WO2016200335A1 - Article moulé à partir d'une composition de polypropylène - Google Patents

Article moulé à partir d'une composition de polypropylène Download PDF

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Publication number
WO2016200335A1
WO2016200335A1 PCT/SG2016/050262 SG2016050262W WO2016200335A1 WO 2016200335 A1 WO2016200335 A1 WO 2016200335A1 SG 2016050262 W SG2016050262 W SG 2016050262W WO 2016200335 A1 WO2016200335 A1 WO 2016200335A1
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Prior art keywords
parts
polymer blend
weight
blend composition
bis
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English (en)
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Manickam RAJAKUMARAN
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Polyolefin Company Singapore Pte Ltd
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Polyolefin Company Singapore Pte Ltd
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    • 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
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/14—Peroxides
    • 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
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/10—Applications used for bottles
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/24—Crystallisation aids

Definitions

  • This invention relates to moulded articles with enhanced impact strength prepared using a blended polymer, where the blended polymer comprises a random polypropylene copolymer and/or a random polypropylene terpolymer, an organic peroxide and an elastomeric polymer.
  • This invention also relates to the blended polymer.
  • Polypropylene copolymers either random copolymers or random terpolymers, are widely used in many applications.
  • polypropylene copolymers are not suitable for use in all applications without further modification.
  • a moulded article made using polypropylene has lower impact strength than would normally be desired in certain applications, such as transparent containers.
  • the polypropylene copolymer can be blended with an elastomer, such as an ethylene- based elastomer (though other elastomers may be used).
  • the resulting article has greater impact strength, making it more suited to the applications envisaged.
  • additives may be combined with the blending of the polypropylene copolymer with an elastomer to improve the properties of the polypropylene copolymer further).
  • nucleating agents can be added to enhance mechanical strength and/or a clarifying agent (e.g. a sorbitol) may be added to reduce haze in moulded articles.
  • the clarifying agent may also increase the stiffness (or flexural modulus) of the resulting polymer composition too.
  • Polypropylene heterophasic copolymers comprise a polymer matrix with a dispersed polymer phase (e.g. a copolymer, ethylene, propylene or any C 4 -C 10 ⁇ -olefin phase).
  • Said heterophasic polymer blends may be produced in the reactor during polymerisation, in the extruder or during dry blending.
  • the transparency of the moulded article will be significantly affected.
  • an impact-resistant polypropylene composition that retains transparency upon moulding, while keeping other desirable properties is quite difficult.
  • the inclusion of an elastomeric polymer results in increased haze and reduced stiffness (or flexural modulus) in the moulded article, which are not desired for certain applications (e.g. for syringes and transparent containers).
  • moulded articles made from polypropylene are subjected to sterilisation using radiation.
  • radiation For example, gamma ray radiation generated from a cobalt 60 source, or electron beam radiation generated from an electron gun at high voltage.
  • sterilisation techniques are commonly used in health care industries to provide sterilised articles for use in a clinical setting.
  • articles subjected to radiation sterilisation include syringes and cups or containers designed to contain any form of liquid and solids that must be kept in a sterile environment.
  • the use of radiation as a sterilisation method causes significant degradation of the polymeric materials, resulting in the loss of mechanical properties due to change in molecular weight.
  • this degradation may also cause a change in the colour/transparency of the moulded article as well. It has been noted that the level of degradation in objects made comprising polypropylene following exposure to radiation is higher than objects made using most other plastic materials. Therefore, given that polypropylene provides many desirable properties, there is still need for compositions of polypropylene that retain mechanical strength after irradiation.
  • This invention provides polypropylene compositions that contain a random polypropylene copolymer or terpolymer in combination with an organic peroxide and an elastomeric polymer that show increased falling weight impact strength compared to polypropylene compositions where the organic peroxide is absent.
  • a polymer blend composition comprising:
  • a polymeric component comprising a random polypropylene copolymer or terpolymer having a Tm of from 120°C to 145°C and an elastomeric polymer having a density of from 0.850 to 0.900 g/cm 3 ;
  • the organic peroxide is present in an amount of from 0.001 to 1.0 parts by weight, per 100 parts by weight of the polymeric component (e.g. from 0.005 to 0.5 parts by weight per 100 parts by weight of the polymeric component);
  • the melt flow rate of the polymer blend composition is from 2 to 40 g/10 minutes (e.g. 8 to 39 g/10 minutes);
  • the falling weight impact of the blend at 23°C after moulding into a 1.4 mm sheet is from 4 to 30 J.
  • the random polypropylene copolymer or terpolymer may have a Tm of from 129°C to 144°C (e.g. from 135°C to 144°C).
  • the random polypropylene copolymer may comprise ethylene or a C 4 -C 10 ⁇ -Olefin as a comonomer, or the random polypropylene terpolymer comprises both ethylene and a C 4 -C 10 ⁇ -Olefin as comonomers (e.g. the random polypropylene copolymer or terpolymer is a random polypropylene copolymer containing ethylene).
  • the polymer blend composition may have a melt flow rate of from 20 to 35 g/10 minutes (e.g. 25 to 30 g/10 minutes).
