CA2113455C - Pouch for packaging flowable materials - Google Patents

Pouch for packaging flowable materials Download PDF

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Publication number
CA2113455C
CA2113455C CA002113455A CA2113455A CA2113455C CA 2113455 C CA2113455 C CA 2113455C CA 002113455 A CA002113455 A CA 002113455A CA 2113455 A CA2113455 A CA 2113455A CA 2113455 C CA2113455 C CA 2113455C
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CA
Canada
Prior art keywords
ethylene
minutes
less
pouch
melt index
Prior art date
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Expired - Lifetime
Application number
CA002113455A
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French (fr)
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CA2113455A1 (en
Inventor
Daniel J. Falla
Robert S. Elliott
Allen W. Ross
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Dow Chemical Co
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Dow Chemical Co
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Publication of CA2113455A1 publication Critical patent/CA2113455A1/en
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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/32Layered products comprising a layer of synthetic resin comprising polyolefins
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B1/00Layered products having a general shape other than plane
    • B32B1/08Tubular products
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/06Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/18Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/30Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/306Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl acetate or vinyl alcohol (co)polymers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J123/00Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/04Homopolymers or copolymers of ethene
    • C09J123/08Copolymers of ethene
    • C09J123/0807Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
    • C09J123/0815Copolymers of ethene with aliphatic 1-olefins
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/30Properties of the layers or laminate having particular thermal properties
    • B32B2307/31Heat sealable
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2439/00Containers; Receptacles
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/13Hollow or container type article [e.g., tube, vase, etc.]
    • Y10T428/1334Nonself-supporting tubular film or bag [e.g., pouch, envelope, packet, etc.]
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/13Hollow or container type article [e.g., tube, vase, etc.]
    • Y10T428/1334Nonself-supporting tubular film or bag [e.g., pouch, envelope, packet, etc.]
    • Y10T428/1345Single layer [continuous layer]
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/24Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24777Edge feature
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/28Web or sheet containing structurally defined element or component and having an adhesive outermost layer
    • Y10T428/2813Heat or solvent activated or sealable
    • Y10T428/2817Heat sealable
    • Y10T428/2826Synthetic resin or polymer
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/31504Composite [nonstructural laminate]
    • Y10T428/31855Of addition polymer from unsaturated monomers
    • Y10T428/31909Next to second addition polymer from unsaturated monomers
    • Y10T428/31913Monoolefin polymer

Abstract

An environmentally friendly polymer film pouch made from a polyethylene film structure for the packaging of flowable materials, for example milk, including, for example, a pouch made from a multilayer film structure such as a two-layer or a three-layer coextruded film containing at least one layer of ultra low density linear polyethylene, as a seal layer.

