WO2007059902A2 - Systeme composite presentant la fonction de capteur/indicateur d'oxygene, et son utilisation - Google Patents

Systeme composite presentant la fonction de capteur/indicateur d'oxygene, et son utilisation Download PDF

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Publication number
WO2007059902A2
WO2007059902A2 PCT/EP2006/011077 EP2006011077W WO2007059902A2 WO 2007059902 A2 WO2007059902 A2 WO 2007059902A2 EP 2006011077 W EP2006011077 W EP 2006011077W WO 2007059902 A2 WO2007059902 A2 WO 2007059902A2
Authority
WO
WIPO (PCT)
Prior art keywords
composite system
oxygen
oxygen sorbent
layer
sorbent
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/EP2006/011077
Other languages
German (de)
English (en)
Other versions
WO2007059902A3 (fr
Inventor
Horst-Christian Langowski
Thomas Wanner
Wolfgang Lohwasser
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
3A Composites International AG
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
Original Assignee
Alcan Technology and Management Ltd
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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 Alcan Technology and Management Ltd, Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV filed Critical Alcan Technology and Management Ltd
Publication of WO2007059902A2 publication Critical patent/WO2007059902A2/fr
Publication of WO2007059902A3 publication Critical patent/WO2007059902A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered 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
    • B32B27/08—Layered 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2250/00—Layers arrangement
    • B32B2250/24—All layers being polymeric
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/412—Transparent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/724—Permeability to gases, adsorption
    • B32B2307/7242—Non-permeable
    • B32B2307/7244—Oxygen barrier
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/74—Oxygen absorber
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2439/00—Containers; Receptacles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2457/00—Electrical equipment
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/012—Additives improving oxygen scavenging properties
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • G01N31/223—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols
    • G01N31/225—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols for oxygen, e.g. including dissolved oxygen