  • the melt flow rate of the polymer blend composition may be from 8 to 40 g/10 minutes (e.g. from 8 to 39 g/10 minutes or from 10 to 40 g/10 minutes, such as 15 to 39 g/10 minutes, more particularly of from 20 to 35 g/10 minutes such as from 25 to 35 g/10 minutes).
  • the elastomeric polymer may have a density of from 0.860 to 0.899 g/cm 3 , such as a density of from 0.870 to 0.899 g/cm 3 (e.g. from 0.880 to 0.899 g/cm 3 or from 0.890 to 0.899 g/cm 3 ).
  • the elastomeric polymer may be a copolymer comprising ethylene and an ⁇ -olefin as comonomers (e.g. ethylene and a C 4 -C 10 ⁇ -olefin as comonomers).
  • the elastomeric copolymer may comprise more than 55 wt% ethylene (e.g. from 55 to 90 wt% (such as from 55 to 85 wt%) ethylene, with the remainder being an ⁇ -olefin).
  • the random polypropylene copolymer or terpolymer may be present in an amount of from 85 wt% to 98 wt% of the polymeric component in the polymer blend composition, and the elastomeric polymer may be present in an amount of from 2 wt% to 15 wt% of the polymeric component in the polymer blend composition (e.g. the random polypropylene copolymer or terpolymer is present in an amount of from 90 wt% to 98 wt% of the polymeric component and the elastomeric polymer is present in an amount of from 2 wt% to 10 wt% of the polymeric component).
  • the organic peroxide may be selected from the group consisting of hydroperoxides, dialkyl peroxides, diacyl peroxides, peroxydicarbonates, peroxyesters, ketone peroxides, peroxyketals, and alkyl peroxy carbonates.
  • the organic peroxide may be a dialkyl peroxide, for example the dialkyl peroxide may be 2,5- bis(£e/t-butylperoxy)-2,5-dimethylhexane:
  • the polymer blend may further comprise a neutralising agent.
  • the neutralising agent may be present in an amount of from 0.001 to 1 parts by weight per 100 parts by weight of the polymeric component (e.g. from 0.01 to 0.10 parts by weight, such as 0.05 parts by weight per 100 parts by weight of the polymeric component).
  • the neutralising agent may be a metal salt of a fatty acid and/or a carbonate mineral (e.g. the neutralising agent may be a metal stearate, such as calcium stearate and/or hydrotalcite).
  • the polymer blend may further comprise an anti-oxidant (when present, the anti-oxidant may be present in an amount of from 0.001 to 1 parts by weight per 100 parts by weight of the polymeric component (e.g. from 0.05 to 0.20, such as from 0.10 to 0.15 parts by weight per 100 parts by weight of the polymeric component)).
  • the anti-oxidant may be a phosphite and/or phosphate.
  • the anti-oxidant may be a tris-(2,4-ditert-butyl phenyl) phosphate and/or bis-( 2,4-ditert-butyl phenyl) pentaerythritol diphosphite.
  • the polymer blend may further comprise a light stabiliser (when present, the light stabiliser may be present in an amount of from 0.001 to 1 parts by weight per 100 parts by weight of the polymeric component (e.g. from 0.05 to 0.15, such as 0.1 parts by weight per 100 parts by weight of the polymeric component)).
  • the light stabiliser may be selected from the group consisting of benzophenones, benzotriazoles, hindered amines, and inorganic light stabilizers.
  • the light stabiliser may be poly-[1 -(2'-hydroxyethyl)-2,2,6,6-tetramethyl-4-hydroxy-piperidyl succinate].
  • the polymer blend may further comprise an ⁇ -nucleating agent (when present, the ⁇ -nucleating agent may be present in an amount of from 0.001 to 1 parts by weight per 100 parts by weight of the polymeric component (e.g. from 0.15 to 0.25 parts by weight per 100 parts by weight of the polymeric component)).
  • the ⁇ - nucleating agent may be a salt of benzoic acid (e.g. a sodium salt), bis-(T-tert butyl- benozate) aluminium hydroxide, a sorbitol and/or a phosphate ester or a sa It/sol vate thereof.
  • the ⁇ -nucleating agent may be one or more selected from the group consisting of the sodium salt of benzoic acid, bis-(T-tert butyl-benozate) aluminium hydroxide, 1 ,3:2,4-bis-(3,4-dimethyl benzylidene) sorbitol, or, more particularly, 1 ,2,3- trideoxy-4,6:5,7-bis-0-[(4-propylphenyl)methylene]-nonitol and the sodium salt of 2,4,8,10- Tetra(tert-butyl)-6-hydroxy-12H-dibenzo[d,g][1 ,3,2]dioxaphosphocin-6-oxide.
  • the polymer blend where the falling weight impact of the blend at 23°C after moulding into a 1.4 mm sheet may be from 4 to 30 J (e.g. from 6.5 to 25 J, such as from 9.0 to 15.0 J). Additionally or alternatively, the polymer blend where the decrease in the falling weight impact of the blend at 23°C after moulding into a 1.4 mm sheet may be less than 25% following exposure to electron beam radiation at 57 KGy. In yet further embodiments, the haze of the polymer blend composition may be less than 20% (e.g. from 10% to 18%), optionally wherein the elastomeric polymer is present in an amount of from 2 wt% to 5 wt% of the polymeric component.
