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WO2017209107A1 - Feuille en couches, matériau d'emballage et article moulé - Google Patents

Feuille en couches, matériau d'emballage et article moulé Download PDF

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Publication number
WO2017209107A1
WO2017209107A1 PCT/JP2017/020039 JP2017020039W WO2017209107A1 WO 2017209107 A1 WO2017209107 A1 WO 2017209107A1 JP 2017020039 W JP2017020039 W JP 2017020039W WO 2017209107 A1 WO2017209107 A1 WO 2017209107A1
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WIPO (PCT)
Prior art keywords
layer
gas barrier
group
laminated sheet
compound
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
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PCT/JP2017/020039
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English (en)
Japanese (ja)
Inventor
伊織 竹内
未悠 松井
雅之 樫村
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.)
Toppan Inc
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Toppan Printing Co Ltd
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Filing date
Publication date
Application filed by Toppan Printing Co Ltd filed Critical Toppan Printing Co Ltd
Priority to JP2018520918A priority Critical patent/JP6947173B2/ja
Publication of WO2017209107A1 publication Critical patent/WO2017209107A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
    • 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
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
    • B65D65/38—Packaging materials of special type or form
    • B65D65/40—Applications of laminates for particular packaging purposes

Definitions

  • the present invention relates to a laminated sheet, a packaging material, and a molded product.
  • This application claims priority on May 31, 2016 based on Japanese Patent Application No. 2016-108159 for which it applied to Japan, and uses the content here.
  • packaging materials used for packaging foods and non-food products such as pharmaceuticals and electronic components have been designed to prevent the alteration of contents and to permeate gases such as oxygen and water vapor in order to maintain their functions and properties. It is required to have a gas barrier property for blocking.
  • an inorganic vapor deposition film in which an inorganic vapor deposition layer is provided on at least one surface of a substrate such as a polyester film is widely used (for example, Patent Document 1).
  • Patent Document 1 an inorganic vapor deposition film as proposed in Patent Document 1 is stressed by bending, stretching, or the like, the inorganic vapor deposition layer is damaged, and the gas barrier property tends to be lowered.
  • Patent Document 2 an aqueous solution or a water / alcohol mixed solution containing a water-soluble polymer and at least one of at least one alkoxide, a hydrolyzate thereof, and tin chloride on an inorganic vapor deposition layer is used as a main agent.
  • a gas barrier laminated film provided with a gas barrier film formed by applying a coating agent to be heated and drying.
  • This gas barrier laminate film exhibits high gas barrier properties, and retains a certain degree of gas barrier properties even after bending, stretching, etc., by coating the inorganic vapor deposition layer with a flexible gas barrier coating. It is also disclosed that it has heat resistance, moisture resistance and water resistance.
  • the heat and moisture resistance of the gas barrier coating disclosed in Patent Document 2 is not sufficient, and when exposed to a high temperature and high humidity atmosphere, the gas barrier coating may swell and the gas barrier properties may deteriorate.
  • the flexibility of this gas barrier coating is not sufficient, and when the gas barrier laminated film is processed such as bending or stretching, it can be processed to an inorganic vapor deposition layer depending on the type and degree of processing. May cause damage to gas barrier properties.
  • the present invention has been made in view of the above circumstances, and an object thereof is to provide a laminated sheet having a layer excellent in flexibility and heat and humidity resistance, a packaging material using the same, and a molded product.
  • the laminated sheet according to the first aspect of the present invention includes a base material, a hydroxyl group-containing polymer compound (A), an epoxy group-containing silane coupling agent (B), and the epoxy group-containing silane coupling agent (B).
  • the ratio of the hydroxyl group-containing polymer compound (A) to the total mass of the silicon compound (C) with respect to the SiO 2 equivalent is 25 to 30% by mass, and the epoxy group-containing silane coupling agent compound (B). The ratio is 5 to 30% by mass.
  • the silicon compound (C) may contain at least one compound (C1) selected from the group consisting of a compound represented by the following formula (c1) and a hydrolyzate thereof.
