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WO1997020889A1 - Compositions de polyolefine et films tubulaires obtenus a partir de celles-ci - Google Patents

Compositions de polyolefine et films tubulaires obtenus a partir de celles-ci Download PDF

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Publication number
WO1997020889A1
WO1997020889A1 PCT/EP1996/005238 EP9605238W WO9720889A1 WO 1997020889 A1 WO1997020889 A1 WO 1997020889A1 EP 9605238 W EP9605238 W EP 9605238W WO 9720889 A1 WO9720889 A1 WO 9720889A1
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WO
WIPO (PCT)
Prior art keywords
weight
fraction
propylene
ethylene
xylene
Prior art date
Application number
PCT/EP1996/005238
Other languages
English (en)
Inventor
Emanuele Burgin
Claude Palate
Pierre Coosemans
Original Assignee
Montell Technology Company B.V.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Montell Technology Company B.V. filed Critical Montell Technology Company B.V.
Priority to AU10663/97A priority Critical patent/AU1066397A/en
Publication of WO1997020889A1 publication Critical patent/WO1997020889A1/fr

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Classifications

    • 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
    • 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
    • C08L23/142—Copolymers of propene at least partially crystalline copolymers of propene with other olefins
    • 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
    • C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
    • 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
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • 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
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Definitions

