenzylidenesorbitol (e.g.
  • 1,3 : 2,4 dibenzylidene sorbitol dibenzylidenesorbitol derivative, preferably dimethyldibenzylidenesorbitol (e.g. 1,3 : 2,4 di(methylbenzylidene) sorbitol), or substituted nonitol-derivatives, such as l,2,3,-trideoxy-4,6:5,7-bis-0-[(4-propylphenyl)methylene]- nonitol, vinylcycloalkane polymer, vinylalkane polymer, and mixtures thereof.
  • dimethyldibenzylidenesorbitol e.g. 1,3 : 2,4 di(methylbenzylidene) sorbitol
  • substituted nonitol-derivatives such as l,2,3,-trideoxy-4,6:5,7-bis-0-[(4-propylphenyl)methylene]- nonitol, vinylcycloalkane polymer, vinylalkane polymer
  • heterophasic propylene copolymer HECO
  • polypropylene composition (PP) contains a vinylcycloalkane, like vinylcyclohexane (VCH), polymer and/or vinylalkane polymer, as the a-nucleating agent.
  • the heterophasic propylene copolymer (HECO) contains a vinylcycloalkane, like vinylcyclohexane (VCH), polymer and/or vinylalkane polymer, preferably vinylcyclohexane (VCH).
  • the vinylcycloalkane is vinylcyclohexane (VCH) polymer which is introduced into the heterophasic propylene copolymer (HECO) and thus into the polypropylene composition (PP) by the BNT technology. More preferably in this preferred embodiment, the amount of vinylcycloalkane, like vinylcyclohexane (VCH), polymer and/or vinylalkane polymer, more preferably of
  • vinylcyclohexane (VCH) polymer, in the heterophasic propylene copolymer (HECO) is not more than 500 ppm, more preferably of 1 to 200 ppm, most preferably 5 to 100 ppm, and the amount of vinylcycloalkane, like vinylcyclohexane (VCH), polymer and/or vinylalkane polymer, more preferably of vinylcyclohexane (VCH) polymer, in the heterophasic propylene copolymer (HECO) is not more than 500 ppm, more preferably of 1 to 200 ppm, most preferably 5 to 100 ppm.
  • the polypropylene composition (PP) contains not more than 500 ppm, more preferably of 0.1 to 200 ppm, most preferably 0.2 to 100 ppm, of vinylcycloalkane, like vinylcyclohexane (VCH) polymer.
  • a catalyst system preferably a Ziegler-Natta procatalyst
  • a vinyl compound in the presence of the catalyst system, comprising in particular the special Ziegler-Natta procatalyst, an external donor and a cocatalyst, which vinyl compound has the formula:
  • R 3 and R 4 together form a 5- or 6-membered saturated, unsaturated or aromatic ring or independently represent an alkyl group comprising 1 to 4 carbon atoms
  • the modified catalyst is used for the preparation of the heterophasic polypropylene according to this invention, i.e. of the heterophasic propylene copolymer (HECO).
  • the polymerized vinyl compound acts as an a- nucleating agent.
  • the weight ratio of vinyl compound to solid catalyst component in the modification step of the catalyst is preferably of up to 5 (5:1), preferably up to 3 (3:1) most preferably from 0.5 (1 :2) to 2 (2:1).
  • the most preferred vinyl compound is vinylcyclohexane (VCH).
  • the polypropylene composition (PP) is prepared by blending the heterophasic propylene copolymer (HECO) with the propylene homopolymer (homo-PP), the high density polyethylene (HDPE), the inorganic filler (F), preferably a polysiloxane (PS), optionally including further additives in an extruder, and extruding the obtained blend of the heterophasic propylene copolymer (HECO), the homo-polymeric
  • polypropylene homo-PP
  • high density polyethylene high density polyethylene
  • HDPE high density polyethylene
  • F inorganic filler
  • PS polysiloxane
  • blending refers according to the present invention to the action of providing a blend out of at least two different, pre-existing materials, i.e. the heterophasic propylene copolymer (HECO), the propylene homopolymer (homo-PP), the high density polyethylene (HDPE), the inorganic filler (F), preferably the polysiloxane (PS) and further optional additives.
  • HECO heterophasic propylene copolymer
  • HDPE high density polyethylene
  • PS polysiloxane
  • heterophasic propylene copolymer HECO
  • homo-PP propylene homopolymer
  • HDPE high density polyethylene
  • F inorganic filler
  • PS polysiloxane
  • a Banbury mixer e.g. a Banbury mixer, a 2-roll rubber mill, Buss- co-kneader or a twin screw extruder may be used.