  • Si (OR 1 ) 4 (c1) (In the formula, R 1 is an alkyl group having 1 to 4 carbon atoms or an alkoxyalkyl group having 1 to 4 carbon atoms, and four R 1 in the formula may be the same or different.)
  • the epoxy group-containing silane coupling agent (B) includes at least one compound (B1) selected from the group consisting of a compound represented by the following formula (b1) and a hydrolyzate thereof. You may go out.
  • the laminated sheet according to the first aspect may further include a gas barrier layer formed from an inorganic material.
  • the packaging material according to the second aspect of the present invention includes the laminated sheet according to the first aspect.
  • the packaging material according to the second aspect may be a packaging material for hot water treatment.
  • the molded product according to the third aspect of the present invention includes the packaging material according to the second aspect.
  • the molded product according to the third aspect may be a vertical bag-filling sealing bag, a vacuum packaging bag, a pouch with a spout, a laminated tube container, an infusion bag, a container lid, a paper container, or a vacuum insulator.
  • each aspect of the present invention it is possible to provide a laminated sheet having a layer excellent in flexibility and heat and humidity resistance, a packaging material and a molded product using the same.
  • FIG. 1 is a cross-sectional view schematically showing a laminated sheet 10 according to the first embodiment of the present invention.
  • the laminated sheet 10 includes a base material 1, a gas barrier layer 3 formed of an inorganic material, and a layer 5 (hereinafter also referred to as “layer of composition (I)”) formed of the following composition (I).
  • layer of composition (I) a hydroxyl group-containing polymer compound (A), an epoxy group-containing silane coupling agent (B), and another silicon compound (C) other than the epoxy group-containing silane coupling agent (B) Including the hydroxyl group-containing polymer compound (A), the epoxy group-containing silane coupling agent (B), and the total amount of the silicon compound (C) in terms of SiO 2.
  • I a composition in which the ratio of the epoxy group-containing silane coupling agent compound (B) is 5 to 30% by mass.
  • the gas barrier layer 3 is laminated on one surface of the substrate 1, and the layer 5 of the composition (I) is laminated on the gas barrier layer 3.
  • the substrate 1 examples include plastics, papers, rubbers, and the like.
  • the substrate 1 is preferably a plastic film from the viewpoint of adhesion between the substrate 1 and the gas barrier layer 3 and the like.
  • plastics examples include polyester (eg, polyethylene terephthalate (PET), polyethylene naphthalate (PEN), etc.), polyolefin (eg, polyethylene, polypropylene, etc.), polystyrene, polyamide (eg, 66-nylon, etc.), polycarbonate, polyacrylonitrile, polyimide, etc. Engineering plastics and the like.
  • PET polyethylene terephthalate
  • PEN polyethylene naphthalate
  • polyolefin eg, polyethylene, polypropylene, etc.
  • polystyrene polyamide
  • polycarbonate eg, 66-nylon, etc.
  • the plastic film may be either stretched or unstretched, and preferably has sufficient mechanical strength and dimensional stability. In particular, a film arbitrarily stretched in the biaxial direction is preferably used.
  • the base material 1 is preferably a polyamide film or a polyester film, and more preferably a polyester film, in consideration of price, moisture resistance, filling suitability, texture, and discardability.
  • the surface of the substrate 1 may be subjected to a surface activation treatment such as corona treatment, flame treatment, and plasma treatment.
  • the thickness of the substrate 1 can be appropriately set according to the use of the laminated sheet 10.
  • the laminated sheet 10 is not particularly limited. However, in consideration of suitability as a packaging material and processability, it is preferably 3 to 200 ⁇ m and more preferably 6 to 30 ⁇ m. .
  • the gas barrier layer 3 is formed from an inorganic material.
  • an inorganic material capable of constituting a layer for imparting gas barrier properties such as oxygen barrier property and water vapor barrier property to the laminated sheet 10 is appropriately selected.
  • metal for example, aluminum
  • inorganic oxidation Form example, aluminum oxide, silicon oxide, magnesium oxide, tin oxide, etc.