  • the polymer blend composition does not contain an inorganic filler material. In yet further embodiments of the invention that may be mentioned herein, the polymer blend composition does not contain any inorganic material.
  • a process for preparing a polymer blend composition as described in the first aspect of the invention or any of the embodiments thereof in a second aspect of the invention, there is provided a process for preparing a polymer blend composition as described in the first aspect of the invention or any of the embodiments thereof.
  • a moulded article comprising a polymer blend composition as described in the first aspect of the invention or any of the embodiments thereof.
  • the moulded article may have been subjected to irradiation.
  • a process for preparing a moulded article comprising a polymer blend composition as described in the first aspect of the invention or any of the embodiments thereof.
  • the process may further comprise the step of irradiating the moulded article.
  • a kit of parts suitable for preparing the polymer blend composition according to the first aspect of the invention or any of the embodiments thereof said kit comprising:
  • an elastomeric polymer having a density of from 0.850 to 0.900 g/cm 3 e.g.
  • 0.860 to 0.899 g/cm 3 such as from 0.870 to 0.899 g/cm 3 (e.g. from 0.880 to 0.899 g/cm 3 or from 0.890 to 0.899 g/cm 3 )); and
  • the fifth aspect of the invention may comprise component parts described in the first aspect of the invention and embodiments thereof. DESCRIPTION
  • a polymeric component comprising a random polypropylene copolymer or terpolymer having a Tm of from 120°C to 145°C and an elastomeric polymer having a density of from 0.850 to 0.900 g/cm 3 ;
  • the organic peroxide is present in an amount of from 0.001 to 1 parts by weight, per 100 parts by weight of the polymeric component (e.g. from 0.005 to 0.5 parts by weight per 100 parts by weight of the polymeric component), the melt flow rate of the polymer blend composition is from 2 to 40 g/10 minutes (e.g. 8 to 39 g/10 minutes), and the falling weight impact of the blend at 23°C after moulding into a 1.4 mm sheet is from 4 to 30 J.
  • the random polypropylene copolymer or terpolymer may have a Tm (i.e. melting point or crystalline melting temperature) of from 120°C to 145°C.
  • Tm i.e. melting point or crystalline melting temperature
  • the Tm may be from 129°C to 144°C, such as from 135°C to 144°C.
  • a method for measuring the Tm is provided in the examples section below.
  • the random polypropylene copolymer may comprise ethylene or a C 4 -C 10 ⁇ -Olefin as a comonomer.
  • the random polypropylene terpolymer may comprise both ethylene and a C 4 -C 10 ⁇ -Olefin as comonomers.
  • the random polypropylene copolymer or terpolymer that may be mentioned herein is a random polypropylene copolymer containing ethylene.
  • the random polypropylene copolymer or terpolymer may be present in an amount of from 85 wt% to 98 wt% of the polymeric component and the elastomeric polymer may be present in an amount of from 2 wt% to 15 wt% of the polymeric component (e.g. the random polypropylene copolymer or terpolymer may be present in an amount of from 90 wt% to 98 wt% of the polymeric component and the elastomeric polymer may be present in an amount of from 2 wt% to 10 wt% of the polymeric component, such as from 2 wt% to 5 wt%).
  • the random polypropylene copolymer or terpolymer may be present in an amount of from 95 wt% to 98 wt% of the polymeric component and the elastomeric polymer may be present in an amount of from 2 wt% to 5 wt% of the polymeric component.
  • the term “elastomeric polymer” refers to a polymer or polymer blends that may be amorphous above its glass transition temperature (Tg), allowing for flexibility, deformability and that can recover its original state to a large degree following deformation.
  • the elastomeric polymers may be formed with cross-linked polymer chains, wherein the cross-linkages enable an elastomeric polymer object to recover all or substantially all of its original configuration/shape when an applied stress is removed from the object instead of being permanently deformed.
  • the elastomeric polymer may be a low density polyethylene-based material (e.g. a polyethylene polymer).
  • the elastomeric polymer may have a density of from 0.850 to 0.900 g/cm 3 , for example a density of from 0.860 to 0.899 g/cm 3 , or a density of from 0.870 to 0.899 g/cm 3 (e.g. from 0.880 to 0.899 g/cm 3 or from 0.890 to 0.899 g/cm 3 ).
  • Particular embodiments that may be mentioned herein include an elastomeric polymer having a density of from 0.895 to 0.899 g/cm 3 .
  • the elastomeric polymer may be a copolymer comprising ethylene and an ⁇ -olefin as comonomers (e.g. the copolymer may comprise ethylene and a C 4 -C 10 ⁇ -olefin as comonomers).
  • the C 4 -C 10 ⁇ -Olefin comonomers may include, but are not limited to, any suitable C 4 -C 10 ⁇ -Olefin, such as 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1- nonene, 1-decene or any suitable derivatives thereof.
  • the elastomeric polymer is a copolymer (e.g. a copolymer of ethylene and an ⁇ -olefin)
  • the copolymer may comprise more than 55 wt% ethylene, such as more than 65 wt%, more than 70 wt% ethylene, such as 75 wt% ethylene.