  • the polymer materials recovered from the extruder are usually in the form of pellets. These pellets are then preferably further processed, e.g. by injection moulding to generate articles and products of the inventive composition.
  • the residence time in the blending apparatus or screw speed of the extruder must be chosen such that a sufficiently high degree of homogenisation is achieved.
  • heterophasic propylene copolymer (HECO) is preferably produced in a sequential polymerization process, i.e. in a multistage process known in the art, wherein the corresponding matrix (propylene homopolymer matrix (M)) is produced at least in one slurry reactor and subsequently the elastomeric copolymer (E) is produced in at least one i.e. one or two, gas phase reactor(s).
  • the heterophasic propylene copolymer (HECO) is obtained by producing the propylene homopolymer matrix (M) in at least one reactor system, said system comprises at least one reactor, transferring said propylene homopolymer matrix (M) into a subsequent reactor system, said system comprises at least one reactor, where in the presence of the propylene homopolymer matrix (M) the elastomeric propylene copolymer (E) is produced.
  • each of the polymerization systems can comprise one or more conventional stirred slurry reactors and/or one or more gas phase reactors.
  • the reactors used are selected from the group of loop and gas phase reactors and, in particular, the process employs at least one loop reactor and at least one gas phase reactor. It is also possible to use several reactors of each type, e.g. one loop and two or three gas phase reactors, or two loops and one or two gas phase reactors, in series.
  • the process for the preparation of the heterophasic propylene copolymer comprises also a prepolymerisation with the chosen catalyst system, as described in detail below, comprising the Ziegler-Natta procatalyst, the external donor and the cocatalyst.
  • the prepolymerisation is conducted as bulk slurry polymerization in liquid propylene, i.e. the liquid phase mainly comprises propylene, with minor amount of other reactants and optionally inert components dissolved therein.
  • the prepolymerisation reaction is typically conducted at a temperature of 0 to 50 °C, preferably from 10 to 45 °C, and more preferably from 15 to 40 °C.
  • the pressure in the prepolymerisation reactor is not critical but must be sufficiently high to maintain the reaction mixture in liquid phase.
  • the pressure may be from 20 to 100 bar, for example 30 to 70 bar.
  • the catalyst components are preferably all introduced to the prepolymerisation step. However, where the solid catalyst component (i) and the cocatalyst (ii) can be fed separately it is possible that only a part of the cocatalyst is introduced into the prepolymerisation stage and the remaining part into subsequent polymerisation stages. Also in such cases it is necessary to introduce so much cocatalyst into the prepolymerisation stage that a sufficient polymerisation reaction is obtained therein.
  • hydrogen may be added into the prepolymerisation stage to control the molecular weight of the prepolymer as is known in the art.
  • antistatic additive may be used to prevent the particles from adhering to each other or to the walls of the reactor.
  • a slurry reactor designates any reactor, such as a continuous or simple batch stirred tank reactor or loop reactor, operating in bulk or slurry and in which the polymer forms in particulate form.
  • “Bulk” means a polymerization in reaction medium that comprises at least 60.0 wt.-% monomer.
  • the slurry reactor comprises a bulk loop reactor.
  • Gas phase reactor means any mechanically mixed or fluid bed reactor.
  • the gas phase reactor comprises a mechanically agitated fluid bed reactor with gas velocities of at least 0.2 m/sec.
  • the particularly preferred embodiment for the preparation of the heterophasic propylene copolymer (HECO) of the invention comprises carrying out the polymerization in a process comprising either a combination of one loop and one or two or three gas phase reactors or a combination of two loops and one or two gas phase reactors.
  • a preferred multistage process is a slurry-gas phase process, such as developed by Borealis and known as the Borstar ® technology. In this respect, reference is made to EP 0 887 379 Al, WO 92/12182, WO 2004/000899, WO 2004/111095, WO 99/24478, WO 99/24479 and
  • a further suitable slurry-gas phase process is the Spheripol ® process of Basell.
  • the heterophasic propylene copolymer (HECO) according to this invention are produced by using a special Ziegler-Natta procatalyst in combination with a special external donor, as described below in detail, preferably in the Spheripol ® or in the Borstar ® -PP process.