  • the gas barrier layer 3 is preferably a deposited film obtained by depositing the inorganic material on the substrate 1 by a deposition method.
  • an aluminum oxide vapor deposition film is a reactive vapor deposition, reactive sputtering, or reactive ion plate that forms a thin film in the presence of a mixed gas of oxygen gas and inert gas such as carbon dioxide gas using aluminum as an evaporation material. It can be formed by ting or the like.
  • a mixed gas of oxygen gas and inert gas such as carbon dioxide gas using aluminum as an evaporation material. It can be formed by ting or the like.
  • some aluminum may exist as it is, or aluminum peroxide may exist.
  • the thickness of the gas barrier layer 3 varies depending on the use of the laminated sheet 10 and the film thickness of the layer 5 of the composition (I), but is preferably 5 to 300 nm, more preferably 10 to 50 nm. If the thickness of the gas barrier layer 3 is less than the lower limit (5 nm) of the above range, the continuity of the gas barrier layer 3 may be impaired. When the thickness of the gas barrier layer 3 exceeds the upper limit (300 nm) of the above range, the flexibility of the gas barrier layer 3 is lowered, and there is a possibility that cracking may occur due to external factors such as bending and pulling after film formation.
  • the layer 5 of the composition (I) is a layer formed from the composition (I).
  • the composition (I) comprises a hydroxyl group-containing polymer compound (A), an epoxy group-containing silane coupling agent (B), and another silicon compound (C) other than the epoxy group-containing silane coupling agent (B). including.
  • the hydroxyl group-containing polymer compound (A) is not particularly limited as long as it is a polymer compound having a hydroxyl group.
  • the hydroxyl group-containing polymer compound (A) is preferably a vinyl alcohol polymer from the viewpoint of gas barrier properties.
  • a vinyl alcohol polymer is a polymer containing vinyl alcohol units. Examples of the vinyl alcohol polymer include polyvinyl alcohol (hereinafter also referred to as “PVA”), an ethylene-vinyl alcohol copolymer, a modified vinyl alcohol polymer, and the like.
  • the degree of polymerization of the vinyl alcohol polymer is preferably 500 or more and 3000 or less, and more preferably 1000 or more and 3000 or less.
  • PVA is particularly preferable.
  • the gas barrier property is particularly excellent.
  • PVA is a material generally obtained by saponifying polyvinyl acetate.
  • the PVA may be completely saponified PVA in which only a few percent of acetate groups remain, or may be partially saponified PVA in which the remaining amount of acetate groups is larger than that.
  • the degree of saponification is high, it is preferable because the water resistance of the layer 5 of the composition (I) is high, and completely saponified PVA is particularly preferable.
  • There are various degrees of polymerization of PVA ranging from 300 to several thousand.
  • PVA having any degree of polymerization may be used, but PVA having a high degree of polymerization is preferred because of its high water resistance.
  • the degree of polymerization of PVA is preferably 500 or more and 3000 or less, and more preferably 1000 or more and 3000 or less.
  • the epoxy group-containing silane coupling agent (B) is not particularly limited as long as it is an silane coupling agent having an epoxy group, and is selected from the group consisting of a compound represented by the following formula (b1) and a hydrolyzate thereof, for example. And at least one compound (B2) selected from the group consisting of a compound represented by the following formula (b2) and a hydrolyzate thereof. Among these, the compound (B1) is preferable.
  • R 3 is (It is an organic group containing an epoxy group, and R 4 is an alkyl group having 1 to 5 carbon atoms.)
  • R 2 is preferably CH 3 , C 2 H 5 , or C 2 H 4 OCH 3 .
  • R 3 include 2- (3,4-epoxycyclohexyl) ethyl group and 3-glycidoxypropyl group.
  • Specific examples of the compound represented by the formula (b1) include 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, and 3-glycidoxypropyltriethoxysilane.