Definitions

  • the invention relates to a composite system with the function as a scavenger / indicator for oxygen, which contains at least one metal as an oxygen sorbent, which is convertible by oxygen in a higher oxidation state. It also contains an activator.
  • the indicator effect is caused by a change in the physical properties of the oxygen sorbent caused by the oxidation of the metal.
  • O 2 scavengers are substances that can sorb oxygen.
  • sorption are meant all known sorption possibilities, eg adsorption, absorption, chemisorption and physisorption.
  • the systems which are currently established according to the prior art can be classified here primarily according to the O 2 scavenger substrate and according to their initialization mechanism. lifi grace. Here one differentiates the following groups:
  • inorganic O 2 scavengers eg iron-based or sulfide-based systems
  • O 2 scavengers are initialized either by UV radiation or by moisture. This means that the O 2 scavenging function is only available after exposure to UV radiation or water, ie air humidity.
  • Indicator systems can generally be classified into Time-Temperature-Indicator (TTI), Gas / Leakage-Indicator and Freshness-Indicator systems.
  • TTI Time-Temperature-Indicator
  • Gas / Leakage-Indicator Gas / Leakage-Indicator
  • Freshness-Indicator systems can generally be classified into Time-Temperature-Indicator (TTI), Gas / Leakage-Indicator and Freshness-Indicator systems.
  • a TTI integrates the time-temperature history of a product and thus makes a direct statement about its storage conditions.
  • the indicator effect is effected by a chemical reaction or by opposite diffusion of two dyes.
  • Gas leakage indicators detect the gas concentration of O 2 , CO 2 or H 2 O in the packaging space. They thus make an indirect statement about the quality of the product.
  • the indicator effect is caused by a chemical reaction with the reactants O 2 , CO 2 or H 2 O.
  • Freshness indicators detect the metabolic products of microorganisms and thus make a direct statement about the quality of the product.
  • the Indicator effect is caused by a chemical reaction of the metabolites.
  • Combined 0 2 scavenger / indicator systems are not currently known in the art.
  • the O 2 scavenger works independently of the O 2 indicator, ie the 0 2 indicator merely signals that a certain 0 2 concentration has been exceeded.
  • a composite system comprising a substrate sheet and at least one scavenger / indicator layer deposited thereon as a thin film.
  • the scavenger / indicator layer contains at least one metal as an oxygen sorbent, which is due to the sorption of Oxygen changes at least one physical property of the oxygen sorbent.
  • the composite system contains at least one activator for the oxidation of the oxygen sorbent, which is in direct contact with the at least one scavenger layer.
  • a thin film is understood to mean all coating systems which can be produced by vacuum coating methods (CVD and PVD) as well as electrolytic deposition or coating in the nanoscale.
  • the functioning of the composite system according to the invention is based on the fact that the oxygen sorbent in the presence of oxygen and moisture can bind the oxygen in the corresponding oxide compounds.
  • the following reaction represents a possible pathway for metal oxidation: 2 Fe + 3 H 2 O + 1 MO 2 - -> 2 Fe (OH) 3
  • the oxygen sorbent can thus change one of its physical parameters under oxygen exposure. With regard to the physical properties concerned, there are no restrictions if they represent a visual or metrologically evaluable change.
  • the oxygen sorbent provides a magnetic or targeted magnetized material, such as e.g. elemental iron formed by contact with oxygen to a non-magnetic or less-magnetic compound, e.g. Iron oxide (s) is reacted.
  • a magnetic or targeted magnetized material such as e.g. elemental iron formed by contact with oxygen to a non-magnetic or less-magnetic compound, e.g. Iron oxide (s) is reacted.
  • the resulting change in permeability or remanence can be reduced by e.g. a sensor can be detected.
  • a magnetometer can be used here, while the change in permeability can be detected by an inductance measurement.
  • the oxygen sorbent is an electrically conductive material, such as elemental iron, and is converted by exposure to oxygen to a no or less electrically conductive compound, such as iron oxide (s).
  • the change in the electrical conductivity can be detected for example by means of a sensor.
  • the coupling of the current takes place on inductive or capacitive ways.
  • the detection during the inductive coupling can preferably carried out via a Wirbelstrommesstechnik.
  • detection can preferably take place according to the capacitor principle.
  • Another preferred variant provides that the electromagnetic absorption of the oxygen sorbent changes.
  • the oxygen sorbent e.g. elemental iron which, when exposed to oxygen, becomes an oxidic compound, e.g. Iron oxide (s) is reacted.
  • This can e.g. be detected by a sensor.
  • photometers or IR measuring devices are used as detectors for the UV / IR range. Detection is also possible in the VIS range (visual range) as well as in the microwave range. Particularly preferred is a visually perceptible color change of the oxygen sorbent.
  • the oxygen sorbents of the invention are based on materials which combine both the O 2 scavenger and the O 2 indicator functions.
  • the O 2 scavenger and indicator has the same reaction kinetics.
  • this has the further advantage that the correlation of the absorbed amount of oxygen of the O 2 scavenger with the color change of the O 2 indicator is independent of the temperature.
  • O 2 indicator function in contrast, has two Reaction kinetics and thus two different temperature dependencies. This means that the correlation of the residual capacity of the O 2 scavenger with the color change of the 0 2 indicator is temperature-dependent.
  • the oxygen sorbent is a metal selected from the group consisting of iron, zinc, aluminum, cobalt, copper, magnesium, chromium, nickel, titanium and tin.
  • the activator contained in the composite system is an electrolyte, a water basic compound, and / or a more noble metal than the oxygen sorbent, i. a metal with a higher normal potential.
  • a noble metal i. a metal with a higher normal potential.
  • these include e.g. Ag, Au and Cu.
  • electrolyte all compounds are suitable which support the electron transfer of the redox reaction. Preference is given to using compounds from the group of alkali metal and alkaline earth metal halides. Likewise, it is also possible to use metallic and non-metallic sulfates and phosphates, but also non-metallic halides, such as ammonium chloride. These electrolytes can be in both liquid and solid form.