Description

2113~~5 POUCH FOR PACKAGING FLOWABLE MATERIALS
This invention relates to a pouch used in consumer packaging made from certain film structures useful for packaging flowable materials, for example liquids such as milk.
U.S. Patent Nos. 4,503,102 and 4,521,437 disclose the preparation of a polyethylene film for use in the manufacture of a disposable pouch for packaging of liquids such as milk. U.S. Patent No. 4,503,102 discloses pouches made from a blend of a linear ethylene copolymer copolymerized from ethylene and an alpha-olefin at the C4 to Coo range and a ethylene-vinyl acetate polymer copolymerized from ethylene and vinyl acetate. The linear polyethylene copolymer has a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.3 to 2.0 g/10 minutes. The ethylene-vinyl acetate polymer has a weight ratio of ethylene to vinyl acetate from 2.2:1 to 24:1 and a melt index of from 0.2 to 10 g/10 minutes. The blend disclosed in U.S. Patent No. 4,503,102 has a weight ratio of linear low density polyethylene to ethylene-vinyl acetate polymer of from 1.2:1 to 4:1. U.S. Patent No. 4,503,102 also discloses laminates having as a sealant film the aforementioned blend.
U.S. Patent No. 4,521,437 describes pouches made from a sealant film which is from SO to 100 parts of a linear copolymer of ethylene and octene-1 having a density of from 0.916 to 0.930 g/cm3 and a melt index of 0.3 to 2.0 g/10 minutes and from 0 to SO parts by weight of at least one polymer selected from the group consisting of a linear copolymer of ethylene and a C4-Coo-alpha-olefin having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.3 to 2.0 g/10 minutes, a high-pressure polyethylene having a density of from 0.916 to 0.924 g/cm3 and a melt index of from 1 to 10 g/10 minutes and blends thereof. The sealant film disclosed in the U.S. Patent No. 4,521,437 is selected on the basis of providing (a) pouches with an M-test val ue substantially smaller, at the same film thickness, than that obtained for pouches made with film of a blend of 85 parts of a linear ethylene/butene-1 copolymer having a density of about 0.919 g/cm3 and a melt index of about 0.75 g/10 minutes and 15 parts of a high pres~cure polyethylene having a density of about 0.918 g/cm3 and a melt index of 8.5 g/10 minutes, or (b) an M(2)-test value of less than about 12 percent, for pouches having a volume of from greater than.l .3 to 5 liters, or (c) an M(1.3)-test value of less than _1_ WO 93/02859 ~ 1 ~. 3 4~'S PCT/US92/06582 about 5 percent for pouches having a volume of from 0.1 to 1.3 liters. The M, M(2) and M(1.3)-tests are defined pouch drop tests in U.S. Patent No. 4,521,437. The pouches may also be made from composite films in which the sealant film forms at least the inner layer.
The polyethylene pouches known in the prior art have some deficiencies. The problems associated with the prior art known films relate to the sealing properties and performance properties of the film for preparing pouches. In particular, prior art films made into pouches have a high incident of "leakers", i.e., seal defects spch as pinholes which develop at or near the seal in which flowable material, for example milk, escapes from the pouch.
Although the seal and performance properties of the prior art films have been satisfactory, there is still a need in the industry for better seal and performance properties in films for manufacture of hermetically sealed pouches containing flowable materials. More particularly, there is a need for improved sealing properties of the film such as hot tack and heat seal initiation temperature in order to improve the processability of the film and to improve pouches made from the films.
For example, the line speed of known packaging equipment used for manufacturing pouches such as form, fill and seal machines, is currently limited by the sealing properties of the film used in the machines. Prior art polyethylene films have high hot tack seal initiation temperatures and a narrow sealing range. Therefore, the speed at which a form, fill and seal machine can produce a pouch is limited and, thus, the number of pouches produced on a form, fill and seal machine is limited. If the heat seal temperature range, where one could obtain strong seals, is broadened, then the speed of a form, fill and seal machine can be increased and, thus, the number of pouches produced can be increased. Until the present invention, many have attempted to broaden the heat seal temperature range of pouch film without success.
It is desired to provide a polyethylene film structure for a pouch container having a broad heat sealing range with performance properties as good or better than the known prior art pouch films.
It is also desired to provide a film structure for a pouch container having a heat seal layer of ultra low density polyethylene such that the film structure has a broader sealing range for pouch conversion and has acceptable physical properties in the finished product.
It is further desired to provide a pouch made from the aforementioned film structures such that the pouch has a reduced failure rate.
One aspect of the present invention is directed to a pouch for the packaging of liquid consumer products, said pouch made from a film structure including at least one layer of an ultra low density polyethylene being a linear ethylene copolymer interpolymerized from ethylene and at least one alpha-olefin in the range of C3-Coo and having (1) a density of less than about 0.915 glcm3, (2) a melt index of less than about 10.0 gJlO minutes and (3) (i) a hot tack or heat seal initiation temperature of less than about 100°C at a force of at least about 1 N/inch (39.4 N/m) or (ii) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at seal bar temperature of about 110°C and at less than about 0.2 seconds using the DTC Hot Tack Strength Method or achieving a heat seal strength of at least 1 lbf/inch 1;175 N/m) at a seal bar temperature of about 110°C and at less than about 0.25 seconds using the DTC Heat Seal Strength Mettuod.
One embodiment of the present invention is a pouch made from a two-layer coextruded film containing an outer layer of linear low density polyethylene and an inner seal layer of the aforementioned ultra low density linear polyethylene.
Another embodiment of the present invention is a pouch made from a three-layer coextruded film containing an outer layer and a core layer of linear low density polyethylene and am inner seal layer of the aforementioned ultra low density linear polyethylene.
Another aspect of the present invention is a process for preparing the aforementioned pouch.
According to one aspect of the present invention there is provided a pouch containing a flowable material, said pouch being made from a film in tubular form and having transversely heat sealed ends, said film being made from a material comprising a film structure comprising (a) from 10 to 100 percent by weight of at least one polymeric seal layer of an ultra low density linear ethylene copolymer interpolymerized from ethylene and at least one alpha-olefin in the range of C3-C10 and having a density of less than about 0.915 g/cm3 and a melt index of less than about 10.0 g/10 minutes (i) a hot tack or heat seal initiation temperature of less than about 1(10°C at a force of at least about 1 N/inch (39.4 N/m) or (ii) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at a seal bar temperature of about 110°C and at least than about 0.2 seconds using the DTC Hot Tack Strength Method or achieving a heat seal strength of at least 1 lbf/inch (175 Nfm) at a seal bar temperature of about 110°C
and at less than about 0.25 seconds using the DTC Heat Seal Strength Method; and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer of ethylene and a C3-C18-alpha-olefin having a density of greater than about 0.916 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes, a high-pressure low density polyethylene having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to lOg/10 minutes and ethylene-vinyl acetate copolymer having a weight ratio of ethylene to vinyl acetate from 2.2:1. to 24:1 and a melt index of from 0.2 to 10 g/10 minutes.
According to a further aspect of the present invention there is~ provided a pouch containing a flowable material, said pouch being made from a multilayer film structure comprising:
(I)(a) from 10 to 100 percent by weight of at least one polymeric seal layer of an ultra low density linear ethylene copolymer interpolymerized from ethylene and at least one alpha-olefin in the range of C3-C10 and having a density -3a-of less than about: 0.915 g/cm3 and a melt index of less than about lO.Og/10 minutes (i) a hot tack or heat seal initiation temperature of less than about 100°C at a force of at least about 1 N/inch (3~~.4 N/m) or (a.i) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at a seal bar temperature of about 110°C and at less than about 0.2 seconds using the DTC Hot Tack Strength Method or achieving a heat seal strength of at least 1 lbf/inch (175 N/m) at a seal bar temperature of about 110°C and at less than about 0.25 seconds using the DTC Heat: Seal Strength Method; and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer of ethylene and a C3-C18-alpha-olefin having a density of greater than about 0.916 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes, a high-pressure low density polyethylene having a density of from 0.916 to 0.930 g/c:m3 and a melt index of from 0.1 to 10 g/10 minutes and ethylene-vinyl acetate copolymer having a weight ratio of ethylene to vinyl acetate from 2.2:1 to 24:1 and a melt index of front 0.2 to 10 g/10 minutes; and (II) at. least one layer of a linear low density ethylene-C3-C18-alpha-olefin copolymer having a density of from 0.916 to 0.935 and a melt index of from 0.1 to 10 g/10 minutes.
According to another aspect of the present invention there is provided a process for preparing a pouch containing a flowable material comprising forming a tubular member having transversely heat-sealed ends, said tubular member being made -3b-from a film structure comprising a film structure for a pouch container comprising (a) from 10 to 100 percent by weight of at least one polymeric seal layer of an ultra low density linear ethylene copolymer interpolymerized from ethylene and at least one alpha-olefin in the range of C3-ClO and having (1) a density of 7.ess than about 0.915 g/cm3, (2) a melt index of less than about: 10.0 g/10 minutes and (3)(i) a hot tack or heat seal initiation temperature of less than about 100°C at a force of at least about 1 N/inch (39.4 N/m) or (ii) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at a seal bar temperature of: about 110°C and at less than about 0.2 seconds using the DTC Heat Seal Tack Strength Method or achieving a heat soeal strength of at least 1 lbf/inch (175 N/m) at a seal bar temperature of about 110°C and at less than about 0.25 seconds using the DTC Heat Seal Strength Method ;
and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer of ethylene and a C3-C18-alpha-olefin having a density of greater than about 0.916 g~/cm3 and a melt index of from 0.1 to 10 g/10 minutes, a high-pressure low density polyethylene having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes and ethylene-vinyl acetate copolymer having a weight ratio of ethylene to vinyl acetate from 2.2:1 to 24:1 and a melt. index of from 0.2 to 10 g/10 minutes.
According to a still further aspect of the present invention there is provided a process for preparing a pouch containing a flowa.ble material comprising forming a tubular member having transversely heat-sealed ends, said tubular B
-3c-member being made from a film structure comprising:
(I)(a) from 10 to 100 percent by weight of at least one polymeric sea7_ layer of an ultra low density linear ethylene copolymer- interpolymerized from ethylene and at least one alpha-olefin in the range of C3-C10 and having a density of less than about: 0.915 g/cm3 and a melt index of less than about 10.0 g/10 minutes and (i) a hot tack of heat seal initiation temperature of less than about 100°C at a force of at least about 1 rf/inch (39.4 N/m) or (ii) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at a seal bar temperature of about 110°C and at less than about 0.2 seconds using the DTC Hot Tack Strength Method or achieving a heat seal strength of apt least 1 lbf/inch (175 N/m) at a seal bar temperature of about 110°C and at less than about 0.25 seconds using the DTC Heat: Seal Strength Method; and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer, of ethylene and a C3-C18-alpha-olefin having a density of greater than about 0.916 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes, a high-pressure low density polyethylene having a density of from 0.916 to 0.930 g/c:m3 and a melt index of from 0.1 to 10 g/10 minutes and ethylene-vinyl acetate copolymer having a weight ratio of ethylene to vinyl acetate from 2.2:1 to 24:1 and a melt index of from 0.2 to 10 g/10 minutes; and (II) at least one layer of a linear low density ethylene-C3-C18-alpha-olefin copolymer having a density of from 0.916 to 0.935 and a melt index of from 0.1 to 10 g/10 minutes.
-3d-According to another aspect of the present invention there is provided a film structure for a pouch container comprising (a) from 10 to 100 percent by weight of at least one polymeric sea7_ layer of an ultra low density linear ethylene copolymer- interpolymerized from ethylene and at least one alpha-olefin in the range of C3-C10 and having (1) a density of less than about 0.915 g/cm3, (2) a melt index of less than about 1(I.0 g/10 minutes and (3)(i) a hot tack or heat seal initiation temperature of less than about 100°C at a force of at least about 1 N/inch (39.4 N/m) or (ii) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at a seal bar temperature of: about 110°C and at less than about 0.2 seconds using the DTC Hot Tack Strength Method or achieving a heat seal strength of at least 1 lbf/inch (175 N/m) at a seal bar temperature of: about 110°C and at less than about 0.25 seconds using the DTC Heat Seal Strength Method; and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer of ethylene and a C3-C18-alphav-olefin having a density of greater than about 0.916 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes, a high-pressure low density polyethylene having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes and ethylene-vinyl acetate copolymer having a weight ratio of ethylene to vinyl acetate from 2.2:1 to 24:1 and a melt. index of from 0.2 to lOg/10 minutes.
It has teen discovered that the film structures for the pouches of the: present invention have a better seal at lower sealing temperatures and shorter dwell times than -3e-currently obtainable with commercially available film. Use of the films for mak~Lng pouches of the present invention in form, fill and seal machines leads to machine speeds higher than currently obtainable with the use of commercially available film.
Figure 7_ shows a perspective view of a pouch package of the present invention.
Figure ~i shows a perspective view of another pouch package of the preaent invention.
Figure ?. shows a partial, enlarged cross-sectional view of the film ectructure of a pouch of the present invention.
Figure 9: shows another partial, enlarged cross-sectional view of another embodiment of the film structure of a pouch of the preaent invention.
Figure ~~ shows yet another partial, enlarged cross-sectional view of another embodiment of the film structure of a pouch of the preaent invention.
Figures 6-8 are graphical illustrations of hot tack strength of various film structures versus temperature.
Figures 9-11 are graphical illustrations of hot tack strength of various film structures versus sealing time.
Figures 12-14 are graphical illustrations of heat seal strength of various film structures versus temperature.
Figures 15-17 are graphical illustrations of heat seal strength of various film structures versus sealing time.
In its broadest scope, the pouch of the present invention, for example as shown in Figures 1 and 2, for -3f-packaging flowablE: materials is manufactured from a monolayer film -3g-,.