  • Specific examples of the compound represented by the formula (b2) include 3-glycidoxypropylmethyldimethoxysilane, 3-glycidoxypropylethyldiethoxysilane, and the like. These can be used alone or in combination of two or more. Among these, 3-glycidoxypropyltrimethoxysilane and 3-glycidoxypropyltriethoxysilane are preferable, and 3-glycidoxypropyltrimethoxysilane is more preferable from the viewpoint of achieving both flexibility and heat and humidity resistance. .
  • OR 2 becomes OH.
  • the hydrolyzate of the compound represented by the formula (b1) or (b2) can be obtained by a known method.
  • the hydrolysis of the compound represented by the formula (b1) or (b2) is typically performed using an acid or alkali catalyst, alcohol and water. In view of easy control of hydrolysis, it is preferable to use an acid catalyst. At this time, in order to further control the hydrolysis, a generally known catalyst or the like may be added.
  • Examples of the silicon compound (C) include at least one compound (C1) selected from the group consisting of a compound represented by the following formula (c1) and a hydrolyzate thereof.
  • Si (OR 1 ) 4 (c1) (In the formula, R 1 is an alkyl group having 1 to 4 carbon atoms or an alkoxyalkyl group having 1 to 4 carbon atoms, and four R 1 in the formula may be the same or different.)
  • R 1 is preferably CH 3 , C 2 H 5 , or C 2 H 4 OCH 3 .
  • the compounds represented by the formula (c1) can be used alone or in combination of two or more.
  • OR 1 becomes OH.
  • the hydrolyzate of the compound represented by the formula (c1) can be obtained by a known method.
  • the hydrolysis of the compound represented by the formula (c1) is typically performed using an acid or alkali catalyst, alcohol and water. In view of easy control of hydrolysis, it is preferable to use an acid catalyst. At this time, in order to further control the hydrolysis, a generally known catalyst or the like may be added.
  • composition (I) may be used in addition to the hydroxyl group-containing polymer compound (A), the epoxy group-containing silane coupling agent (B), and the silicon compound (C) as long as the gas barrier property and heat and humidity resistance are not impaired.
  • Other components may be further included. Examples of other components include additives such as plasticizers, resins, dispersants, surfactants, softeners, stabilizers, antiblocking agents, film forming agents, pressure-sensitive adhesives, oxygen absorbers, and viscosity minerals. .
  • the content of the hydroxyl group-containing polymer compound (A) includes the mass of the hydroxyl group-containing polymer compound (A), the mass of the epoxy group-containing silane coupling agent (B), and the silicon compound (C).
  • the mass ratio of the mass of the hydroxyl group-containing polymer compound (A) to the total mass of the epoxy group-containing silane coupling agent (B) and the silicon compound (C) in terms of SiO 2 ((A) / [ (B) + (C)]) is preferably in the range of 25/75 to 30/70.
  • the gas barrier property of the layer 5 of the composition (I) is excellent. Moreover, it is excellent also in the softness
  • the content of the hydroxyl group-containing polymer compound (A) is not more than the upper limit (30% by mass) of the above range, the heat and moisture resistance of the layer 5 of the composition (I) is excellent, and the gas barrier property is high even under high temperature and high humidity conditions.
  • the SiO 2 equivalent amount of the silicon compound (C), all the silicon atoms contained in the silicon compound (C) is a SiO 2 mass assuming that became SiO 2, silicon atoms having a silicon compound (C) It is calculated from the quantity.
  • the content of the epoxy group-containing silane coupling agent (B) is the mass of the hydroxyl group-containing polymer compound (A), the mass of the epoxy group-containing silane coupling agent (B), and the silicon compound (C) in terms of SiO 2.
  • the total mass with respect to the amount is preferably 5 to 30% by mass, more preferably 5 to 25% by mass, and still more preferably 10 to 20% by mass.
  • the content of the epoxy group-containing silane coupling agent (B) is less than the lower limit (5% by mass) of the above range, the heat and humidity resistance may be insufficient, and the upper limit (30% by mass) of the above range. If it is too high, the flexibility of the layer 5 of the composition (I) may be reduced, or the functional group of the epoxy group-containing silane coupling agent (B) may become pores and gas barrier properties may be reduced. .