  • One preferred multistage process may therefore comprise the steps of:
  • the temperature is preferably from 40 to 110 °C, preferably between 50 and 100 °C, in particular between 60 and 90 °C, with a pressure in the range of from 20 to 80 bar, preferably 30 to 60 bar, with the option of adding hydrogen in order to control the molecular weight in a manner known per se.
  • the reaction product of the slurry polymerization which preferably is carried out in a loop reactor, is then transferred to the subsequent gas phase reactor(s), wherein the temperature preferably is within the range of from 50 to 130 °C, more preferably 60 to 100 °C, at a pressure in the range of from 5 to 50 bar, preferably 8 to 35 bar, again with the option of adding hydrogen in order to control the molecular weight in a manner known per se.
  • the average residence time can vary in the reactor zones identified above.
  • the average residence time in the slurry reactor for example a loop reactor, is in the range of from 0.5 to 5 hours, for example 0.5 to 2 hours, while the average residence time in the gas phase reactor generally will be from 1 to 8 hours.
  • the polymerization may be effected in a known manner under supercritical conditions in the slurry, preferably loop reactor, and/or as a condensed mode in the gas phase reactor.
  • the heterophasic polypropylene is preferably obtained by a multistage polymerization process, as described above, in the presence of a catalyst system comprising as component (i) a Ziegler-Natta procatalyst which contains a trans-esterification product of a lower alcohol and a phthalic ester.
  • the procatalyst used according to the invention is prepared by
  • R 1 and R 2 are independently at least a C 5 alkyl
  • step c) optionally reacting the product of step c) with additional TiCl 4.
  • the procatalyst is produced as defined for example in the patent applications WO 87/07620,
  • the adduct which is first melted and then spray crystallized or emulsion solidified, is used as catalyst carrier.
  • dialkylphthalate of formula (I) is a dioctylphthalate (DOP), like di-iso-octylphthalate or diethylhexylphthalate, in particular diethylhexylphthalate,
  • dialkylphthalate of formula (I) to form preferably at least 80 mol-%, more preferably 90 mol-%, most preferably 95 mol.-%, of a dialkylphthalate of formula (II)
  • R 1 and R 2 being methyl or ethyl, preferably ethyl
  • dialkylphthalat of formula (II) being the internal donor
  • the adduct of the formula MgCl2*nROH, wherein R is methyl or ethyl and n is 1 to 6, is in a preferred embodiment melted and then the melt is preferably injected by a gas into a cooled solvent or a cooled gas, whereby the adduct is crystallized into a morphologically advantageous form, as for example described in WO 87/07620.
  • This crystallized adduct is preferably used as the catalyst carrier and reacted to the procatalyst useful in the present invention as described in WO 92/19658 and WO 92/19653.
  • the procatalyst used according to the invention contains 2.5 wt.-% of titanium at the most, preferably 2.2% wt.-% at the most and more preferably 2.0 wt.-% at the most.
  • Its donor content is preferably between 4 to 12 wt.-% and more preferably between 6 and 10 wt.-%.
  • the procatalyst used according to the invention has been produced by using ethanol as the alcohol and dioctylphthalate (DOP) as dialkylphthalate of formula (I), yielding diethyl phthalate (DEP) as the internal donor compound.
  • DOP dioctylphthalate
  • DEP diethyl phthalate
  • the catalyst used according to the invention is the catalyst as described in the example section; especially with the use of dioctylphthalate as dialkylphthalate of formula (I) according to WO 92/19658).
  • the Ziegler-Natta procatalyst can be modified by polymerising a vinyl compound in the presence of the catalyst system, comprising the special Ziegler-Natta procatalyst, an external donor and a cocatalyst, which vinyl compound has the formula:
  • R 3 and R 4 together form a 5- or 6-membered saturated, unsaturated or aromatic ring or independently represent an alkyl group comprising 1 to 4 carbon atoms
  • the modified catalyst is used for the preparation of the heterophasic polypropylene composition according to this invention.
  • the polymerized vinyl compound can act as an a-nucleating agent. This modification is in particular used for the preparation of the heterophasic polypropylene (HECO).
  • the catalyst system used preferably comprises in addition to the special Ziegler-Natta procatalyst an organometallic cocatalyst as component (ii).
  • the cocatalyst from the group consisting of trialkylaluminium, like triethylaluminium (TEA), dialkyl aluminium chloride and alkyl aluminium sesquichloride.
  • TAA triethylaluminium
  • dialkyl aluminium chloride dialkyl aluminium chloride
  • alkyl aluminium sesquichloride alkyl aluminium sesquichloride.