  • the present invention relates to polyolefin compositions which are particularly suitable for use in the preparation of blown films with improved mechanical properties.
  • the present invention relates to polyolefin compositions comprising: (A) a heterogeneous polyolefin composition itself comprising a fraction (Al) which is insoluble in xylene and a fraction (A2) which is soluble in xylene, and (B) a branched propylene polymer.
  • the present invention moreover relates to a process for the preparation of blown films which have improved mechanical properties, this process comprising the use of the said compositions.
  • a further aspect of the present invention moreover relates to the blown films obtained from the said compositions.
  • the blown films sector constitutes an area of ever-increasing importance in the field of polyolefin films.
  • the reason for this is that the films obtained by blowing have a tubular shape which makes them particularly advantageous in the production of bags for a wide variety of uses (bags for urban refuse, bags used in the storage of industrial materials, for frozen foods, carrier bags, etc.) as the tubular structure enables the number of welding joints required for formation of the bag to be reduced when compared with the use of flat films, with consequent simplification of the process.
  • the versatility of the blown-film technique makes it possible, simply by varying the air-insufflation parameters, to obtain tubular films of various sizes, therefore avoiding having to trim the films down to the appropriate size as is necessary in the technique of extrusion through a flat head.
  • polyethylene understood as LDPE, LLDPE or mixtures thereof, since they are endowed with properties in the molten state which enable films to be obtained with a high level of production efficiency, and in a very wide thickness range, without compromising the stability of the bubble.
  • polyethylene-based films have mechanical properties that are not as good, thereby making it necessary in certain particular applications such as, for example, bags used to store industrial materials, to use quite thick (180 - 200 ⁇ ) tubular films with a consequent increase in costs.
  • (A2) a fraction which is soluble in xylene at room temperature, comprising a substantially linear ethylene copolymer
  • the composition (A) is preferably present in amounts ranging from 70 to 99%, more preferably from 80 to 95%, by weight relative to the total weight of (A) + (B) .
  • the fraction (Al) which is insoluble in xylene preferably comprises a substantially linear propylene homopolymer and/or a substantially linear copolymer of propylene, preferably with ethylene, containing more than 90% by weight of units derived from propylene.
  • the amount of the fraction (Al) is preferably between 40 and 75 parts by weight, more preferably between 50 and 70 parts by weight.
  • the fraction (A2) which is soluble in xylene preferably comprises a copolymer of ethylene with propylene, optionally containing smaller proportions of a diene, containing more than 20% by weight of units derived from ethylene and preferably having an intrinsic viscosity of between 1.5 and 4 dl/g.
  • the amount of fraction (A2) which is soluble in xylene is preferably between 25 and 60, more preferably between 30 and 50, parts by weight.
  • heterogeneous polyolefin compositions examples include USP 4,521,566, EP-A-400,333 and EP-A-472,946, the description of which is incorporated herein by way of reference.
  • a particularly preferred aspect of the invention consists of polyolefin compositions comprising (A) and (B) as described above in which the composition (A) is obtained by mixing: (A') a first heterogeneous polyolefin composition having: (A'l) 75-95% by weight of a fraction which is insoluble in xylene at room temperature, comprising a substantially linear propylene homopolymer or a substantially linear copolymer of propylene with ethylene and/or another ⁇ -olefin CH ⁇ CH 1 , where R 1 is an alkyl radical having from 2 to 10 carbon atoms, this fraction containing more than 85% by weight of units derived from propylene; and (A'2) from 5 to 25% by weight of a fraction which is soluble in xylene at room temperature, comprising a substantially linear amorphous copolymer of ethylene with propylene and/or another ⁇ -olefin CH ⁇ CHR 1 , where R 1 has the meaning described above, this fraction optionally containing smaller
  • the heterogeneous compositions (A') and (A") may be prepared as described above for the composition A. Examples of heterogeneous polyolefin compositions (A') and methods for preparing them are described in USP 4,521,566 already mentioned, while examples of heterogeneous polyolefin compositions (A") and methods for preparing them are described in EP-A-400,333 and EP-A-472,946 already mentioned.
  • the component (B) of the present invention may be any propylene polymer with a branching number of less than 1, preferably of between 0.1 and 0.9, and more preferably of between 0.2 and 0.7. Generally, the said polymers have a melt strength of between 5 and 40 cN, preferably of between 10 and 35 cN and more preferably of between 15 and 30 cN.
  • the branching number (g) of the component (B) of the present invention is defined by the ratio [ ⁇ ] Br / [*?] Lin where [ ⁇ ] Br and [ * ] Lin are, respectively, the intrinsic viscosity (determined in tetrahydronaphthalene (THN) at 135°C) of a branched polymer and of a corresponding linear polymer having the same molecular weight (Mw) .