  • the elastomeric copolymer may comprise more than 55 wt% ethylene (e.g. from 55 to 90 wt% (such as from 55 to 85 wt%) ethylene, with the remainder being an ⁇ -olefin).
  • Elastomeric polymers that may be mentioned herein are ExcellenTM EUL731-M, ExcellenTM FX CX4008 and ENGAGETM 8407.
  • the polymer blend composition may have a melt flow rate of from 2 to 40 g/10 minutes, such as from 8 to 39 g/10 minutes, more particularly of from 20 to 35 g/10 minutes such as from 25 to 35 g/10 minutes. Additionally or alternatively, the melt flow rate of the polymer blend composition may be from 8 to 40 g/10 minutes (e.g.
  • melt flow rate from 8 to 39 g/10 minutes or from 10 to 40 g/10 minutes, such as from 15 to 39 g/10 minutes, more particularly of from 20 to 35 g/10 minutes such as from 25 to 35 g/10 minutes).
  • melt index i.e. melt index
  • melt flow rate of fractions of a polymer blend composition an alternative molecular weight measurement, such as gel permeation chromatography can be used together with know correlations between molecular weight and melt flow rate to determine the melt flow rate for the polymer blend composition. For an example, see A. Giijsels, Ind. Polym. Process, 9, 252 (1994).
  • the organic peroxide may be present in an amount of from 0.001 to 1.0 parts by weight, per 100 parts by weight of the polymeric component such as from 0.005 to 0.50 parts by weight per 100 parts by weight of the polymeric component. In certain embodiments, the organic peroxide may be present in an amount of from 0.010 to 0.10 parts by weight, per 100 parts by weight of the polymeric component such as from 0.015 to 0.080 parts by weight, per 100 parts by weight of the polymeric component (e.g. from 0.020 to 0.040 parts by weight).
  • the organic peroxide may be selected from one or more of the group consisting of hydroperoxides, dialkyl peroxides, diacyl peroxides, peroxymonocarbonates, peroxydicarbo nates, peroxyesters, ketone peroxides, peroxyketals, and a!kyl peroxy carbonates.
  • Hydroperoxides that may be mentioned herein include, but are not limited to, p-menthane hydroperoxide.
  • Peroxymonocarbonates that may be mentioned herein include, but are not limited to, tert- hexylperoxy isopropyl monocarbonate.
  • Peroxyesters that may be mentioned herein include, but are not limited to, tert-butylperoxy- 3,5,5-trimethyl hexanoate, tert-butyl peroxy laurate, tert-butylperoxyacetate and tert- butylperoxybenzoate.
  • Peroxyketals that may be mentioned herein include, but are not limited to, n-butyl-4,4- bis(tert-peroxy)valerate, 1 ,1-bis(tert-butylperoxy)cyclohexane, 2,2-bis(4,4-di-tert- butylperoxy)cyclohexyl)propane, 1,1-bis(tert-butylperoxy)cyclododecane and di-tert- butylperoxyisophthalate.
  • Diakyl peroxides that may be mentioned herein include, but are not limited to, 2,5-dimethyl- 2,5-di-(benzoylperoxy)hexane, 2,2-bis(tert-butylperoxy)butane, tert-butyl cumyl peroxide, di- tert-butyl peroxide, dicumyl peroxide, ⁇ -a'-bis(tert-butylperoxy-m-isopropyl)benzene, 1,3- bis(tert-butylperoxydiisopropyl)benzene, 2,5-bis(tert-butylperoxy)-2,5-dimethy!hex-3-yne, 2- methyl-2-[(2-methyl-2-propanyl)peroxy]propane, 2-methyl-2-[(2-methyl-2-butanyl)peroxy]butane, ⁇ 2-[(2-methyl-2-propanyl)peroxy]-2-propanyl ⁇ benzene, 1
  • the organic peroxide may include Trigonox 101-20PP and/or
  • the organic peroxide may act as chain transfer agent to influence the molecular viscosity and/or melt flow rate of the polymer blend composition.
  • the molecular weight distribution of the polymer blend composition is narrowed when an organic peroxide is added to the composition, as compared to other conventional chain transfer agents such as hydrogen.
  • the polymer blend composition may also include additives such as, but not limited to, neutralising agents, anti-oxidants, light stabilisers, ⁇ -nucleating agents or any combination thereof.
  • neutralising agents that may be mentioned herein include a metal salt of a fatty acid and/or a carbonate mineral.
  • the neutralising agent may be any metal stearate such as zinc stearate, sodium stearate, calcium stearate, magnesium stearate or any combination thereof.
  • the neutralising agent may be calcium stearate.
  • the neutralising agent may include a carbonate mineral such as hydrotalcite (e.g. magnesium aluminium hydroxy carbonate).
  • the neutralising agent When present in the composition, the neutralising agent may be present in an amount of from 0.001 to 1 parts by weight per 100 parts by weight of the polymeric component (e.g. from 0.01 to 0.10 parts by weight, such as 0.05 parts by weight per 100 parts by weight of the polymeric component).
  • Anti-oxidants that may be mentioned herein includes any suitable phosphite and/or phosphate.