  • the hydrolyzate of the compound represented by the formula (b1) or (b2) is used as the epoxy group-containing silane coupling agent (B)
  • the content of the epoxy group-containing silane coupling agent (B) is hydrolyzed. Calculated based on the mass of the previous compound.
  • the silicon compound (C) when using a hydrolyzate of the compound represented by formula (c1), SiO 2 equivalent amount of the silicon compound (C) is calculated based on the weight of the unhydrolyzed compounds.
  • the total mass of the hydroxyl group-containing polymer compound (A), the epoxy group-containing silane coupling agent (B), and the silicon compound (C) in terms of SiO 2 is the total mass. 70 mass% or more is preferable with respect to the mass of solid content, and 90 mass% or more is more preferable. The upper limit of this content is not specifically limited, 100 mass% may be sufficient.
  • the thickness of the layer 5 of the composition (I) varies depending on the use of the laminated sheet 10, but is preferably 5 to 300 nm, more preferably 10 to 50 nm.
  • the thickness of the layer 5 of the composition (I) is not less than the lower limit (5 nm)
  • the heat and humidity resistance is excellent. It is excellent in a softness
  • the laminated sheet 10 can be manufactured, for example, by a manufacturing method including the following steps ( ⁇ 1) and ( ⁇ 2).
  • ⁇ 1 A step of forming the gas barrier layer 3 made of an inorganic material on one surface of the substrate 1.
  • ⁇ 2 A hydroxyl group-containing polymer compound (A), an epoxy group-containing silane coupling agent (B), a silicon compound (C), and a solvent on the surface of the substrate 1 on which the gas barrier layer 3 is formed.
  • the coating liquid (a) containing is formed, the coating film comprised from the said coating agent (a) is formed, the said coating film is dried, and the layer 5 of composition (I) is formed.
  • Step ( ⁇ 1) As a method for forming the gas barrier layer 3, a known method can be used.
  • a known vapor deposition method can be used.
  • the vapor deposition method include a vacuum vapor deposition method, a sputtering method, an ion plating method, a chemical vapor deposition method, and the like.
  • a heating means of the vacuum deposition apparatus by the vacuum deposition method an electron beam heating method, a resistance heating method, an induction heating method, or the like is preferable.
  • reactive vapor deposition may be performed by blowing oxygen gas or the like at the time of vapor deposition.
  • the coating liquid (a) is the same as the composition (I) except that it contains a solvent.
  • a solvent water or a mixed solvent of water and an organic solvent is preferable, and a mixed solvent of water and a lower alcohol having 1 to 5 carbon atoms is more preferable.
  • the coating method of the coating liquid (a) is not particularly limited.
  • casting method dipping method, roll coating method, gravure coating method, screen printing method, reverse coating method, spray coating method, kit coating method, die coating method.
  • Metal ring bar coating method chamber doctor combined coating method, curtain coating method and the like.
  • the method for drying the coating film is not particularly limited, and examples thereof include a hot air drying method, a hot roll contact method, an infrared heating method, and a microwave heating method. Drying may be performed by any one of these methods alone or in combination.
  • the drying temperature is not particularly limited, but when the above-mentioned water or a mixed solvent of water and an organic solvent is used as a solvent, it is usually preferably 50 to 160 ° C.
  • the pressure during drying is usually preferably normal pressure or reduced pressure, and is preferably normal pressure from the viewpoint of facility simplicity.
  • coating and drying of the coating liquid (a) for forming each layer are continuous. It may be performed continuously, or may be performed discontinuously through a winding process and a curing process.
  • the laminated sheet 10 includes the gas barrier layer 3 formed of an inorganic material and the layer 5 of the composition (I) on the substrate 1, the laminated sheet 10 is excellent in gas barrier properties such as oxygen barrier properties and water vapor barrier properties. Further, the layer 5 of the composition (I) is excellent in flexibility. Therefore, the abuse resistance of the laminated sheet 10 is high, and the gas barrier property is not easily deteriorated even after abuse such as bending and stretching.