  • Component (iii) of the catalysts system used is an external donor represented by formula (Ilia) or (Illb).
  • Formula (Ilia) is defined by Formula (Ilia)
  • R 5 represents a branched-alkyl group having 3 to 12 carbon atoms, preferably a branched- alkyl group having 3 to 6 carbon atoms, or a cyclo-alkyl having 4 to 12 carbon atoms, preferably a cyclo-alkyl having 5 to 8 carbon atoms.
  • R 5 is selected from the group consisting of iso-propyl, iso-butyl, iso- pentyl, tert.-butyl, tert.-amyl, neopentyl, cyclopentyl, cyclohexyl, methylcyclopentyl and
  • R x and R y can be the same or different, representing a hydrocarbon group having 1 to 12 carbon atoms.
  • R x and R y are independently selected from the group consisting of linear aliphatic hydrocarbon group having 1 to 12 carbon atoms, branched aliphatic hydrocarbon group having 1 to 12 carbon atoms and cyclic aliphatic hydrocarbon group having 1 to 12 carbon atoms.
  • R x and R y are independently selected from the group consisting of methyl, ethyl, n- propyl, n-butyl, octyl, decanyl, iso-propyl, iso-butyl, iso-pentyl, tert.-butyl, tert.-amyl, neopentyl, cyclopentyl, cyclohexyl, methylcyclopentyl and cycloheptyl.
  • both R x and R y are the same, yet more preferably both R x and R y are an ethyl group.
  • the external donor of formula (Illb) is diethylaminotriethoxysilane .
  • the external donor is of formula (Ilia), like dicyclopentyl dimethoxy silane
  • polypropylene compositions (PP) of the present invention are suitable for a wide range of applications.
  • the instant polypropylene compositions (PP) maintain highly desired mechanical properties, such as excellent stiffness and impact strength, while further exhibiting very good anti-scratch properties.
  • polypropylene composition PP
  • PP polypropylene composition
  • another aspect of the present invention is directed to an article comprising the polypropylene composition (PP) as defined above.
  • the article comprises the polypropylene composition (PP) in an amount of at least 60.0 wt.-%, more preferably at least 80.0 wt.-% and most preferably at least 95.0 wt.-%, based on the total weight of the article.
  • the article consists of the instant polypropylene composition (PP).
  • the article is a moulded article, preferably an injection moulded article.
  • Preferred examples of such injection moulded articles are large parts for applications in the automotive or household industry.
  • the present invention is directed to automotive articles, especially to car interiors and exteriors, like bumpers, body panels, spoilers, dashboards and/or door panels.
  • the present invention is especially directed to automotive articles, especially to car interiors and exteriors, like bumpers, body panels, spoilers, dashboards, door panels and the like, in particular bumpers and/or door panels, comprising at least 60.0 wt.-%, more preferably at least 80.0 wt.-%, yet more preferably at least 95.0 wt.-%, like consisting, of the instant polypropylene composition (PP).
  • PP polypropylene composition
  • composition (PP) as defined above for the preparation of a moulded article. It is preferred that the polypropylene composition (PP) as defined above is used for the preparation of an injection moulded article.
  • the present invention is described in further detail by the examples provided below.
  • NMR nuclear-magnetic resonance
  • Quantitative 13 C ⁇ 1 H ⁇ NMR spectra were recorded in the solution-state using a Bruker Advance III 400 NMR spectrometer operating at 400.15 and 100.62 MHz for 1H and 13 C respectively. All spectra were recorded using a C optimised 10 mm extended temperature probe head at 125°C using nitrogen gas for all pneumatics.
  • Standard single-pulse excitation was employed utilising the NOE and bi-level WALTZ 16 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) transients were acquired per spectra.
  • the tacticity distribution was quantified through integration of the methyl region between 23.6-19.7 ppm correcting for any sites not related 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., Macromolecules 30 (1997) 6251).
  • the isotacticity was determined at the pentad level and reported as the percentage of isotactic pentad (mmmm) sequences with respect to all pentad sequences:
  • the amount of 2,1 erythro regio-defects was quantified using the average integral of the two characteristic methyl sites at 17.7 and 17.2 ppm:
  • the amount of 1 ,2 primary inserted propene was quantified based on the methyl region with correction undertaken for sites included in this region not related to primary insertion and for primary insertion sites excluded from this region:
  • the total amount of propene was quantified as the sum of primary inserted propene and all other present regio-defects:
  • the comonomer fraction was quantified using the method of W-J. Wang and S. Zhu,
  • Macromolecules 2000, 33 1157 through integration of multiple signals across the whole spectral region in the 13 C ⁇ 1 H ⁇ spectra. This method was chosen for its robust nature and ability to account for the presence of regio-defects when needed. Integral regions were slightly adjusted to increase applicability across the whole range of encountered comonomer contents.