  • the branched propylene polymer which constitutes the component (B) of the present invention may be prepared by many techniques, starting from the corresponding linear polymers.
  • it may be prepared by subjecting a linear polymer to a process of controlled modification which takes place by means of free radicals generated by peroxide initiators or by means of radiation. Examples of such processes and of the products obtained are described in American patents USP 4,916,198, USP 5,047,446 and USP 5,047,485, the descriptions of which are to be understood as included herein by way of reference.
  • compositions of the present invention may be prepared using technologies known in the art, such as the mechanical mixing of the two components (A) and (B) using high-shear internal mixers of the Banbury type, or by mixing directly in the extruder. If compositions (A') and (A") described above are used, they may be mixed separately to form the polyolefin composition (A) of the present invention. Alternatively, the compositions (A') and (A") and the component B may be mixed together, in a mixer or directly in the extruder, to form the composition (A) + (B) of the present invention.
  • compositions of the present invention are used in the process for the preparation of mono- or multilayer blown films, by which process films having improved mechanical properties are obtained.
  • the said films may be prepared by the processes and with the related equipment generally used in the technique of blown films according to that which is known to those skilled in the art.
  • the compositions according to the invention may contain additives capable of imparting specific properties to the articles which the composition is intended to produce.
  • Additives which may be used are those conventionally used in thermoplastic polymer compositions such as, for example, stabilizers, antioxidants, anti-corrosion agents, antislip agents, antiblocking agents, etc.
  • compositions of the invention may moreover contain inorganic or organic, including polymeric, fillers.
  • the abovementioned additives and fillers may be used in conventional amounts, as is known by those skilled in the art or as may readily be determined by routine tests, generally in amounts up to 5% by weight of the final composition.
  • the optional additives do not modify the weight ranges described for the components of the present invention which are to be understood as relative weight ratios between the components (Al) , (A2), (B) or (A'l), A'2), (A"l) , (A"2) and (B) .
  • the compositions of the present invention are surprisingly processable. Indeed, the compositions A+B allowed an increase in the throughput of the extruder without any problems of bubble instability being encountered, consequently, under the same process conditions, about a 25% improvement in production efficiency was found when compared with that of compositions in which the component B is absent, and essentially in line with the production efficiency obtained using LDPE; in particular, it was seen that, under the same conditions, the ratio between the production efficiency obtained using the compositions of the invention and the production efficiency obtained with LDPE is equal to or greater than 0.9.
  • the blown films obtained with compositions (A)+(B) according to the present invention have improved mechanical properties both with respect to the films obtained from LDPE and with respect to the films obtained from compositions in which component B is absent.
  • the said films have very much greater resistance to deformation (given in the examples as Actual Force which expresses the force required to effect the yield at a given temperature) , both with respect to LDPE films of greater thickness and with respect to films obtained from compositions (A) alone.
  • the films of the invention moreover possess improved properties also in terms of tensile modulus and load at yield.
  • composition of the polymers weight percentage of the various monomers determined by I.R.;
  • Insolubility in xylene 2 g of polymer are dissolved in 250 cm 3 of xylene at 135°C with stirring. After 20 minutes the solution is left to cool with continued stirring until it reaches a temperature of 25°c. After 30 minutes the insoluble polymer precipitated is separated out by filtration. The solvent is removed from the solution by evaporation under a stream of nitrogen and the residue is dried under vacuum at 80°c until the weight remains con ⁇ stant. In this way, the percentage of polymer soluble in xylene at 25°C is calculated and, consequently, the percentage of insoluble polymer is determined;
  • Melt strength The method consists in measuring the resistance of a "thread" of molten polymer, working at a specific drawing speed.
  • the polymer is extruded at 200°C through a circular slot with a diameter of l mm; the polymer is then drawn at a constant acceleration of 0.0012 cm/sec 2 , with the resistance offered being measured using an instrument for measuring the force of the molten material (Rheotens melt tension instrument model 2001 produced by Gottfert) which records the force as a function of drawing.
  • the test is continued to the breaking point and the maximum value measured corresponds to the melt strength.
  • Melt index E ASTM D 1238, condition E;
  • Melt index F (MIF) : ASTM D 1238, condition F;
  • Melt index L ASTM D 1238, condition L;
  • F/E ratio between the Melt Index F and the Melt Index E