211345 , structure of a polymeric seal layer which is a polyethylene film layer, preferably, a polyethylene referred to hereinafter as "ultra low density polyethylene" ("ULDPE"). An example of a commercially available ULDPE is ATTANE° (Trademark of and commercially available from The Dow Chemical Company). The ULDPE of the present invention is generally a linear copolymer of ethylene with at least one a-olefin having from 3 to 10 carbon atoms, for example, the ULDPE may be selected from ethylene-1-propylene, ethylene-1-butene, ethylene-1-pentene, ethylene-4-methyl-1-pentene, ethylene-1-hexene, ethylene-1-heptene, ethylene-1-octene and ethylene-1-decene copolymers, preferably ethylene-1-octene copolymer.
Generally, the polymeric seal layer has a density of less than about 0.915 g/cm3, preferably from 0.89 to 0.915 g/cm3; generally has a melt index of less than about 10 g/10 minutes, preferably from 0.1 to 10 g/10 minutes; more preferably from 0.5 to 5.0 g/10 minutes;
and generally has an indicator of molecular weight distribution (lip/Iz) of less than about 20, preferably from 5 to 20, more preferably from 7 to 20 and even more preferably from 6 to 18.
The thickness of the seal layer may be from at least about 0.1 mil (2.5 microns) and greater, preferably from 0.2 mil (5 microns) to 10 mil (254 microns) and more preferably from 0.4 mil (10 microns) to 5 mil (127 microns).
A surprising feature of the pouch's film structure of the present invention is the film's broad heat sealing range. Generally, the heat sealing range of the film structure can be from 70°C to 140°C and preferably from 75°C to 130°C. It has been found that the seal layer of the present invention has a broader heat seal range than prior art polyethylene film having higher densities. A broad heat sealing range is important to allow for more flexibility in the heat sealing process used for making pouches from the film structure.
Another unexpected feature of the pouch's film structure of the present invention is the film's heat seal strength at low temperatures. Generally, the film structure of the present invention achieves a hot tack strength of at least about 1 Nlinch (39.4 N/m) at a seal bar temperature of about 110°C and at less than about 0.2 seconds using the DTC Hot Tack Strength Method defined hereinbelow or achieves a heat seal strength of at least 1 Ibf/inch (175 N/m) at a seal bar temperature of about 110°C and at less than 0.25 seconds using the DTC
Heal Seal Strength Method defined hereinbelow. The film structure of the present invention also has a hot tack or heat seal initiation temperature of less than about 100°C at a force of at least about 1 N/inch (39.4 N/m). It has been found that a seal made with the seal layer of the present invention has a higher strength at lower sealing temperatures than seals with a prior art polyethylene having higher densities. A high heat seal strength at low temperatures is important to allow conventional packaging equipment such as a vertical form, fill and seal machine to run at faster rates and to produce pouches with fewer leakers.
It is believed that the use of ULDPE in a film structure for pouches of the present invention (1) provides a pouch that can be fabricated at a fast rate through a form, fill and seal machine and (2) provides a pouch package having few leakers, particularly when the pouch of ~11345~
the present invention is compared to pouches made with linear low density polyethylene, low density polyethylene or a combination thereof.
Another embodiment of the present invention includes a pouch made from a blend of (a) from 10 to 101) percent by weight of at least one linear ethylene copolymer interpolymerized from ethylene and at least one alpha-olefin in the range of C3-Cep and having a density of less than about 0.915 g/cm3 and a melt index of less than about 10.0 g/10 minutes, and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer of ethylene and a C3-C~a-alpha-olefin having a density of greater than about 0.916 i~/cm3 and a melt index of from 0.1 to 10 g/10 minutes, a high-pressure low-density polyethylene having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes and an ethylene-vinyl acetate (EVA) copolymer having a weight ratio of ethylene to vinyl acetate from 22:1 to 24:1 and a melt index of from 0.2 to 20 g/10 minutes.
With reference to Figures 3 to 5, the film structure of the pouch of the present invention also includes a multilayer or composite film structure 30, preferably containing the above-described polymeric seal layer being the inner layer of the pouch.
As will be understood by those skilled in the art, the multilayer film structure for the pouch of the present invention may contain various combination of film layers as long as the seal layer forms part of the ultimate film structure. The multilayer film structure for the pouch of the present invention may be a coextruded film, a coated film or a laminated film.
The film structure also includes the seal layer in combination with a barrier film such as polyester, nylon, EVOH, polyvinylidene dichloride (PVDC) such as SARAN°
(Trademark of The Dow Chemical Company) ~~nd metallized films. The end use for the pouch tends to dictate, in a large degree, the selection of the other material or materials used in combination with the seal layer film. The pouches dE~scribed herein will refer to seal layers used at least on the inside of the pouch.
One embodi ment of the film structure 30 for the pouch of the present invention, shown in Figure 3, compri~;es an ultra low density polyethylene seal layer 31 and at least one polymeric outer layer 32. 'The polymeric outer layer 32 is preferably a polyethylene film layer, more preferably a polyethylene referred to hereinafter as "linear low density polyethylene"
("LLDPE"). An example of a commercially available LLDPE is DOWLEX° 2073 (Trademark of and commercially available from The Dow Chemical Company). The LLDPE is generally a linear copolymer of ethylene and a minor amount of an alpha-olefin having from 3 to 18 carbon atoms, preferably from 4 to 10 carbon atoms and most preferably 8 carbon atoms. The LLDPE
for the outer layer 32 general ly has a density of greater than 0.916 g/cm3, more preferably from 0.916 to 0.935 g/cm3, mores preferably from 0.918 to 0.926 g/cm3; generally has a melt index of from 0.1 to 10 g/10 minutes, preferably from 0.5 to 2 g/10 minutes; and generally has an I~o/12 2113.4~~
ratio of from 5 to 20, preferably from 7 to 20. The thickness of the outer layer 32 may be any thickness so long as the seal layer 31 has a minimum thickness of about 0.1 mil (2.5 microns).
Another embodiment of the film structure 30 for the pouch of the present invention, shown in Figure 4, comprises the polymeric layer 32 sandwiched between two polymeric seal layers 31.
Still another embodiment of the film structure 30 for the pouch of the present invention, shown in Figure 5, comprises at least one polymeric core'layer 33 between at least one polymeric outer layer 32 and at least one polymeric seal layer 31. The polymeric layer 33 may be the same LLDPE film layer as the outer layer 32 or preferably a different LLDPE, and more preferably an LLDPE, for example DOWLEX'" 2049 (Trademark of and commercially available from The Dow Chemical Company) that has a higher density than the outer layer 32.
The thickness of the core layer 33 may be any thickness so long as the seal layer 31 has a minimum thickness of about 0.1 mil (2.5 microns).
Yet another embodiment (not shown) of the film structure for the pouch of the present invention can be a structure including a seal layer 31 and another polyethylene film layer referred to hereinafter as "high pressure low-density polyethylene"
("LDPE"). The LDPE
layer generally has a density of from 0.916 to 0.930 g/cm3 and has a melt index of from 0.1 to 10 g/10 minutes. The thickness of the LDPE layer may be any thickness so long as the seal layer 31 has a minimum thickness of about 0.1 mil (2.5 microns).
Still another embodi ment (not shown) of the film structure for the pouch of the present invention can be a structure including a seal layer 31 and a layer of EVA copolymer having a weight ratio of ethylene to vinyl acetate from 22:1 to 24:1 and a melt index of from 0.2 to 20 g/10 minutes. The thickness of the EVA layer may be any thickness so long as the seal layer 31 has a minimum thickness of about 0.1 mil (2.5 microns).
The ultimate film thickness of the final film product used for making the pouch of the present invention is from 0.5 mil (12.7 microns) to 10 mils (254 microns), preferably from 1 mil (25.4 microns) to S mils (127 microns); more preferably from 2 mils (50.8 microns) to 4 mils (100 microns).
Additives, known to those skilled in the art, such as anti-block agents, slip additives, UV stabilizers, pigments and processing aids may be added to the polymers from which the pouches of the present invention are made.
As can be seen from the different embodiments of the present invention shown in Figures 3-5, the film structure for the pouches of the present invention has design flexibility.
Different LLDPE can be used in the outer and core layers to optimize specific film properties such as film stiffness. Thus, the film can be optimized for specific applications such as for a vertical form, film and seal machine.
The polyethylene film structure used to make a pouch of the present invention is made by either the blown tube extrusion method or the cast extrusion method, methods wel I