  • the layer 5 of the composition (I) is excellent in heat and humidity resistance. Therefore, the gas barrier property can be exhibited at a high level even under high temperature and high humidity. Further, the gas barrier property can be maintained at a high level even after hot water treatment such as boil treatment and retort treatment.
  • FIG. 2 is a cross-sectional view schematically showing a laminated sheet 20 according to the second embodiment of the present invention.
  • the laminated sheet 20 includes a substrate 1, a gas barrier layer 3 formed of an inorganic material, a layer 5 of the composition (I), and a layer formed of the following composition (II) (hereinafter referred to as “composition (II). )) And 7).
  • the layer 7 of the composition (II) is provided between the gas barrier layer 3 and the layer 5 of the composition (I).
  • composition (II) A hydroxyl group-containing polymer compound (A) and a silicon compound (C) other than the epoxy group-containing silane coupling agent (B), and the epoxy group-containing silane coupling agent (B) No composition.
  • the composition (II) comprises an epoxy group-containing silane coupling agent (B), a mass of the hydroxyl group-containing polymer compound (A), a mass of the epoxy group-containing silane coupling agent (B), and a silicon compound (C ) Less than 5% by mass with respect to the total mass with the SiO 2 equivalent.
  • the laminated sheet 20 is the same as that of the first embodiment except that the laminated sheet 20 further includes a layer 7 of the composition (II).
  • composition (II) The hydroxyl group-containing polymer compound (A) and the silicon compound (C) in the composition (II) are the same as those described for the composition (I), and the preferred embodiments are also the same.
  • the composition (II) may further contain other components other than the hydroxyl group-containing polymer compound (A), the epoxy group-containing silane coupling agent (B), and the silicon compound (C) as necessary. Examples of the other components include the same as those mentioned for the composition (I).
  • the content of the hydroxyl group-containing polymer compound (A) is 25 to 30% by mass with respect to the total of the hydroxyl group-containing polymer compound (A) and the silicon compound (C) in terms of SiO 2.
  • the content is 27 to 30% by mass.
  • the content of the hydroxyl group-containing polymer compound (A) is not less than the lower limit of the above range, the gas barrier property and flexibility of the layer 7 of the composition (II) are more excellent.
  • the content of the hydroxyl group-containing polymer compound (A) is not more than the upper limit of the above range, the heat and humidity resistance of the layer 7 of the composition (II) is more excellent.
  • the content of the hydroxyl group-containing polymer compound (A) and the epoxy group-containing silane coupling agent (B) contains the epoxy group-containing silane coupling agent (B)
  • the total mass of the mass and the SiO 2 equivalent of the silicon compound (C) is preferably less than 5% by mass, and more preferably less than 3% by mass.
  • the content of the epoxy group-containing silane coupling agent (B) is within the above range, the gas barrier property is more excellent.
  • the total mass of the hydroxyl group-containing polymer compound (A) and the silicon compound (C) in terms of SiO 2 is preferably 70% by mass or more, and 90% by mass with respect to the total solid content. The above is more preferable. The upper limit of this content is not specifically limited, 100 mass% may be sufficient.
  • the thickness of the layer 7 of the composition (II) varies depending on the use of the laminated sheet 10, but is preferably 5 to 300 nm, more preferably 10 to 50 nm.
  • the thickness of the layer 7 of the composition (II) is not less than the lower limit (5 nm)
  • the gas barrier property in a state where abuse is not performed is excellent. It is excellent in a softness
  • the laminated sheet 20 can be manufactured, for example, by a manufacturing method including the following steps ( ⁇ 1), ( ⁇ 2), and ( ⁇ 3).
  • Step ( ⁇ 1) The step ( ⁇ 1) can be performed in the same manner as the step ( ⁇ 1).
  • the step ( ⁇ 2) can be performed in the same manner as the step ( ⁇ 2) except that the coating solution (b) is used instead of the coating solution (a).
  • the coating liquid (b) is the same as the composition (II) except that it contains a solvent.
  • the solvent of the coating liquid (b) water or a mixed solvent of water and an organic solvent is preferable, and a mixed solvent of water and a lower alcohol having 1 to 5 carbon atoms is more preferable.