  • Elmendorf Tear Strength ASTM D 1922, determined both in the direction of the machine (MD) and in the transverse direction (TD) ;
  • the composition used (pelletized) was made up of 90% of a composition (A) containing: (A'l) about 88% of a fraction which is insoluble in xylene, containing a propylene homopolymer with an isotactic index of greater than 90; (A'2) about 12% of a fraction soluble in xylene, containing an ethylene/propylene copolymer containing about 5% ethylene; (A"l) 35% of a fraction which is insoluble in xylene, containing a propylene/ethylene copolymer containing about 3% ethylene; (A"2) about 65% of a fraction which is soluble in xylene, containing an ethylene/propylene copolymer containing about 30% ethylene;
  • extrusion conditions were as follows: Barrel temp. 190-220°C; head temp. 220°C; blowing ratio 2.5; extruder speed 100 rpm. Slot aperture 1.2 mm.
  • Example 3 A blown film 100 ⁇ m in thickness was produced using the apparatus and the conditions described in Example 1. The same composition as in Example 1 was used (pelletized) , replacing the amount of absent component (B) with composition A". The results of the tests to which the film was subjected are given in Table 1. EXAMPLE 3
  • a blown film 100 ⁇ m in thickness was produced using the apparatus and the conditions described in Example 1.
  • a composition was used (in dry-blend form) containing 96% of composition (A) of Example 1 and 4% of component (B) of Example 1.
  • the results of the tests to which the film was subjected are given in Table 1.
  • Example 5 A blown film 100 ⁇ m in thickness was produced using the apparatus and the conditions described in Example 1. The same composition was used as in Example 1 (in dry-blend form), containing 92% of composition (A) and 8% of component (B) . The results of the tests to which the film was subjected are given in Table 1. EXAMPLE 5
  • a blown film 100 ⁇ m in thickness was produced using the apparatus and the conditions described in Example 1.
  • a composition was used (in dry-blend form) containing 96% of composition (A) of Example 1 and 4% of a component (B) having a branching number of 0.56, a melt strength of 23 cN and a melt index (MIL) of 2 dg/min.
  • MIL melt index
  • a blown film 100 ⁇ m in thickness was produced using the apparatus and the conditions described in Example 1.
  • a composition was used (in dry-blend form) containing 92% of composition (A) of Example 1 and 8% of a component (B) having a branching number of 0.56, a melt strength of 23 cN and a melt index (MIL) of 2 dg/min.
  • the results of the tests to which the film was subjected are given in Table 1.
  • Example 1 A blown film 100 ⁇ m in thickness was produced using the apparatus and the conditions described in Example 1. The same composition as in Example 1 was used (in dry-blend form), replacing the amount of absent component (B) with composition
  • a blown film 100 ⁇ m in thickness was produced using the apparatus and the conditions described in Example 1.
  • the composition used consisted of 90% of a composition (A) containing:
  • (A'l) about 88% of a fraction which is insoluble in xylene, containing a propylene homopolymer with an isotactic index of greater than 90; (A'2) about 12% of a fraction which is soluble in xylene, containing an ethylene/propylene copolymer containing about 5% ethylene; (A"l) * 37% of a fraction which is insoluble in xylene, containing a propylene/ethylene copolymer containing about 3% ethylene; (A"2) about 63% of a fraction which is soluble in xylene, containing an ethylene/propylene copolymer containing about 30% ethylene; where the sum of A'l and A"l is equal to 64 parts by weight and the sum of A'2 and A"2 is equal to 26 parts by weight; and 10% of component (B) comprising a propylene homopolymer with a branching number of 0.56, a melt strength of 23 cN and an MIL of 5 d
  • Example 8 A blown film 100 ⁇ m in thickness was produced using the apparatus and the conditions described in Example l. The same composition was used as in Example 8, replacing the amount of the absent component (B) with the composition A". The results of the test to which the film was subjected are given in Table 1.
  • a film 140 ⁇ m in thickness was obtained using the composition of Example 8 and the apparatus and conditions described in Example 1, but using a blowing ratio of 2.
  • the film thus obtained was subjected to mechanical tests at temperatures of 50 and 75°C to evaluate the behaviour of bags produced from the said film when subjected to filling with hot materials and/or storage at summer temperatures. The results are given in Table 2.
  • a film 140 ⁇ m in thickness was obtained using the composition of Comparative Example 9 and the apparatus and conditions described in Example 1, but using a blowing ratio of 2.
  • the results of the mechanical tests at 50 and 70°C are given in
  • a one-layer film 180 ⁇ m in thickness was obtained using a blend consisting of 80% LDPE and 20% LLDPE modified with 1-butene.
  • a three-layer film 200 ⁇ m in thickness consisting of
  • LDPE/LLDPE/LDPE named as "Hot Filling" and marketed by BONAR was subjected to the mechanical tests at 50 and 70°C as in the above examples. The results are given in Table 2.
  • L/D ratio 30, compression rate >2.5 and a slot aperture of between 0.8 and 1.2 depending on the thickness of the films, which were between 100 and 150 ⁇ m.
  • the maximum production efficiency was calculated based on the maximum speed which could be applied to the extruder without the bubble becoming unstable.