known in the art. The blown tube extrusion method is described, for example, in Modern Plastics Mid-October 1989 Encyclopedia Issue, Volume 66, Number 11, pages 264 to 266. The cast extrusion method is described, for example, in Modern Plastics Mid-October 1989 Encyclopedia Issue, Volume 66, Number 11, pages 256 to 257.
Embodiments of the pouches of the present invention, shown in Figures 1 and 2, are hermetically sealed containers filled with "flowable materials". By "flowable materials" it is meant, materials which are flowable under gravity or which may be pumped, but the term "flowable materials" does not include gaseous materials. The flowable materials include liquids for example milk, water, fruit juice, oil; emulsions for example ice cream mix, soft margarine; pastes for example meat pastes, peanut butter; preservers for example jams, pie fillings marmalade; jellies; Boughs; ground meat for example sausage meat;
powders for example gelatin powders,. detergents; granular solids for example nuts, sugar;
and like materials. The pouch of the present invention is particularly useful for liquid foods for example milk. The flowable material may also include oleaginous liquids for example, cooking oil or motor oil.
Once the film structure for the pouch of the present invention is made, the film structure is cut to the desired width for use in conventional pouch-forming machi nes. The embodiments of the pouch of the present invention shown in Figures 1 and 2 are made in so-called form, fill and seal machines well known in the art. With regard to Figure 1, there is shown a pouch 10 being a tubular member 11 having a longitudinal lap seal 12 and transverse seals 13 such that, a "pillow-shaped" pouch is formed when the pouch is filled with flowable material.
With regard to Figure 2, there is shown a pouch 20 being a tubular member 21 having a peripheral fin seal 22 along three sides of the tubular member 11, that is, the top seal 22a and the longitudinal side seals 22b and 22c, and having a bottom substantially concave or "bowl-shaped" member 23 sealed to the bottom portion of the tubular seal 21 such that when viewed in cross-section, longitudually, substantially a semi-circular or "bowed-shaped"
bottom portion is formed when the pouch is filled with flowable material. The pouch shown in Figure 2 is the so-called "Enviro-Pak" pouch known in the art.
The pouch manufactured according to the present invention is preferably the pouch shown in Figure 1 made on so-called vertical form, fill and seal (VFFS) machines well known in the art. Examples of commercially available VFFS machines include those manufactured by Hayssen or Prepac. A VFFS machine is described in the following reference: F.
C. Lewis, "Form-Fill-Seal," Packaging Encyclopedia, page 180, 1980.
In a VFFS packaging process, a sheet of the plastic film structure described herein is fed into a VFFS machine where the sheet is formed into a continuous tube in a tube-forming section. The tubular member is formed by sealing the longitudinal edges of the film together -either by lapping the plastic film and sealing the film using an inside/outside seal or by fin _7_ sealing the plast~.c film using an inside/inside seal. Next, a sealing bar seals the tube transversely at one end being the bottom of the "pouch", and then the fill material, for example milk, is added to the "pouch". The sealing bar then seals the top end of the pooch and either burns through the plastic film or cuts the film, thus, separating the formed completed pouch from the tube. The process of making a pouch with a VFFS
machine is generally described in U.S. Patent Nos. 4,503,102 and 4,521,437.
The capacity of the pouches of the present invention may vary. Generally, the pouches may contain from 5 millilitres to 10 liters, preferably from 1 millilitre to 8 liters, and more preferably from 1 millilitre to 5 liters of flowable material.
The film structure for the pouch of the present invention has precisely controlled strength. The use of the film structure described in the present invention for making a pouch results in a. stronger pouch, and, therefore, more preferably, the pouch contains fewer use-related leakers. The use of ULDPE seal layer of the present invention in a two or three-layer coextruded film product will provide a film structure that can. be used for making pouches at a faster rate in the VFFS and such pouches produced will contain fewer leakers.
The pouches of the present invention have excellent performance results when tested by the Milk Pouch Drop Test and Step Stair Drop Test--tests which are defined herein.
Under the Step Stair Drop Test, the pouches preferably have a "50 percent failure height" of greater than about 10 feet (3.0 m) and more preferably greater than about 13 feet (4m).
i _g_ Under the Milk Pouch Drop Test, the pouches of the present invention preferably have a failure rate of less than about 10 percent and more preferably less than about 7 percent.
With the: trend in today's consumer package industry moving toward providing the consumer with more environmentally friendly packages, the polyethylene pouch of the present invention is a good alternative. The use of the polyethylene pouch for packaging consumer liquids such as milk has its advantages over containers used in the past: the glass bottle, paper carton, and high density polyethylene jug. The previously used container consumed large amounts of natural resources in their manufacture, required a significant amount of space in landfill, used a large amount of storage space and used more energy a.n temperature control of the product (due to the heat transfer properties of the container).
The polyethylene pouch of the present invention made of thin polyethylene film, used for liquid packaging, offers many advantages over the containers used in the past. The polyethylene pouch. (1) consumes less natural resources, (2) requires less space in a landfill, (3) can be recycled, (4) can be processed easily, (5) requires less storage space, (6) uses less energy for storage (heat transfer properties for package), (7) can be safely incinerated and (8) can be reused, for example, the empty pouch can be used for other applications such as freezer bags, sandwich bags, and general purpose storage bags.
The following resins described in Table I were used to make blended and coextruded blown film samples described in the Examples and Comparative Examples:
-8a-Table I _ Resin Resin Melt Index Density Designation Type (g/10 minutes)(g/cm3) Resi n A LDPE 2.0 0.922 Resin B LLDPE 0.75 0.921 Resi n C LLDPE 1.0 0.926 Resin D ULDPE 1.0 0.912 Resin E ULDPE 0.8 0.905 Erucamide, a slip agent; Si02, an antiblock agent; and a processing aid were added to each of the resins. described in Table I such that the final concentrations of the additives were as follows: 1200 ppm Erucamide; 2500 ppm SiOz (4000 ppm for the ULDPE
coextruded products); and 900 ppm processing aid. Film structures were made at 2 mil (50.8 microns) and 3 mil (76.2 microns) target thickness.
Film structures produced were subjected to physical testing to determine its various properties including:
(1) Punct~~re, using method ASTM D3763;
(2) Dart Impact, using ASTM D1709, Method A and Method B;
(3) Elmendorf Tear, using ASTM D1922;
(4) Tensile~s, using ASTM D882;
(5) Gloss, using method ASTM D2457;
(6) Clarity, using method ASTM D1746;
(7) Coefficient of Friction, using method ASTM D1894;
(8) 2 percEmt Secant Modulus, using ASTM D882;
(9) Hot Tack Strength (only 3 mil (76.2 microns) films), using method described hereinhelow; and (10) Heat S~aal Strength (only 3 mil (76.2 microns) films), using method described herei nbelow;
The present invention is illustrated by the following examples but is not to be limited thereby.
Examples 1-4 and Comparative Examales A and B
Film samples~described in Table II were made as a monolayer using a Macro blown film line. The extruder was 2- ~/2 inches (6.4 cm) in diameter and had a 24:1 UD and a barrier screw with a Maddock mixing head. A 6 inch (15.2 cm) diameter die was used with a 40 mil (1,016 microns) die gap for the manufacture of the test films.