  • the mole percent comonomer incorporation was calculated from the mole fraction.
  • the weight percent comonomer incorporation was calculated from the mole fraction.
  • Density is measured according to ISO 1183-1 - method A (2004). Sample preparation is done by compression moulding in accordance with ISO 1872-2:2007.
  • Median particle size dso (Laser diffraction) is calculated from the particle size distribution [mass percent] as determined by laser diffraction (Mastersizer) according to ISO 13320-1.
  • Specific surface area is determined as the BET surface according to DIN 66131/2.
  • the column set was calibrated using universal calibration (according to ISO 16014-2:2003) with at least 15 narrow MWD polystyrene (PS) standards in the range of 0,5 kg/mol to 11 500 kg/mol. Mark Houwink constants for PS, PE and PP used are as described per ASTM D 6474-99. All samples were prepared by dissolving 5.0 - 9.0 mg of polymer in 8 mL (at 160 °C) of stabilized TCB (same as mobile phase) for 2.5 hours for PP or 3 hours for PE at max. 160°C under continuous gentle shaking in the autosampler of the GPC instrument.
  • PS polystyrene
  • MFR 2 (230 °C) is measured according to ISO 1133 (230 °C, 2.16 kg load).
  • MFR 2 (190 °C) is measured according to ISO 1133 (190 °C, 2.16 kg load).
  • Intrinsic viscosity is measured according to DIN ISO 1628/1, October 1999 (in Decalin at 135 °C).
  • DSC is run according to ISO 11357 / part 3 /method C2 in a heat / cool / heat cycle with a scan rate of 10 °C/min in the temperature range of - 30 to +225°C.
  • Flexural Modulus and Flexural strength were determined in 3 -point-bending according to ISO 178 on injection molded specimens of 80 x 10 x 4 mm prepared in accordance with ISO 294-1 : 1996.
  • Charpy impact test The Charpy notched impact strength (Charpy NIS) is measured according to ISO 179-1/leA / DIN 53453 at 23 °C, -20 °C and -30 °C, using injection molded bar test specimens of 80x10x4 mm 3 mm 3 prepared in accordance with ISO 294- 1 : 1996.
  • Izod impact test The notched izod impact strength is measured according to ISO 180 / 1A at 23 °C by using injection moulded test specimens as described in EN ISO 1873-2 (80 x 10 x 4 mm) .
  • the scratch resistance (anti-scratch property) was measured according to the PV 3952 2002 scratch method of Volkswagen AG company on an Erichsen scratching device, with a load of 10N.
  • the resulting value dL is a measure for the scratch resistance, a low dL value corresponding to high scratch resistance; this means that the scratch does not turn white but keeps the original colour of the scratched plaque.
  • dL should be at least lower than 1.5, but values below 1.0 are even more desired.
  • a mechanically conducted scratching prick scratches a cross pattern having a line spacing of about 2 mm into a painted/unpainted plastic surface. Per scratch, it is scratched only once in one direction. Afterwards the color deviation with regard to the unscratched surface is determined by means of a colormeter.
  • Scratch device e.g. electromotive cross hatch cutter, Erichsen, model 430
  • the testing specimen have to be carved out of the components to be tested and should be of such form and size that a flat support on the testing specimen carrier and on the supporting table of the respective spectral photometer is ensured.
  • the testing surface must be plane-parallel to the supporting surface.
  • the surface of the samples must be homogenous and may not show any impurities. The handling should occur with clean and non-greasy hands exclusively.
  • the samples are stored in a standardized climate according to DIN 50 014-23/50-2 for at least 48 h.
  • the testing is accomplished at (23 ⁇ 5) °C.
  • a cross pattern (crosscut test) of at least (40 x 40) mm is created by means of a scratch device.
  • the present invention is illustrated by the following examples.
  • the heterophasic propylene copolymers HECOl and HECO 2 were used for the inventive examples, which were prepared with one slurry loop reactor and three gas phase reactors by the known Borstar ® technology, as disclosed in EP 0 887 379 Al.