  • the anti-oxidant may include tris-(2,4-ditert-butyl phenyl) phosphate, bis(2,4-di-t-butyl phenyl) pentaerythritol diphosphite, even more particularly IrgafosTM 168.
  • the anti-oxidant may be present in an amount of from 0.001 to 1 parts by weight per 100 parts by weight of the polymeric component (e.g. from 0.05 to 0.20, such as from 0.10 to 0.15 parts by weight per 100 parts by weight of the polymeric component).
  • Light stabilisers that may be mentioned herein include benzophenones, benzotriazoles, hindered amine light stabilisers, and inorganic light stabilizers, or any combination thereof.
  • the light stabiliser may include hindered amine light stabilisers such as poly-[1- (2'-hydroxyethyl)-2,2,6,6-tetramethyl-4-hydroxy-piperidyl succinate], or, more particularly, TinuvinTM 622 LD.
  • the light stabiliser may be present in an amount of from 0.001 to 1 parts by weight per 100 parts by weight of the polymeric component (e.g. from 0.05 to 0.15, such as 0.1 parts by weight per 100 parts by weight of the polymeric component).
  • ⁇ -Nucleating agents that may be mentioned herein include, but are not limited to one or more of a salt of benzoic acid (e.g. a sodium salt), bis-(T-tert butyl-benozate) aluminium hydroxide, a sorbitol and a phosphate ester or a salt/solvate thereof.
  • a salt of benzoic acid e.g. a sodium salt
  • bis-(T-tert butyl-benozate) aluminium hydroxide e.g. a sodium salt
  • sorbitol e.g. sorbitol and a phosphate ester or a salt/solvate thereof.
  • the ⁇ - nucleating agent may be one or more selected from the group consisting of the sodium salt of benzoic acid, bis-(T-tert butyl-benozate) aluminium hydroxide, 1 ,3:2,4-bis-(3,4-dimethyl benzylidene) sorbitol, 1 ,2,3-trideoxy-4,6:5,7-bis-0-[(4-propylphenyl)methylene]-nonitol and the sodium salt of 2,4,8,10-Tetra(tert-butyl)-6-hydroxy-12H-dibenzo[d,g][1 ,3,2]- dioxaphosphocin-6-oxide.
  • the ⁇ -nucleating agent may include MilladTM 3988i, MilladTM NX8000J, ADK STAB NA-21 or any combination thereof.
  • the ⁇ -nucleating agent may be present in an amount of from 0.001 to 1 parts by weight per 100 parts by weight of the polymeric component (e.g. from 0.15 to 0.25 parts by weight per 100 parts by weight of the polymeric component).
  • the polymer blend composition does not contain an inorganic filler material.
  • filler material refers to any material that can be used to increase the bulk of a composition, without reacting with any of the other components within the composition.
  • the polymer blend composition does not contain any inorganic material.
  • inorganic refers to a chemical compound that does not contain any material that can be termed “organic”, that is a compound that comprises carbon and hydrogen atoms, optionally in combination with one or more nitrogen, sulfur, oxygen and phosphorous atoms or salts thereof (e.g. metal salts thereof).
  • the random polypropylene copolymers or terpolymers present in the polymeric component may be produced using a conventional polymerization technique and a conventional catalyst.
  • the conventional catalyst include:
  • a catalyst comprising a solid catalyst component obtained by reacting a magnesium compound with a titanium compound, and an organoaluminium compound;
  • a catalyst comprising a solid catalyst component obtained by reacting a magnesium compound with a titanium compound, an organoaluminium compound, and, optionally, a third component such as an electron donating compound;
  • Catalysts of type (2) may comprise a solid catalyst component comprising magnesium, titanium, and halogen (e.g. TiCI 4 , MgCI 2 ) as essential components (i.e. a heterogeneous Ziegler-Natta catalyst suitable for use in the polymerisation of propylene), an organoaluminium compound (e.g. AI(C 2 H 5 )3), and an electron donating compound may optionally be used.
  • halogen e.g. TiCI 4 , MgCI 2
  • an organoaluminium compound e.g. AI(C 2 H 5 )3
  • an electron donating compound may optionally be used.
  • this type of catalyst include the catalysts disclosed in JP 61-218606 A, JP 61-287904 A, or JP 7-216017 A.
  • Examples of conventional polymerization include: (a) slurry polymerization and solvent polymerization, each using an inactive hydrocarbon solvent;
  • liquid phase-gas phase polymerization in which liquid phase polymerization and gas phase polymerization are conducted continuously.
  • a random polypropylene copolymer or terpolymer formed as a result of polymerization may be heated under reduced pressure at a temperature lower than the temperature at which the polypropylene melts in order to remove the remaining solvent and oligomers generated as by-products of the polymerisation process.
  • Examples of the method of heating under reduced pressure include the methods of drying under reduced pressure disclosed in JP 55- 75410 A and JP 2-80433 A.
  • Random polypropylene copolymers or terpolymers may be combined with any suitable elastomeric polymer to form the polymeric component as described herein.
  • the polymeric component may then be used to produce the polymer blend compositions, as described herein.
  • the polymer blend compositions may be provided as, but not limited to, pellets, granules or sheets.