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2.5 blow-up ratio 216°C melt temperature The results o~f testing the above film samples are shown in Tables VI and VII.
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The film sam~Ales described in Tables III, IV and V were produced using an Egan 3-layercoextrusion line.
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2.5 blow-up ratio 216°C melt temperature The results of testing the above films samples are shown in Tables VI and VII.
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The results of testing the comparative film samples are shown in Tables VI and VI1.
Comparative Example E
Comparative Sample 3 in Table VI is SCLAIRFILM SM-3 film (herein SM-3 Film) commercially available from DuPont Canada. Two 24-centimeters diameter x 38 centimeters x 3 mil (76.2 microns) rolls of SM-3 Film were tested concurrently with the fabricated films of the present invention as in Examples 5-24. A publication by DuPont Canada discloses that SM-3 Film has a density of 0.918 g/cm3.

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WO 93/02859 , PCT/US92/06582 21:13459 In liquid packaging, the pouches may be subjected to a wide variety of abuses.
These include dropping of the pouch on the floor, dropping objects onto the pouch, picking the pouch up from one er~d and poking it with fingers or other objects.
Performance Tests--puncture, dart drop test, I:Imendorf tear and tensile--are intended to duplicate the type of abuse that the pouches would encounter during normal use. In general, the properties of the film structure for the pow:hes of the present invention were as good, and in some cases better than, the properties of prior art films.
For example, in the puncture test, of the 3 mil (76.2 microns) films that were tested, Sample 2A, Comparative Sample 1A and Sample 10A had the highest puncture resistance. Of the 2-mil (50.8 microns) gauge films, Comparative Sample 1 B
had the highest puncture resistance, followed by Sample 10B.
In the Elmen~dorf Tear test, however, it was unexpectedly found that some prior art films performed poorls~ in the Elmendorf tear tests, while the coextruded films with ULDPE
in one of the layers performed well. The films made with LLDPE either coextruded or monolayer, typically had gear values less than the coextruded films with ULDPE
in one of the layer.
The coefficient of friction (COF) property of the films generally ranged from 0.10 to 0.30.
In order for a film to properly move over the forming collars in a vertical form, fill and seal machine, the film is required to have a specific COF range. If the COF is high, the film may be too tacky for the VFFS to pull the film over the forming collar. If the COF is low, the film may be too slippery and the pull belts may not be able to grip the film to pull it. The process of coextrusion advantageou~cly allows for varying slip properties between the inside and outside of the film by varying the ~>lip concentration in the independent film layers.
The "2 percent secant modulus" property of the film structures is a measure of film stiffness. The stiffness of the film structures (2 percent secant modulus) is measured according to the method of ASTM-D882.
A specific amount of stiffness in a film is required for use of the film for producing pouches. If too much stiffness is present in the film, the film could experience too much fold when pulled over the edge of the forming collar and forming tube of a VFFS.
Excessive stiffness can cause the film to "hang-up" in the VFFS. On the other hand, if enough stiffness is not present in the film consumer problems are inevitable. For example, in milk packaging, a pouch is usually placed inside of ~~ support container which holds the pouch upright with approximately 2-1/2 inches (6 cm) to 3-1/2 inches (9 cm) of the pouch remaining above the container. To open the pouch, the corner is cut with a pair of scissors. If the film does not have enough stiffness (or wall strength), the film wall could collapse while the consumer is pouring the liquid from the pouch.

- - The film structures for the pouches of the present invention advantageously have precisely controlled stiffness which is required for the film structure to run through a VFFS.
Generally, the stiffness of the fil m structure of the present invention is from 1,400 MPa machine direction (MD)/1600 MPa cross direction (CD) to 2,100 MPa MD/2,500 MPa CD and preferably from 1,412 MPa MD/1,615 MPa CD to 2,050 MPa MD/2,358 MPa CD. If the film lacks stiffness, the film may become "bunched" in the corners of the VFFS unit. If the film is too stiff, the film will not bend properly for the sealing of longitudinal edges.
Advantageously, the stiffness of the structure can be changed by using different polyethylene layers. For example, it was found that by varying the amount of the higher density resin, for example Resin C (LLDPE having a density of 0.926) used in the core layer of the coextruded films, the stiffness of the film could be altered. For example, film Sample 7A had a MD 2 percent secant value of 1,891 MPa and film Sample 8A had a MD 2 percent secant value of 1,593 MPa.
The above Examples illustrates that the use of ULDPE as the sealing layer in a film 1 S structure for the pouch of the present invention allows for the development of a designed structure with the appropriate amount of tear resistance, dart impact resistance, elongation and stiffness (2 percent secant).
Example 25 - Hot Tack Strength The hot tack strength of the 3 mil (76.2 microns) films was measured using the "DTC Hot Tack Test Method." The "DTC Hot Tack Test Method" is a test method which measures the force required to separate a heat seal before the seal has had a chance to fully cool (crystallize). This simulates the filling of material into a pouch before the seal has had a chance to cool.
The "DTC Hot Tack Test Method" is a test method using a DTC Hot Tack Tester Model #52D according to the following conditions:
Specimen Width: _25.4 mm Sealing Time: 0.5 seconds Sealing Pressure: 0.27 N/mm/mm Delay Time: 0:5 seconds Peel Speed: 150 mm/second Number of Samples/Temperature: 3 Temperature Increments: 5°C
Temperature Range: 70°C- 130°C

WO 93/02859 2 ~1 ~13 4 5 5 ' P~/US92/06582 The hot tack ~~esultsforthe individual films may be found in Table VIII.
Table VIII: Hot Tack Seal Initiation Temperature and Hot Tack Strength Hot Tack SealTemperature Maximum Hot Sample Initiation at Tack No. Temperature Maximum Hot Strength, N/inch (C) Tack ( C~ (N/m) ngth Sample 98 120 3.3 (130) Sample 10!i 120 3.1 (122) Comparative102.5 115 3.4 (134) Sample Com parati ve Sample 102 115 3.5 (138) Sample 86 115 3.2 (126) Sample 86..'5 115 3.4 (134) Sample 87 115 2.9 (114) Sample 88..'i 105 3.1 (122) Sample 86.!5 105 3.7 (146) Sample 86 105 3.3 (130) Sample 76.!5 105 3.4 (134) Sample 76.!i 105 3.3 (130) Sample 87 105 3.4 (134) Sample 87 105 3.2 (126) Comparative Sample 104.5 120 3.6 (142) The "Maximum Hot Tack Strength" (maximum hot tack seal force) of the films and the temperature at which the Maximum Hot Tack Strength of the films occurs is shown in Table VIII.
The "Hot Tach Seal Initiation Temperature" ("Hot Tack Ti") shown in Table VIII
is the lowest temperature at which a seal is formed. A seal force of 1.0 N/inch (39.4 N/m) was selected as the force required to form an adequate seal, and therefore, Hot Tack Ti is found at a force of 1.0 N/inch (39.4 N/rn).
A low Hot Tack T; and a broad heat seal range is important for VFFS packaging.
A
low initiation temperature and a broad heat seal range allows the VFFS machine to run at faster line speeds by allowing the sealing jaws of the VFFS to close for short periods of time while still obtaining an adequate heat seal.
The Hot Tack'T; for 3 mil (76.2 microns) films in Table VIII shows that the coextruded films with Resin E in the seal layer showed the lowest Hot Tack T;
(76.5°C) followed by films with Resin D in the sealing layer (86°C).