  • the catalyst used in the polymerization processes has been produced as follows: First, 0.1 mol of MgCl 2 x 3 EtOH was suspended under inert conditions in 250 ml of decane in a reactor at atmospheric pressure. The solution was cooled to the temperature of -15°C and 300 ml of cold TiCl 4 was added while maintaining the temperature at said level. Then, the temperature of the slurry was increased slowly to 20 °C. At this temperature, 0.02 mol of dioctylphthalate (DOP) was added to the slurry. After the addition of the phthalate, the temperature was raised to 135 °C during 90 minutes and the slurry was allowed to stand for 60 minutes.
  • DOP dioctylphthalate
  • inventive polypropylene compounding compositions based on the recipe as summarized in Tables 2a and 2b are prepared by using a Coperion STS-35 twin-screw extruder (available from Coperion (Nanjing) Corporation, China) with a diameter of 35 mm.
  • the twin-screw extruder runs at an average screw speed of 400 rpm with a temperature profile of zones from 190-235 °C. It has a L/D of 44.
  • the temperature of each zone, throughput and the screw speed of the extruder for preparing the compositions of inventive examples are listed in Tables 3a and 3b.
  • the temperature of each zone, throughput and screw speed of the extruder are initiative parameters, and are set on control panel of the extruder.
  • Melt temperature (temperature of the melt in the die) and torque of the extruder are passive parameters shown on control panel of the extruder.
  • a vacuum bump is located in zone 9 and generates a vacuum of -0.01 MPa inside the extruder.
  • Table 2a Composition recipe for the Inventive Examples (with HECOl):
  • Table 2b Composition recipe for the Inventive Examples (with HEC02):
  • Filler 16 16 16 16 *rest to 100 wt.-% were typical additives, like antioxidants (0.30 wt% of Irganox PS 802 FL and 0.40 wt% of Irganox B225 FF of BASF SE) and UV light stabilizer (0.2 wt% of UV-3808PP5 of Cytec Chemical, USA).
  • Petrochem. Co. (Panjin, Liaoning, China) having a density of 0.95g/cm 3 and a MFR 2 (190 °C, 2.16 kg) of 7.5g/10min.
  • siloxane content is 50%.
  • Zone 1 [°C] 210 210 210 210 210 210 zone2 r°ci 215 215 225 215 225 215 zone 3 [°C] 210 210 220 210 220 210 zone 4 [°C] 215 215 220 210 221 210 zone 5 [°C] 200 200 200 190 195 190 zone 6 [°C] 190 190 200 190 200 190 zone 7 [°C] 195 195 201 195 201 195 zone 8 [°C] 200 200 195 200 195 zone 9 [°C] 205 205 210 205 215 205 zone 10 r°ci 205 205 208 205 205 205 zone 11 r°ci 200 200 197 200 197 200 die [°C] 200 200 210 200 210 200 melt temp.
  • Comparative example 1 is the commercial product "C3322T-2" of Pret Composites Co.Ltd (Shanghai, China), which is a compounding material with a MFR 2 (230 °C, 2.16 kg) of 1 lg/lOmin, comprising: a high crystallization block copolymer of propylene, C2-C8 elastomer copolymer, talc, and balanced additives.
  • C3322T-2 does not contain propylene homopolymer. It can be seen from Table 4 that the compounding compositions of the inventive examples show an excellent stiffness (flexural modulus and tensile strength), especially higher flexural modulus.
  • the compounding compositions show a balance of mechanical properties, in terms of charpy notched (impact strength) and stiffness. Furthermore, elongation@break and MFR are improved in the compositions according to the invention when compared to the material of comparative example 1. In addition, such improvements are achieved without the use of the relatively expensive polyolefin elastomeric component being mandatory in the composition of the comparative composition.
  • dL value (anti-scratch properties) of the compoundings of inventive examples are greatly reduced as compared with the CE1. It means that anti-scratch properties are excellent in the inventive compositions and superior to the anti-scratch characteristics of the comparative material of CE 1. Inventors of the invention believe that the significantly improved anti-scratch property of inventive examples results from not only polysiloxane, but also propylene homopolymer in the compounding material. Homopolymer of propylene improves stiffness of the compounding. A higher stiffness is believed good for gaining a better anti-scratch.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne une composition de polypropylène (PP), un article comprenant ladite composition de polypropylène (PP) ainsi que l'utilisation de ladite composition de polypropylène pour la préparation d'un article moulé.