  • polymer blend compositions can be performed using any suitable technique including, but not limited to, blending the desired components (e.g. polymeric component, organic peroxide and/or additives) in the desired proportions using conventional blending techniques and apparatus, including high speed mixers from Mitsui Mike Machinery Co, Banbury mixer (available from Farrel Corp., Ansonia, Conn.) or laboratory extruders, such as the Polylab Twin Screw Extruder (available from Thermo Electron (Karsruhe), Karsruhe, Germany) which are suitable for preparing small batches of material.
  • the mixing apparatus used may include any suitable tank capacity and/or processing capacity, for example, the mixing apparatus may include a tank capacity of 75 litres and a process capacity of 50 litres.
  • the polymer blend compositions may be prepared using other types of mixing equipment capable of premixing and directly feeding materials into downstream processing apparatus.
  • downstream processing apparatus may include, but is not limited to, an extruder or any suitable polymer manufacturing equipment to produce polymer blend compositions as pellet samples.
  • the desired components may be premixed using a high speed mixer to provide "premixed material".
  • the premixing may be performed for from 10 seconds to 3600 seconds or more specifically, from 20 seconds 1800 seconds, such as 30 seconds.
  • the premixing of desired components may be performed at a speed of from 500 to 3000 rpm, such as from 750 to 2500 rpm or more particularly from 820 rpm to 1640 rpm.
  • the premixed material may be converted into polymer blend composition pellets using other kinds of equipment capable of melting, mixing and extruding the polymer blend compositions. Extruded polymer blend compositions may then be converted into polymer blend composition pellet and/or granule samples using any suitable equipment, for example an underwater pellet cutter or pellet maker. Commercial scale pelletizing extruders may also be used for preparing larger quantities of the blend.
  • the polymer blend compositions disclosed herein may be used to prepare various kinds of moulded articles suitable for different applications.
  • the polymer blend compositions may be used to prepare moulded articles including, but not limited to, automotive components, housings/covers for electrical appliances and packaging for consumer goods.
  • Particular moulded articles that may be mentioned herein relate to articles for use in the healthcare and medical fields (e.g. containers and syringes).
  • the moulded articles may be prepared from the polymer blend compositions by any suitable moulding process.
  • suitable moulding processes include injection moulding, compression moulding, extrusion and extrusion compression moulding.
  • the moulding process may include, but is not limited to, a step of feeding the desired polymer blend composition into any suitable moulding apparatus.
  • the polymer blend composition may be in the form of a polymer blend composition pellet and/or granule samples.
  • the moulding process may also include a step of heating the polymer blend composition in a heating barrel/chamber to produce a polypropylene polymer melt.
  • the step of heating the polymer blend composition to produce a polypropylene polymer melt may be performed at a temperature of from 150°C to 250°C, more particularly, from 175 to 240°C such as from 190 to 235°C.
  • the polypropylene polymer melt may then be fed into a mould (also known as a die) having one or more cavities of any desired shape.
  • the polypropylene polymer melt located within the mould may be solidified using any suitable conditions to produce a moulded article.
  • the polypropylene polymer melt may be solidified by cooling with any suitable fluid (e.g. water or air) to produce the moulded article.
  • the polypropylene polymer melt may also be subjected to high pressures to produce the moulded article. These high pressures may be applied during the step of heating the polymer blend composition in the heating barrel/chamber.
  • Cooling of the injected polymer melt may be performed by subjecting the article to a temperature of from 10°C to 50°C under the clamped force of the injection moulding machine.
  • the moulded article may then be removed from the mould before being optionally subjected to further processing or conditioning.
  • the article may be placed in a separated container such that it does not contact any other plastic materials (e.g. a box of tray made from paper or cardboard) and subjected to irradiation.
  • 2,5-Bis(ferf-butylperoxy)-2,5-dimethylhexane was obtained as LuperoxTM 101 PP20 from Arkema or as Trigonox 101-20PP from Akzo Nobel. Both materials listed provide the organic peroxide mixed with a carrier material (polypropylene) and in a concentration of from 10 wt% to 30 wt%. Unless otherwise stated herein, the peroxide is provided at a concentration of 20 wt%.
  • ExcellenTM EUL731-M (an elastomeric polymer; a copolymer of ethylene and 1-butene) was obtained from Sumitomo Chemical Co Ltd, Japan.
  • ExcellenTM EUL731-M has a melt flow rate of 10 g/10 mins measured at 190°C and a load of 2.16 kg.
  • ExcellenTM EUL731-M has a density of 895 kg /m 3 (0.895 g/cm 3 ).
  • Excel len FX CX4008 (an elastomeric polymer; a copolymer of ethylene and 1-hexene) was obtained from Sumitomo Chemical Co Ltd Japan.
  • ExcellenTM FX CX4008 has a melt flow rate of 8 g/10 mins measured at 190°C and a load of 2.16 kg.
  • ExcellenTM FX CX4008 has a density of 880 kg/m 3 (0.880 g/cm 3 ).
  • ENGAGETM 8407 (an elastomeric polymer; a copolymer of ethylene and 1-octene) was obtained from The Dow Chemical Company.
  • ENGAGETM 8407 has a melt flow rate of 30 g/10 mins measured at 190°C and a load of 2.16 kg.