~1w1345 5 ~ The 3-layer and 2-layer coextruded films with an ULDPE in the sealing layer had the lowest temperature (105°C) at which the highest hot tack strength was achieved.
Figures 6-8 illustrate the Hot Tack Seal Initiation Temperature and the temperature at which the maximum Hot Tack Strength was achieved for various film samples.
The temperature between Hot Tack Ti and the temperature of maximum Hot Tack Strength indicates the size of the hot tack sealing range. Figures 6-8 shows that films with ULDPE as the sealing layer have a much larger sealing range than the LLDPE and/or LLDPE/LDPE blend films.
Example 26 - Hot Tack Strength versus Sealing Time This Example was carried out using the DTC Hot Tack Test Method described in Example 25 except that the temperature was held constant at 110°C and the sealing time was varied from 0.1 second to 1 second. Only 3 mil (76.2 microns) films were tested.
The conditions used on the DTC Hot Tack Tester Model #52D were as follows:
Specimen Width: 25.4 mm Sealing Time: varied Delay Pressure: 0.27 Nlmm/mm Peel Speed: 150 mm/second Number of SampIesITime: 3 Sealing Time Range: 0.1 second to 1 second Temperature: 110°C
The results of the Hot Tack Strength for the various films are found in Table IX.
Table IX
Sample Number Hot Tack ngth, Stre N/inch (N/m) l S

ea Time Compara-Compara-(s) five five SampleSample SampleSampleSample Sample Sample 1A 3A 8A 10A 12A

0.0 0.1 0.17 0.30 0.68 2.07 2.21 2.92 2.37 (6.7) ( 11.8)(26.8)(81.6) (87.1 ( 115)(93.4) ) 0.2 0.58 0.85 1.74 2.75 3.03 3.04 2.89 (22.9) (33.5) (69.6)( 108) ( 119)( 120)( 114) 300,4 1.89 1.46 2.46 2.89 3.07 3.06 3.26 (74.5) (70.9) (96.9)( 114) ( 121 ( 121 ( 128) ) ) 0.6 2.40 1.80 2.52 3.06 3.23 3.12 3.15 (94.6) (70.9) (99.3)( 121 ( 127)( 123)( 124) ) 0.8 2.23 1.97 2.57 3.17 3.32 3.30 3.28 (87.9) (77.6) ( 101 ( 125) ( 131 ( 130)( 129) ) ) 1.0 2.36 1.99 2.55 3.15 3.39 3.39 3.25 (93.0) (78.4) ( 100)( 124) ( 134)( 134)( 128) WO 93/02859 ~ ~ , ~ ~ ~ ~ ~A PCT/US92/06582 Tables VIII and IX show that films made with ULDPE in the sealing layer have higher hot tack strengths for shorter sealing timesthan the comparative samples tested at 110°C.
The data of fable IX is shown specifically in Figures 9 to 11.
Example 27- Heat Seal Strength The heat seal strength of the 3 mil (76.2 microns) films was measured using the "DTC Heat Seal Strength Test Method." The "Heat Seal Strength Test Method" is a test method which measures the force required to separate a seal after the material has cooled to 23°C
temperature. The film samples were exposed to a relative humidity of SO
percent and a temperature of 23°C for a minimum of 24 hours prior to testing.
The "DTC Heat Seal Strength Test Method" is a test method using a DTC Hot Tack Tester Model #52D, wherein the heat seal portion of the tester is used, according to the following conditions:
Specimen Width: 25.4 mm Sealing Time: 0.5 seconds Sealing Pressure: 0.27 N/mm/mm Number of SampIes/Temperature: 3 Temperature Increments: 10°C
Temperature Range: 70°C- 140°C
The seal strength of the film samples was determined using an Instron Tensile Tester Model #1122 according to the following test conditions:
Direction of Pull: 90° to seal Crosshead Speed : 500 m m/mi nute Full Scale Load: 5 kg Number of Samples/'~hreshold: 31 percent of FSL
Break Criterion: 80 percent Gauge Length: 2.0 inches (50.8 millimeters) Sample Width: 1.0 inch (25.4 millimeters) The monolayer films were tested insidelinside, while the coextruded films were tested insidernside and inside/outside.
The heat seal results for the individual films are found in Table X.

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yf V a a WO 93/02859 ~ '~ ~~ 3 (~ 5 ~ ~~ PCT/US92/06582 The "Maximum Heat Seal Strength" (maximum heat seal force) of the film samples and the temperature at which the Maximum Heat Seal Strength of the films occurs is shown in Table X.
The "Heat Seal Initiation Temperature" ("Heat Seal Ti ") shown in Table X is the lowest temperature at which a seal is formed. A seal force of 1.0 Ibf/inch ( 175 N/m) was selected as the force required to form an adequate seal, and therefore, Heat Seal T; is found at a force of 1.0 I b/i n ( 175 N/m).
A low Heat'.ieal Ti and a broad heat seal range is important for VFFS
packaging. A
low initiation temperature and a broad heat seal range allows the VFFS machine to run at faster line speeds by allowing the sealing jaws of the VFFS to close for short periods of time while still obtaining an adequate heat seal.
The monolayer films and most of the coextruded films have a smooth heat seal curve as shown in Figures 12-14; however, the films with higher concentrations of ULDPE in the sealing layer appeared to have two maximum sealing temperatures. It is believed that these two peaks are the maximum sealing forces achieved for the ULDPE layer and the LLDPE layer.
As the heat is applied to the film, the ULDPE layer beings to form a seal at lower temperatures than the LLDPE (Heat Seal Ti of 82.5°C vs. 111°C). As more heat is applied to the seal, the ULDPE
layer reaches its maximum sealing temperature and strength. This phenomenon occurs below the Heat Seal Ti for the LLDPE film. After the maximum sealing temperature has been achieved, the sealing strength drops and then it increases reaching a maximum at the same temperature that the LLDPE film does.
As expected, based on the hot tack results, the filmswith Resin E in the sealing layer had the lowest Heat Seal Ti and the LLDPE had the highest Heat Seal Ti.
The Heat Seal Ti results were very similar to the Hot Tack Ti results.
Example 28 - Heat Seal Strength versus Sealing Time This Example was carried out using the DTC Hot Seal Test Method described in Example 27 except that the temperature was held constant at 110°C and the sealing time was varied from 0.1 second to 1 second. Only 3 mil (76.2 microns) films were tested.
The heat seal portion of the DTC Hot Tack #52D Tester Model was used. The conditions on the DTC Hoi: Tack Tester Model #52D were as follows:
Specimen Width: 25.4 mm Sealing Time: varied Sealing Pressure: 0.27 N/mm/mm Number of SampIes/Time: 4 Sealing Time Range: 0.1 second to 1 second Temperature: 110°C

) ~ ~ ~ ~ The seal strength was determined using an Instron Tensile Tester Model No. 112.
The film samples were exposed to a relative humidity of 50 percent and a temperature of 23°C
for a minimum of 24 hours prior to testing. The following were the test conditions:
Direction of Pull: 90° to seal Crosshead Speed: 500 mm/minute Full Scale Load: 5 kg Threshold: 1 percent of FSL
Break Criterion: 80 percent Gauge Length: 2.0 inches (50.8 mm) Sample Width: 1.0 inch (25.4 mm) The results of the heat seal force for various films are found in Table XI.
Table XI
Sample Number Heat gth, ch Seal Ibf/in(N/m) Stren l Sea TimeCompara-Compara-(s) tive tive SampleSampleSampleSampleSample Sample Sample 1A 3A 8A 10A 12A