  • the activator is a water-basic compound.
  • the added base-reacting compound causes, upon contact with water, ie at a certain relative humidity of the air, a basic environment is created in which then the oxygen sorbent can sorb the oxygen. In the dry state, however, there is no oxygen sorption due to the lack of basic environment.
  • the at least one water-basic compound is preferably selected from the group of hydroxides, carbonates, sulfides, thiosulfates, oxides, phosphates, polyphosphates of alkali or alkaline earth metals. Likewise, alkali or alkaline earth metal salts of organic acids are preferred. But it is also possible to use any other water-basic compounds.
  • the oxygen scavenger / indicator contains magnesium hydroxide, sodium thiosulfate or calcium oxide as the basic reacting compound.
  • the oxygen scavenger / indicator contains a polymer electrolyte and / or a gel electrolyte.
  • Polymers in combination with salts can be used in particular as polymer electrolytes, such as, for example, polyethyloxide (PEO) with LiPF 6 , polypropylene oxide (PPO) with LiCF 3 FO 3 or polyethylene oxide with LiClO 4 and optionally TiO 2 .
  • an electrolyte and a water-basic compound are used together as an activator.
  • the deposited scavenger / indicator layers preferably have a layer thickness in the range of 10 to 1000 nm.
  • the layer thickness used depends on the required scavenger capacity.
  • a preferred variant provides that the scavenger / indicator layer is transparent in the visible region of the spectrum.
  • the composite system according to the invention may also have at least one further layer.
  • This is preferably a lacquer layer, an adhesive layer, a further vapor-deposited layer or a polymer film. It is preferred that this further layer contains the above-described activator.
  • the further layer is a polymer film
  • this preferably consists of a polymer selected from the group of polyethylene terephthalate (PET), polyolefins, in particular polypropylene (PP) and polyethylene (PE), polyamides (PA), polystyrenes (PS ), Polycarbonates (PC) and their copolymers and polymer blends.
  • PET polyethylene terephthalate
  • PP polypropylene
  • PE polyethylene
  • PA polyamides
  • PS polystyrenes
  • PC Polycarbonates
  • the polymer film used as a further layer is non-positively connected to the scavenger / indicator layer with a laminating adhesive. In this case it is then possible for the activator to be contained in the laminating adhesive.
  • this layer can then be modified by foaming and / or stretching. In this way it is possible subsequently to influence the oxygen permeability of the composite system.
  • Such mixed metal layers then consist of the oxygen sorbent and a spacer.
  • the spacer can be another metal suitable as oxygen sorbent or also a metal without scavenger property.
  • the substrate film itself is a composite film.
  • the substrate film it is then particularly preferred for the substrate film to have a barrier layer for oxygen.
  • the barrier layers consisting of silicon oxides and aluminum oxides can be produced, for example, by a vacuum thin-layer method, the preferred layer thicknesses being in the range from 1 nm to 200 nm.
  • the material of the substrate film preferably consisting of a polymer selected from the group of polyethylene terephthalates, polyolefins, in particular polypropylene and polyethylene, polyamides, polystyrenes, polycarbonates and / or their copolymers and polymer blends.
  • the at least one activator is integrated into the scavenger / indicator layer.
  • the composite system according to the invention can be present in two variants, ie as a non-visible and visible variant.
  • the visible variant enables a visual perception and evaluation, which is generally sufficient with regard to qualitative evaluations.
  • the non-visible variant is in turn based on the change of other physical properties, which, as described above, can be evaluated with appropriate measuring instruments and thus can also provide additional quantitative results.
  • the information is often important, how the headspace atmosphere behaves in the packaging.
  • the composite system according to the invention has the special feature that the weight ratio of oxygen sorbent to activator is adjustable so that the oxygen sorbent at a defined time, which represents the residual capacity of the oxygen sorbent, changes at least one of its physical properties. This particularly preferably includes a color change point.
  • a further variant according to the invention provides that the weight ratio of oxygen sorbent to activator is set so that the oxygen sorbent undergoes a change in its physical properties at a defined point in time, which exceeds a certain oxygen concentration. indicating onszeitspanne has.
  • a preferred physical property is also the electromagnetic absorption, ie the change in the color of the sorbent. By means of the color change point, a defined residual capacity of the oxygen sorbent is to be signaled visually or with the aid of a measurement.
  • a third variant according to the invention provides that the weight ratio of oxygen sorbent to activator is adjusted so that the oxygen sorbent changes at least one of its physical properties at a defined time, which indicates the exceeding of a certain oxygen concentration.
  • the preferred physical property here too is the color transition point.
  • the composite systems described are very suitable as packaging films for any packaged goods, especially food. Likewise, the composite systems can be used to protect moisture sensitive components in electronic or electrical equipment.
  • the applications include the food industry, pharmaceutical products and devices, the electronics industry, the chemical industry as well as cultural and military sectors.
  • FIG. 1 shows the oxygen uptake over time, normalized to the O 2 scavenger dimensions, of composite systems according to the invention.
  • oxygen sorbent here iron, aluminum and zinc were used.
  • FIG. 2 shows the oxygen uptake over time, normalized to the O 2 scavenger dimensions, of a composite system according to the invention.
  • the scavenger / indicator layer vapor-deposited in vacuum is based on aluminum as the oxygen sorbent.
  • an activator is additionally integrated into the scavenger / indicator layer.
  • the composite system according to the invention additionally comprises a film of polyethylene.