  • ENGAGETM 8407 has a density of 870 kg/m 3 (0.870 g/cm 3 ).
  • Tris-(2,4-ditert-butyl phenyl) phosphate (an anti-oxidant) was obtained from BASF as IrgafosTM 168.
  • Poly-[1-(2'-hydroxyethyl)-2,2,6,6-tetramethyl-4-hydroxy-piperidyl succinate] (a hindered amine light stabilising agent) was obtained from BASF as TinuvinTM 622 LD.
  • the homopolymers, random copolymers and terpolymers described herein are prepared using a Ziegler-Natta catalyst, using AI(C 2 H 5 ) 3 as a co-catalyst using the liquid phase-gas phase polymerisation technique.
  • a Ziegler-Natta catalyst using AI(C 2 H 5 ) 3 as a co-catalyst using the liquid phase-gas phase polymerisation technique.
  • suitable catalysts are disclosed in JP 61- 218606 A, JP 61-287904 A, or JP 7-216017 A.
  • the polypropylenes were formed as a result of polymerization are heated under reduced pressure at a temperature lower than the temperature at which the polypropylene melts in order to remove the remaining solvent and oligomers generated as by-products of the polymerisation process. Examples of the method used to make the current polypropylenes are disclosed in JP 55-75410 A and JP 2-80433 A. The polypropylenes prepared are listed in Table 1.
  • compositions were prepared using the amounts provided in Table 2.
  • the premixed material was then fed into an extruder to produce pellet samples.
  • a single screw extruder was used (manufactured by Tanabe Plastic Machinery Co.), having the following parameters:
  • the pellets produced in step (a) were converted into a sheet for property measurement by an injection moulding process, wherein the pellets are provided to an injection moulding machine (Model SH100C from Sumitomo Heavy Industries, having a screw diameter of 32 mm) and are formed into a sheet having 1.4 mm thickness through, using a barrel temperature of between 190 to 235°C (inclusive).
  • the resulting sheets were conditioned for at least 12 hours at 23°C and 50% RH before analysis.
  • Orifice Dimension 2.095 mm inner diameter, 8.0 mm length
  • Samples for density testing were prepared by compression moulding. Before subjecting the specimens to compression, the specimen was pre-heated to 150°C and was then subjected to bumping to remove any gas bubbles. Each specimen had the dimensions of 30 mm x 25 mm x 1 mm and was subjected to a moulding temperature of 150°C at a moulding pressure of 50 kg/cm 3 for 5 minutes using Tester Sangyo Co. Ltd, Model: SA-303. The specimen was then subjected to a cooling temperature of 23°C and a cooling pressure of 20 kg/cm 3 for 3 minutes using Tester Sangyo Co. Ltd, Model: SA-302.
  • the specimen was annealed at 100°C for 1 hour in distilled water, after which the specimen was conditioned in a standard laboratory atmosphere (23°C, 50% relative humidity) for 16 hours.
  • the density of the specimens produced by the procedure above were then tested using ASTM D792 - standard test methods for density and specific gravity (relative density) of plastics by displacement, using Test Method A - for testing solid plastics in water.
  • the tests were conducted using equipment from Ohaus Corporation, Model: DV215D (Balance) & 77402-00 (Density Kit).
  • Melting Temperature (Tm) Polymer sample was first compressed into sheet of 0.3 mm or 0.5 mm thickness by using a compressing moulding machine.
  • the moulded sheet or film sample was punched into small circular pieces and a sample of 10.000 ⁇ 0.1 mg was obtained on an accurate mass balance.
  • the melting temperature was measured using a Differential Scanning Calorimeter, where the weighed sample of circular pieces were cur into smaller pieces that better fit into the aluminium sample pan of the equipment.
  • the sample was annealed by rapidly heating it up to 220°C, which temperature was then held for 5 minutes and then the sample was cooled down to 65°C. The sample was then heated from 65°C to 220°C at 20°C/min.
  • the endothermic peak temperature recorded at this step is the Melting Temperature, as reported herein.
  • Circular specimens having a 50 mm diameter were obtained from the sheets obtained in Preparation 2(b) using a circular hand-punch.
  • Haze is measured using a direct-reading haze meter.
  • the measurement and computation principle are given in ASTM D1003.
  • the haze meter is calibrated without the presence of a specimen and the calibration is checked with a haze meter.
  • the polymer samples were compressed into sheet of 0.3 mm thickness using a compressing moulding machine using the parameters below.
  • Ethylene content (wt%) for the compressed sheet was measured using an IR spectrum measurement method described in the Polymer Analysis Hand Book (issued by Asakura Publishing Co. Ltd., 1985) on page 256.
  • the polymer samples were compressed into sheet of 0.3 mm thickness using a compressing moulding machine using the parameters below.
  • Preheating Period 180 seconds Pressure - kg/cm 2 / Moulding time -minutes: 1-50/60, II- 50/30, 111-50/30
  • Cooling pressure 20 kg/cm 2 1-butene content was measured using the IR spectrum measurement method described in Polymer Analysis Handbook (published by Kinokuniya Co., Ltd., 1995) on page 619.