0.0 0' 0.00 0.00 0.12 1.46 3.10 3.68 2.73 ~

(0.00) (0.00) (21) (256) (543) (644)(478) 0.2 0.18 0.00 0.44 2.44 3.49 3.62 3.83 (31 ) (0.00) (77) (427) (611 (634)(671 ) ) 0.4 0.46 0.25 2.67 3.21 3.57 3.71 3.96 (81) (44) (468) (562) (625) (650)(694) 0.6 0.68 0.32 3.11 3.34 3.41 4.02 (119) (56) (545) (585) (597)(704) 0.8 0.73 0.35 3.82 3.98 3.38 3.49 3.92 ( 128) (61 ) (669) (697) (592) (611 (687) ) 1.0 0.87 0.37 3.84 3.64 3.62 3.19 3.86 (152) (65) (672) (637) (634) (559)(676) Examples 25-28 illustrate that the use of ULDPE in the sealing layer of a film structure of the present invention is found to significantly increase the heat seal and hot tack range. The wider range of heat seal and hot tack would allow for faster line speeds on a VFFS
unit.
Example 29 A. Pouch Fabrication A Hayssen Ultima VFFS unit was used to make 2L water-filled pouches with a lay flat dimension of 7 inches (17.8 centimeters) x 12.5 inches (31.8 centimeters) for drop testing.
The following conditions were used on the Hayssen Ultima VFFS unit:

WO 93/02859 '~ ~ (~ 5 ~ '., PCT/US92/06582 Model Number: RCMB2-PRA
M.A. Number: 019644 Mass of Water: 2,000 g Bag Size: 7 inches x 12.5 inches Registration rolls on from 5° to 135°
Pull 6~elts on from 5° to 135°
Jaw Close: from 136° to 275°
Plate~~: from 136°to265°
Start Delay: 50 ms Type of Seal : Lap A Pro/Fill 3000 liquid filler was attached to the VFFS. The settings on the Pro/Fill 3000 were:
P.S.: '99 Volurne: 3539 1 S C.O.A..: 70 B. Drop Testing of Water Filled Pouches Two types of pouch drop tests were used to measure the performance of films produced in the Examples: (1) Milk Pouch Drop Test, and (2) Step Stair Drop Test. In the Milk Pouch Drop Test pouches were dropped "end-on" from a height of 5 feet ( 1.5 m). Any leak was classified as a failure. The pouches in the Step Stair Drop Test were also dropped "end-on"
from varying heights to deatermine a pouch's "50 percent failure height". The "50 percent failure height" means the height at which 50 percent of the pouches dropped will fail (leak).
Results of the drop testing are shown in Table XII below.

,~ 1 ~:13 ~ ~ Table XI I: Pouch s 4 5 5 Drop Test Milk Pouch Drop Ten Step Stair Drop Ten H
i h g t e At 5 Feet (1.5 m) Sample Gauge SO% Failure Failure No. Rate at (mil) Height, 13 Feet (4m) Number Number Failure Teased Failed (Percent)Feet (m) (percent) Sample 3 100 7 7 > 13 (>4 m) 36 Sample 2 9.6 (2.88 m) Sample 3 Sample 2 COULD NOT RUN THROUGH

Comparative COULD NOT MAKE-POUCH/SEALFAILURE

Sample 3 Comparative COULDNOTMAKE- POUCH/SEALFAILURE

Sample Comparative3 100 8 8 11.9 (3.57 m) Sample 2 100 15 15 6.4 (1.92 m) Comparative Sample Sample 3 > 13 ( >4 m) 24 Sample 2 11.7 (3.51 m) Sample 3 105 1 0.95 > 13 (>4 m) 20 Sample 2 100 2 2 10.8 (3.24 m) Sample 3 > 13 (>4 m) 36 Sample 2 Sample 3 105 1 0.95 >13 (>4m) 36 Sample 2 100 3 3 10.4 (3.13 m) SampIe7A 3 105 1 0.95 >13(>4m) 24 Sample 2 100 2 2 9.8 (2.94 m) SampIe8A 3 100 1 1 >13(>4m) 16 Sample 2 9.2 (2.76 m) 2p Sample 3 105 0 0 > 13 (>4 m) 16 Sample 2 100 2 2 10.3 (3.09 m) SampIelOA 3 105 0 0 >13(>4m) 16 Sample 2 10.5 (3.15 m) Sample 3 105 1 0.95 >13(>4m) 24 Sample 2 Sample 3 > 13 (>4 m) 24 Sam le 2 Comparative Sample 3 100 7 7 9.1 (2.73 m) Film Sample 7A was placed in the VFFS and 130 pouches were made of the sample film at the following temperatures:
Seam seal - 235°F
Front jaw - 285°F
Rear jaw - 285°F
One hundred five (105) pouches were dropped as per the Milk Pouch Drop Test and 25 were dropped as per the Step Stair Drop Test. In the Step Stair Drop Test, the maximum height that the pouches could be safely dropped from was 13 feet (4 m) as the results show in Table XII.
The following temperature settings were used to make all of the other~films tested and shown in Table XII:

Seam seal - 240°F
Front jaw - 300°F ,~ 4_ . '.
Rear jaw - 300 F °' ~ '.~
The number of pouches tested by the Milk Pouch Drop Test is shown in Table XI1.
The number of pouches tested by the Step Stair Drop Test was 25 for all samples.
Most of leakers for the 3 mil (76.2 microns) film in the Milk Pouch Drop Test and Step Stair Drop Test were from the seals. However, most of the leakers for the 2 mil (50.8 microns) films were film f~3ilures. The 2 mil (50.8 microns) films appeared to have stronger seals which was expected due to the thinner gauge through which sealing would occur.
As described in Table XII, the results of the Milk Pouch Drop Test showed that the 3 mil (76.2 microns) films (Samples of 9A and 10A) made with ULDPE (Resin E) in the sealing layer did not have any failures from the 5 foot (1.5 m) drop height. As noted in Table XII, a number of films could not be run on the VFFS.
Pouches made coextruded films with ULDPE (Resin D) in the sealing layer had Milk Pouch Drop Test failure rates less than the SM-3 Fiim and LLDPE/LDPE pouches.
The Milk Pouch Drop Test for the 2 mil (50.8 microns) samples showed that the LLDPE/LDPE pouch (Comparative Sample 2B) had the highest failure rate (15 percent) and Sample 4B with ULDPE layer had the lowest failure rate (2 percent). Unlike the 3 mil (76.2 microns) film where all of the failures were seal related, the 2 mil (50.8 microns) film failures were film related.
With regard to the Step Stair Drop Test, the SM-3 Film was found to have a "50 percent failure height" of about 9.1 feet r2.73 m) as shown in Table XII.
The 3 mil (76.2 microns) films made with ULDPE had "50 percent failure heights"
greater than 13 feet (4 m). Since 13 feet (4 m) was the maximum height that the pouches could be safely dropped, 25 poua:h samples were dropped from a height of 13 feet (4 m) and the percent failure at 13 feet (.4 m) was determined.
The 2 mil (50.8 microns) LLDPE/LDPE pouch (Comparative Sample 2B) had the lowest "50 percent failure height", while the ULDPE coextruded films had higher "SO percent failure heights". All of they film failures were film related as opposed to seal related.
Example 29 shows that water filled pouches made with U LDPE in the sealing layer are found to have a low failure rate in the Milk Pouch Drop Test, and a high "50 percent failure height" in the Step Stair Drop Test.
More particularly, the coextruded films for the pouches of the present invention having a heat seal layer comprised of an U LDPE provide a broader sealing range for pouch conversion and provide physical properties in finished pouches such that the pouches have a reduced failure rate.