PCT/CN2013/001383 2013-11-14 2013-11-14 Composition de polypropylène à résistance aux rayures améliorée et propriétés mécaniques équilibrées WO2015070360A1 (fr)

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EP3124537A1 (fr) * 2015-07-31 2017-02-01 Borealis AG Composition de polypropylène à faible volatilite
US9725537B2 (en) 2015-06-05 2017-08-08 Exxonmobil Chemical Patents Inc. High activity catalyst supportation
US9725569B2 (en) 2015-06-05 2017-08-08 Exxonmobil Chemical Patents Inc. Porous propylene polymers
US9738779B2 (en) 2015-06-05 2017-08-22 Exxonmobil Chemical Patents Inc. Heterophasic copolymers and sequential polymerization
WO2017129711A3 (fr) * 2016-01-29 2017-09-08 Borealis Ag Copolymère de propylène hétérophasique à faible clte
US9809664B2 (en) 2015-06-05 2017-11-07 Exxonmobil Chemical Patents Inc. Bimodal propylene polymers and sequential polymerization
US9920176B2 (en) 2015-06-05 2018-03-20 Exxonmobil Chemical Patents Inc. Single site catalyst supportation
EP3303419A4 (fr) * 2015-06-05 2018-06-20 ExxonMobil Chemical Patents Inc. Copolymères hétérophasiques et polymérisation séquentielle
US10077325B2 (en) 2015-06-05 2018-09-18 Exxonmobil Chemical Patents Inc. Silica supports with high aluminoxane loading capability
JP2018533642A (ja) * 2015-11-17 2018-11-15 ボレアリス エージー 自動車内装用の機械的性質のバランスが優れた高流動性ｔｐｏ組成物
US10280240B2 (en) 2016-05-27 2019-05-07 Exxonmobil Chemical Patents Inc. Metallocene catalyst compositions and polymerization process therewith
US10280235B2 (en) 2015-06-05 2019-05-07 Exxonmobil Chemical Patents Inc. Catalyst system containing high surface area supports and sequential polymerization to produce heterophasic polymers
US10280233B2 (en) 2015-06-05 2019-05-07 Exxonmobil Chemical Patents Inc. Catalyst systems and methods of making and using the same
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US10570219B2 (en) 2015-06-05 2020-02-25 Exxonmobil Chemical Patents Inc. Production of heterophasic polymers in gas or slurry phase
US10626261B2 (en) * 2015-01-27 2020-04-21 Borealis Ag Flame retardant polypropylene composition
US10723821B2 (en) 2015-06-05 2020-07-28 Exxonmobil Chemical Patents Inc. Supported metallocene catalyst systems for polymerization
US10759886B2 (en) 2015-06-05 2020-09-01 Exxonmobil Chemical Patents Inc. Single reactor production of polymers in gas or slurry phase
RU2748694C2 (ru) * 2016-07-21 2021-05-28 Омиа Интернэшнл Аг Карбонат кальция в качестве кавитационного агента для биаксиально ориентированных полипропиленовых пленок
US11945926B2 (en) 2018-05-16 2024-04-02 Abu Dhabi Polymers Co. Ltd (Borouge) Llc. Foamed polypropylene composition
EP4372047B1 (fr) 2022-11-16 2024-12-04 Hanwha TotalEnergies Petrochemical Co., Ltd. Composition de résine de polypropylène présentant une excellente résistance aux chocs à basse température et article moulé à partir de celle-ci

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CN114729168A (zh) * 2019-12-05 2022-07-08 博禄塑料（上海）有限公司 具有电磁干扰屏蔽性能的聚烯烃组合物

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US10626261B2 (en) * 2015-01-27 2020-04-21 Borealis Ag Flame retardant polypropylene composition
US10294316B2 (en) 2015-06-05 2019-05-21 Exxonmobil Chemical Patents Inc. Silica supports with high aluminoxane loading capability
US10723821B2 (en) 2015-06-05 2020-07-28 Exxonmobil Chemical Patents Inc. Supported metallocene catalyst systems for polymerization
US9725569B2 (en) 2015-06-05 2017-08-08 Exxonmobil Chemical Patents Inc. Porous propylene polymers
US9738779B2 (en) 2015-06-05 2017-08-22 Exxonmobil Chemical Patents Inc. Heterophasic copolymers and sequential polymerization