  • CXS The content of components soluble in 20°C xylene
  • a sample of 1 g was dissolved completely in 100 mL of boiling xylene, and then cooled to 20°C and left at rest for 4 hours. Subsequently, the resultant mixture was separated into precipitates and a solution by filtration, and the filtrate was dried at 70°C under reduced pressure, affording a residue. The residue was weighed and the content of components soluble in 20°C xylene (henceforth called CXS) was calculated.
  • Circular specimens of 65 mm diameter with a thickness of 1.4 mm were directly obtained by injecting the materials of Preparation 2(a) into a circular disc mould in an injection moulding machine having a barrel temperature of 190-235°C.
  • the mould was a 2 cavity type mould.
  • the apparatus that is used to test Falling Weight Impact strength is called a Falling Weight Impact tester or Du Pont Type Impact Tester.
  • Specimen Clamping system Pneumatic clamping system Procedure in brief: Each test specimen was placed in a specimen holder and clamped to the falling weight apparatus. The impact head hits the specimen perpendicularly when the load is released. The load rests in a pillar containing a release pin, when the pin is released, the load falls onto the specimen in the specimen holder, the resulting impact may (or may not) break the specimen, which is determined in the manner outlined below.
  • the purpose of the test is to obtain three data points having an approximate breakage rate of 10-30%, 40-60% and 70-90%, respectively for each material. Any minor or major opening in the specimen resulting from impact is treated as a breakage. Both brittle and ductile failures are also considered to be a breakage.
  • Breakage percentage (Number of broken specimen/Number of tested specimen) X100
  • the resulting data represents one data point for the material at one of the breakage ranged of 10-30%, 40-60% and 70-90%.
  • the specimens were irradiated by JISCo (Japan Irradiation Service Co) Japan.
  • the specimens were subjected to cyclical exposure to the electron beam to achieve a desired radiation dose of 57 KGy.
  • Apparatus Cockcroft-Walton type Electron Beam Processing System manufactured by NHV Corporation. Energy of Electron Beam: 5 MeV
  • Example 1 shows that the moulded material shows a falling weight impact that is approximately double that achieved in any of Comparative Examples 1-3.
  • the composition of Example 1 retains its strength even after being subjected to electron beam (EB) irradiation. This is not the case for Comparative Example 1 , where the composition's strength is severely weakened.
  • the compositions of Examples 2 and 3 result in a falling weight impact that is slightly higher than Example 1 , due to the inclusion of a greater amount of elastomeric polymer.
  • Comparative Example 10 shows that removing the elastomeric polymer from the composition significantly reduces the falling weight impact value.

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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 mélange de polymères, qui comprend un constituant polymère comprenant un copolymère ou un terpolymère de polypropylène aléatoire possédant une Tm située dans la plage allant de 120 °C à 145 °C et un polymère élastomère possédant une masse volumique située dans la plage allant de 0,850 à 0,900 g/cm3 ; et un peroxyde organique, ledit peroxyde organique étant présent en une proportion allant de 0,001 à 1 partie en poids, pour 100 parties en poids du constituant polymère (par exemple, de 0,005 à 0,5 partie en poids pour 100 parties en poids du constituant polymère) ; l'indice de fluidité de la composition de mélange de polymères étant de 8 à 40 g/10 minutes (par exemple de 15 à 39 g/10 minutes) ; et la résistance au choc d'une masse tombante du mélange à 23 °C après moulage sous forme de feuille de 1,4 mm étant de 4 à 30 J. L'invention concerne également un procédé de préparation de ladite composition polymère et un kit d'éléments appropriés pour la fabrication de ladite composition.
PCT/SG2016/050262 2015-06-12 2016-06-06 Article moulé à partir d'une composition de polypropylène Ceased WO2016200335A1 (fr)

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GBGB1510293.2A GB201510293D0 (en) 2015-06-12 2015-06-12 Moulded article from polypropylene composition
GB1510293.2 2015-06-12

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WO2016200335A1 true WO2016200335A1 (fr) 2016-12-15

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WO2019043087A1 (fr) 2017-09-01 2019-03-07 Sabic Global Technologies B.V. Composition de polypropylène
JP2019044122A (ja) * 2017-09-06 2019-03-22 サンアロマー株式会社 ポリプロピレン組成物
CN112912434A (zh) * 2018-09-07 2021-06-04 布拉斯科有限公司 Co2排放影响低的聚合物组合物及其制备方法
WO2022136131A1 (fr) 2020-12-21 2022-06-30 Ineos Europe Ag Mélange de polypropylène

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019043087A1 (fr) 2017-09-01 2019-03-07 Sabic Global Technologies B.V. Composition de polypropylène
EP3676327B1 (fr) 2017-09-01 2023-03-15 SABIC Global Technologies B.V. Composition de polypropylène
JP2019044122A (ja) * 2017-09-06 2019-03-22 サンアロマー株式会社 ポリプロピレン組成物
CN112912434A (zh) * 2018-09-07 2021-06-04 布拉斯科有限公司 Co2排放影响低的聚合物组合物及其制备方法
WO2022136131A1 (fr) 2020-12-21 2022-06-30 Ineos Europe Ag Mélange de polypropylène

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