Claims (11)

THE EMBODIMENT OF THE INVENTION IN WHICH AN EXCLUSIVE PROPERTY
OR PRIVILEGE IS CLAIMED AS FOLLOWS:
1. A pouch containing a flowable material, said pouch being made from a film in tubular form and having transversely heat sealed ends, said film being made from a material comprising a film structure comprising (a) from 10 to 100 percent by weight of at least one polymeric seal layer of an ultra low density linear ethylene copolymer interpolymerized from ethylene and at least one alpa-olefin in the range of C3-C10 and having a density of less than 0.915 g/cm3 and a melt index of less than about 10.0 g/10 minutes (i) a hot tack or heat seal initiation temperature of less than about 100°C at a force of at least about 1 N/inch (39.4 N/m) or (ii) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at a seal bar temperature of about 110°C and at less than about 0.2 seconds using the DTC Hot Tack Strength Method or achieving a heat seal strength of at least 1 lb f/inch (175 N/m) at a seal bar temperature of about 110°C and at less than about 0.25 seconds using the DTC Heat Seal Strength Method; and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer of ethylene and a C3-C18-alpha-olefin having a density of greater than about 0.916 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes, a high-pressure low density polyethylene having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to 10g/10 minutes and ethylene-vinyl acetate copolymer having a weight ratio of ethylene to vinyl acetate from 2.2:1 to 24:1 and a melt index of from 0.2 to 10g/10 minutes.
2. A pouch containing a flowable material, said pouch being made from a multilayer film structure comprising:
(I) (a) from 10 to 100 percent by weight of at least one polymeric seal layer of an ultra low density linear ethylene copolymer interpolymerized from ethylene and at least one alpha-olefin in the range of C3-C10 and having a density of less than about 0.915 g/cm3 and a melt index of less than about 10.0 g/10 minutes (i) a hot tack or heat seal initiation temperature of less than about 100°C at a force of at least about 1 N/inch (39.4 N/m) or (ii) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at a seal bar temperature of about 110°C and at less than about 0.2 seconds using the DTC Hot Tack Strength Method or achieving a heat seal -34a-strength of at least 1 lb f/inch (175 N/m) at a seal bar temperature of about 110°C and at less than about 0.25 seconds using the DTC Heat Seal Strength Method; and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer of ethylene and a C3-C18-alpha-olefin having a density of greater than about 0.916 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes, a high-pressure low density polyethylene having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes and ethylene-vinyl acetate copolymer having a weight ratio of ethylene to vinyl acetate from 2.2:1 to 24:1 and a melt index of from 0.2 to 10 g/10 minutes; and (II) at least one layer of a linear low density ethylene-C3-C18-alpha-olefin copolymer having a density of from 0.916 to 0.935 and a melt index of from 0.1 to 10 g/10 minutes.
3. The pouch of Claim 2 comprising:
(III) at least one layer of a high-pressure polyethylene having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes.
4. The pouch of Claim 3 wherein layer (II) is an outer layer, layer (III) is a core layer and layer (I) is a seal layer.
5. The pouch of Claim 1 wherein the pouch holds from mL to 5000 mL of flowable material and the flowable material is milk.
6. The pouch of Claim 1 wherein the copolymer (a) has an indicator of molecular weight distribution (I 10/I2) of from 5 to 20.
7. The pouch of Claim 1 wherein the film structure contains a slip agent, antiblock agent, a processing aid, a pigment of an ultraviolet light absorbing additive.
8. A process for preparing a pouch containing a flowable material comprising forming a tubular member having transversely heat-sealed ends, said tubular member being made from a film structure comprising a film structure for a pouch container comprising (a) from 10 to 100 percent by weight of at least one polymeric seal layer of an ultra low density linear ethylene copolymer interpolymerized from ethylene and at least one alpha-olefin in the range of C3C10 and having (1) a density of less than about 0.915 g/cm3, (2) a melt index of less than about 10.0 g/10 minutes and 3(i) a hot tack or heat seal initiation temperature of less than about 100°C at a force of at least about 1 N/inch (39.4 N/m) or (ii) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at a seal bar temperature of about 110°C and at less than about 0.2 seconds using the DTC Hot Tack Strength Method or achieving a heat seal strength of at least 1 lb f/inch (175 N/m) at a seal bar temperature of about 110°C and at less than about 0.25 -35a-seconds using the DTC Heat Seat Strength Method; and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer of ethyelene and a C3-C18-alpha-olefin having a density of greater than about 0.916 g/cm3 and, a melt index of from 0.1 to 10 g/10 minutes, a high-pressure low density polyethylene having a density of -35b-from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to 10g/10 minutes and ethylene-vinyl acetate copolymer having a weight ratio of ethylene to vinyl acetate from 2.2:1 to 24:1 and a melt index of from 0.2 to 10 g/10 minutes.
9. A process for preparing a pouch containing a flowable material comprising forming a tubular member having transversely heat-sealed ends, said tubular member being made from a film structure comprising:
(I)(a) from 10 to 100 percent by weight of at least one polymeric seal layer of on ultra low density linear ethylene copolymer interpolymerized from ethylene and at least one alpha-olefin in the range of C3-C10 and having a density of less than about 0.915 g/cm3 and a melt index of less than about 10.0 g/10 minutes and (i) a hot tack or heat seal initiation temperature of less than about 100°C at a force of at least about 1 N/inch (39.4 N/m) or (ii) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at a seal bar temperature of about 110°C and at less than about 0.2 seconds using the DTC Hot Tack Strength Method or achieving a heat seal strength of at least 1 lb f/inch (175 N/m) at a seal bar temperature of about 110°C and at less than about 0.25 seconds using the DTC Heat Seal Strength Method;
and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer, of ethylene and a C3-C18-alpha-olefin having a density of greater than about 0.916 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes, a high-pressure low density polyethylene having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes and ethylene-vinyl acetate copolymer having a weight ratio of ethylene to vinyl acetate from 2.2:1 to 24:1 and a melt index of from 0.2 to 10 g/10 minutes; and (II) at least one layer of a linear low density ethylene-C3-C18-alpha-olefin copolymer having a density of from 0.916 to 0.935 and a melt index of from 0.1 to 10 g/10 minutes.
10. The process of Claim 9 wherein the film structure includes:
(III) a high-pressure polyethylene having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes.
11. A film structure for a pouch container comprising (a) from 10 to 100 percent by weight of at least one polymeric seal layer of an ultra low density linear ethylene copolymer interpolymerized from ethylene and at least one alpha-olefin in the range of C3-C10 and having (1) a density of less than about 0.915 g/cm3, (2) a melt index of less than about 10.0 g/10 minutes and (3)(i) a hot tack or heat seal initiation temperature of less than about 100°C at a force of at least about 1 N/inch (39.4 N/m) or (ii) achieving a hot tack strength of at least 1 N/inch (39.4 N/m) at a seal bar temperature of about 110°C and at less than about 0.2 seconds using the DTC Hot Tack Strength Method or achieving a heat seal strength of at least 1 lb f/inch (175 N/m) at a seal bar temperature of about 110°C and at less than about 0.25 seconds using the DTC Heat Seal Strength Method; and (b) from 0 to 90 percent by weight of at least one polymer selected from the group consisting of a linear copolymer of ethylene and a C3-C18-alpha-olefin having a density of greater than about 0.916 g/cm3 and a melt index of from 0.1 to g/10 minutes, a high-pressure low density polyethylene having a density of from 0.916 to 0.930 g/cm3 and a melt index of from 0.1 to 10 g/10 minutes and ethylene-vinyl acetate copolymer having a weight ratio of ethylene to vinyl acetate from 2.2:1 to 24:1 and a melt index of from 0.2 to 10 g/10 minutes.

-37a-
CA002113455A 1991-08-09 1992-08-07 Pouch for packaging flowable materials Expired - Lifetime CA2113455C (en)

Applications Claiming Priority (3)

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US07/742,800 1991-08-09
US07/742,800 US5288531A (en) 1991-08-09 1991-08-09 Pouch for packaging flowable materials
PCT/US1992/006582 WO1993002859A1 (en) 1991-08-09 1992-08-07 Pouch for packaging flowable materials

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CA2113455A1 CA2113455A1 (en) 1993-02-18
CA2113455C true CA2113455C (en) 2000-01-04

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EP (1) EP0598017B1 (en)
JP (1) JPH06510310A (en)
AU (1) AU668879B2 (en)
CA (1) CA2113455C (en)
DE (1) DE69228935T2 (en)
ES (1) ES2132126T3 (en)
FI (1) FI940569A0 (en)
NZ (1) NZ243873A (en)
WO (1) WO1993002859A1 (en)

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ES2132126T3 (en) 1999-08-16
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AU2436392A (en) 1993-03-02
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AU668879B2 (en) 1996-05-23
JPH06510310A (en) 1994-11-17

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