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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)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

Ces compositions de polyoléfine comprennent: A) une composition de polyoléfine hétérogène comportant une fraction (A1) insoluble dans le xylène à température ambiante et une fraction (A2) soluble dans le xylène à température ambiante, et B) un polymère de propylène ramifié. Ces compositions présentent notamment une bonne aptitude à la mise en oeuvre lorsqu'on les utilise dans le procédé de préparation de films tubulaires. De surcroît, les films obtenus à l'aide de ce procédé sont caractérisés par d'excellentes propriétés mécaniques.
PCT/EP1996/005238 1995-12-01 1996-11-27 Compositions de polyolefine et films tubulaires obtenus a partir de celles-ci WO1997020889A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU10663/97A AU1066397A (en) 1995-12-01 1996-11-27 Polyolefin compositions and blown films obtained therefrom

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT95MI002525A IT1277013B1 (it) 1995-12-01 1995-12-01 Composizioni poliolefiniche e film soffiati da esse ottenuti
ITMI95A002525 1995-12-01

Publications (1)

Publication Number Publication Date
WO1997020889A1 true WO1997020889A1 (fr) 1997-06-12

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PCT/EP1996/005238 WO1997020889A1 (fr) 1995-12-01 1996-11-27 Compositions de polyolefine et films tubulaires obtenus a partir de celles-ci

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AU (1) AU1066397A (fr)
CA (1) CA2211392A1 (fr)
IT (1) IT1277013B1 (fr)
WO (1) WO1997020889A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6472473B1 (en) 1999-06-24 2002-10-29 Dow Global Technology Inc. Polyolefin composition with improved impact properties
US6593005B2 (en) 2000-01-24 2003-07-15 Dow Global Technologies Inc. Composition and films thereof
US6776924B2 (en) 2000-05-04 2004-08-17 Dow Global Technologies Inc. Molecular melt and methods for making and using the molecular melt
US6800669B2 (en) 2000-12-22 2004-10-05 Dow Global Technologies Inc. Propylene copolymer foams
US6939919B2 (en) 2000-05-26 2005-09-06 Dow Global Technologies Inc. Polyethylene rich/polypropylene blends and their uses
US9611338B2 (en) 2007-12-18 2017-04-04 Basell Poliolefine Italia S.R.L. Copolymers of propylene with hexene-1 and blown films obtained from them

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4916198A (en) * 1985-01-31 1990-04-10 Himont Incorporated High melt strength, propylene polymer, process for making it, and use thereof
EP0472946A2 (fr) * 1990-08-01 1992-03-04 Montell North America Inc. Composition élastoplastique de polyoléfine
EP0634454A1 (fr) * 1993-07-15 1995-01-18 Montell North America Inc. Composition de polymères oléfiniques irradiés et non-irradiés à brillance réduite
US5409992A (en) * 1994-02-28 1995-04-25 Himont Incorporated Calenderable blends containing broad molecular weight distribution propylene polymer material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4916198A (en) * 1985-01-31 1990-04-10 Himont Incorporated High melt strength, propylene polymer, process for making it, and use thereof
EP0472946A2 (fr) * 1990-08-01 1992-03-04 Montell North America Inc. Composition élastoplastique de polyoléfine
EP0634454A1 (fr) * 1993-07-15 1995-01-18 Montell North America Inc. Composition de polymères oléfiniques irradiés et non-irradiés à brillance réduite
US5409992A (en) * 1994-02-28 1995-04-25 Himont Incorporated Calenderable blends containing broad molecular weight distribution propylene polymer material

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6472473B1 (en) 1999-06-24 2002-10-29 Dow Global Technology Inc. Polyolefin composition with improved impact properties
US6841620B2 (en) 1999-06-24 2005-01-11 Dow Global Technologies Inc. Polyolefin composition with improved impact properties
US6593005B2 (en) 2000-01-24 2003-07-15 Dow Global Technologies Inc. Composition and films thereof
US6776924B2 (en) 2000-05-04 2004-08-17 Dow Global Technologies Inc. Molecular melt and methods for making and using the molecular melt
US7141182B2 (en) 2000-05-04 2006-11-28 Dow Global Technologies Inc. Molecular melt and methods for making and using the molecular melt
US7326361B2 (en) 2000-05-04 2008-02-05 Dow Global Technologies, Inc. Molecular melt and methods for making and using the molecular melt
US7399808B2 (en) 2000-05-04 2008-07-15 Dow Global Technologies Inc. Molecular melt and methods for making and using the molecular melt
US6939919B2 (en) 2000-05-26 2005-09-06 Dow Global Technologies Inc. Polyethylene rich/polypropylene blends and their uses
US6800669B2 (en) 2000-12-22 2004-10-05 Dow Global Technologies Inc. Propylene copolymer foams
US9611338B2 (en) 2007-12-18 2017-04-04 Basell Poliolefine Italia S.R.L. Copolymers of propylene with hexene-1 and blown films obtained from them
US10544271B2 (en) 2007-12-18 2020-01-28 Basell Poliolefine Italia S.R.L. Copolymers of propylene with hexene-1 and blown films obtained from them

Also Published As

Publication number Publication date
CA2211392A1 (fr) 1997-06-12
ITMI952525A1 (it) 1997-06-01
ITMI952525A0 (fr) 1995-12-01
AU1066397A (en) 1997-06-27
IT1277013B1 (it) 1997-11-04

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