US11192961B2 (en) 2015-06-05 2021-12-07 Exxonmobil Chemical Patents Inc. Production of heterophasic polymers in gas or slurry phase
US9809664B2 (en) 2015-06-05 2017-11-07 Exxonmobil Chemical Patents Inc. Bimodal propylene polymers and sequential polymerization
US9920176B2 (en) 2015-06-05 2018-03-20 Exxonmobil Chemical Patents Inc. Single site catalyst supportation
US10329360B2 (en) 2015-06-05 2019-06-25 Exxonmobil Chemical Patents Inc. Catalyst system comprising supported alumoxane and unsupported alumoxane particles
EP3303419A4 (fr) * 2015-06-05 2018-06-20 ExxonMobil Chemical Patents Inc. Copolymères hétérophasiques et polymérisation séquentielle
US10759886B2 (en) 2015-06-05 2020-09-01 Exxonmobil Chemical Patents Inc. Single reactor production of polymers in gas or slurry phase
US10077325B2 (en) 2015-06-05 2018-09-18 Exxonmobil Chemical Patents Inc. Silica supports with high aluminoxane loading capability
US10119016B2 (en) 2015-06-05 2018-11-06 Exxonmobil Chemical Patents Inc. Heterophasic copolymers and sequential polymerization
US10287372B2 (en) 2015-06-05 2019-05-14 Exxonmobil Chemical Patents Inc. Bimodal propylene polymers and sequential polymerization
US10570219B2 (en) 2015-06-05 2020-02-25 Exxonmobil Chemical Patents Inc. Production of heterophasic polymers in gas or slurry phase
US10280235B2 (en) 2015-06-05 2019-05-07 Exxonmobil Chemical Patents Inc. Catalyst system containing high surface area supports and sequential polymerization to produce heterophasic polymers
US10280233B2 (en) 2015-06-05 2019-05-07 Exxonmobil Chemical Patents Inc. Catalyst systems and methods of making and using the same
US9725537B2 (en) 2015-06-05 2017-08-08 Exxonmobil Chemical Patents Inc. High activity catalyst supportation
CN107849319B (zh) * 2015-07-31 2020-02-28 博里利斯股份公司 低efo聚丙烯组合物
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US10358546B2 (en) 2015-07-31 2019-07-23 Borealis Ag Low EFO polypropylene composition
RU2705580C2 (ru) * 2015-07-31 2019-11-08 Бореалис Аг Композиция полипропилена с низкой эмиссией и слабовыраженным запахом
WO2017021257A1 (fr) * 2015-07-31 2017-02-09 Borealis Ag Composition de polypropylène à efo bas
EP3124537A1 (fr) * 2015-07-31 2017-02-01 Borealis AG Composition de polypropylène à faible volatilite
US10472509B2 (en) 2015-11-17 2019-11-12 Borealis Ag High flow TPO composition with excellent balance in mechanical properties for automotive interior
JP2018533642A (ja) * 2015-11-17 2018-11-15 ボレアリス エージー 自動車内装用の機械的性質のバランスが優れた高流動性ｔｐｏ組成物
CN108495867A (zh) * 2016-01-29 2018-09-04 博里利斯股份公司 具有低clte的多相丙烯共聚物
CN108495867B (zh) * 2016-01-29 2020-08-25 博里利斯股份公司 具有低clte的多相丙烯共聚物
US11053379B2 (en) 2016-01-29 2021-07-06 Borealis Ag Heterophasic propylene copolymer with low CLTE
WO2017129711A3 (fr) * 2016-01-29 2017-09-08 Borealis Ag Copolymère de propylène hétérophasique à faible clte
US10280240B2 (en) 2016-05-27 2019-05-07 Exxonmobil Chemical Patents Inc. Metallocene catalyst compositions and polymerization process therewith
US11059918B2 (en) 2016-05-27 2021-07-13 Exxonmobil Chemical Patents Inc. Metallocene catalyst compositions and polymerization process therewith
US11492425B2 (en) 2016-05-27 2022-11-08 Exxonmobil Chemical Patents Inc. Metallocene catalyst compositions and polymerization process therewith
RU2748694C2 (ru) * 2016-07-21 2021-05-28 Омиа Интернэшнл Аг Карбонат кальция в качестве кавитационного агента для биаксиально ориентированных полипропиленовых пленок
US11746196B2 (en) 2016-07-21 2023-09-05 Omya International Ag Calcium carbonate as cavitation agent for biaxially oriented polypropylene films
US11945926B2 (en) 2018-05-16 2024-04-02 Abu Dhabi Polymers Co. Ltd (Borouge) Llc. Foamed polypropylene composition
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