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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)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Gas Separation By Absorption (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

L'invention concerne un système composite présentant la fonction de capteur/indicateur d'oxygène, comprenant au moins un métal qui sert d'agent de sorption d'oxygène et qui peut atteindre un degré d'oxydation supérieur par l'intermédiaire de l'oxygène. Le système composite selon l'invention comprend également un activateur. La fonction d'indicateur est mise en oeuvre par modification des propriétés physiques de l'agent de sorption d'oxygène, qui est induite par l'oxydation du métal.
PCT/EP2006/011077 2005-11-22 2006-11-17 Systeme composite presentant la fonction de capteur/indicateur d'oxygene, et son utilisation Ceased WO2007059902A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200510055635 DE102005055635B4 (de) 2005-11-22 2005-11-22 Verbundsystem mit Sauerstoff-Scavenger/Indikator-Funktion und dessen Verwendung
DE102005055635.3 2005-11-22

Publications (2)

Publication Number Publication Date
WO2007059902A2 true WO2007059902A2 (fr) 2007-05-31
WO2007059902A3 WO2007059902A3 (fr) 2007-07-12

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PCT/EP2006/011077 Ceased WO2007059902A2 (fr) 2005-11-22 2006-11-17 Systeme composite presentant la fonction de capteur/indicateur d'oxygene, et son utilisation

Country Status (2)

Country Link
DE (1) DE102005055635B4 (fr)
WO (1) WO2007059902A2 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012091587A1 (fr) 2010-12-30 2012-07-05 Uniwersytet Ekonomiczny W Poznaniu Éliminateurs d'oxygène à base de nano-fer
JPWO2014203942A1 (ja) * 2013-06-21 2017-02-23 三菱瓦斯化学株式会社 酸素検知多層体、並びにそれを用いた酸素検知包装材及び脱酸素剤包装体

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6469338A (en) * 1987-09-11 1989-03-15 Kansai Paint Co Ltd Film laminate having oxygen absorbing capacity
US5399289A (en) * 1992-10-01 1995-03-21 W. R. Grace & Co.-Conn. Compositions, articles and methods for scavenging oxygen which have improved physical properties
DE69925658T2 (de) * 1998-03-12 2005-11-10 Mitsubishi Gas Chemical Co., Inc. Sauerstoffabsorbierende Mehrschichtfolie, deren Herstellungsverfahren und Verpackungsbehälter
JP3896823B2 (ja) * 2001-11-13 2007-03-22 東洋製罐株式会社 酸素吸収材料の品質検査方法
US7326988B2 (en) * 2002-07-02 2008-02-05 Matsushita Electric Industrial Co., Ltd. Semiconductor device and method for fabricating the same
GB2401862B (en) * 2004-01-14 2005-04-13 Giovanni Maria Laporta Improved bottle stopper
US7435704B2 (en) * 2004-03-10 2008-10-14 Hekal Ihab M Oxygen absorber
US20060069197A1 (en) * 2004-09-27 2006-03-30 Tammaji Kulkarny S Oxygen scavenging composition

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012091587A1 (fr) 2010-12-30 2012-07-05 Uniwersytet Ekonomiczny W Poznaniu Éliminateurs d'oxygène à base de nano-fer
JPWO2014203942A1 (ja) * 2013-06-21 2017-02-23 三菱瓦斯化学株式会社 酸素検知多層体、並びにそれを用いた酸素検知包装材及び脱酸素剤包装体

Also Published As

Publication number Publication date
WO2007059902A3 (fr) 2007-07-12
DE102005055635A1 (de) 2007-05-31
DE102005055635B4 (de) 2008-03-06

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