  • Step ( ⁇ 3) The step ( ⁇ 3) can be performed in the same manner as the step ( ⁇ 2).
  • the laminated sheet 20 includes the gas barrier layer 3 formed of an inorganic material and the layer 5 of the composition (I) on the substrate 1, it has excellent gas barrier properties as in the first embodiment.
  • the layer 5 of the composition (I) is excellent in flexibility and heat and humidity resistance.
  • the layer 7 of the composition (II) there is a tendency that gas barrier properties in a state where abuse is not performed are more excellent.
  • FIG. 3 is a cross-sectional view schematically showing a laminated sheet 30 according to the third embodiment of the present invention.
  • the laminated sheet 30 includes a base material (first base material) 1, a gas barrier layer 3 formed from an inorganic material, a layer 5 of the composition (I), and another base material (second base material) 9. With.
  • the other base material 9 is laminated on the layer 5 of the composition (I) via an adhesive layer 11.
  • the laminated sheet 30 is the same as that of the first embodiment except that the laminated sheet 30 further includes another base material 9 and an adhesive layer 11.
  • the laminated sheet 30 may further include a layer 7 of the composition (II) between the gas barrier layer 3 and the layer 5 of the composition (I). In this case, the laminated sheet 30 is the same as that of the second embodiment except that the laminated sheet 30 further includes another base material 9 and an adhesive layer 11.
  • the other base material 9 is laminated
  • the other base material 9 is appropriately selected depending on the purpose and is not particularly limited, but plastic films and papers are usually preferable. Plastic films and papers may be used alone or in combination of two or more. For example, plastic films and paper may be laminated and used, or two or more kinds of plastic films may be laminated and used.
  • the laminated sheet 30 When the laminated sheet 30 is used in a molded product such as a vertical bag-filling sealing bag, a vacuum packaging bag, a pouch with a spout, a laminated tube container, an infusion bag, a container lid, a paper container, a vacuum insulator, etc. It is preferable that a heat-sealable layer is disposed as the other base material 9 on the outermost layer of the sheet 30. Thereby, the lamination sheet 30 becomes a structure which has heat-sealing property, and the process to a molded article becomes easy. A polyolefin layer is preferred as the heat-sealable layer.
  • the polyolefin is not particularly limited as long as it is a structure suitable for heat sealing, and examples thereof include low density polyethylene (LDPE) and unstretched polypropylene (CPP).
  • LDPE low density polyethylene
  • CPP unstretched polypropylene
  • the thickness of the heat-sealable layer is not particularly limited, but typically can be appropriately set within a range of 5 to 300 ⁇ m, preferably within a range of 10 to 100 ⁇ m.
  • the adhesive layer 11 is a layer that adheres the layer 5 of the composition (I) and another substrate 9.
  • the material of the adhesive layer 11 is not particularly limited, and can be appropriately selected from known adhesives used in, for example, a dry laminating method, a wet laminating method, and an extrusion laminating method.
  • the laminated sheet 30 can be manufactured by, for example, a manufacturing method including the following steps ( ⁇ 1), ( ⁇ 2), and ( ⁇ 3).
  • ( ⁇ 1) A step of forming the gas barrier layer 3 made of an inorganic material on one surface of the substrate 1.
  • the coating liquid (a) containing is formed, the coating film comprised from the said coating agent (a) is formed, the said coating film is dried, and the layer 5 of composition (I) is formed.
  • ( ⁇ 3) A step of laminating another base material 9 via the adhesive layer 11 on the surface of the base material 1 on which the gas barrier layer 3 and the layer 5 of the composition (I) are formed.
  • Step ( ⁇ 1) The step ( ⁇ 1) can be performed in the same manner as the step ( ⁇ 1).
  • the step ( ⁇ 2) can be performed in the same manner as the step ( ⁇ 2).
  • the laminated sheet 30 includes the gas barrier layer 3 formed of an inorganic material and the layer 5 of the composition (I) on the substrate 1, it has excellent gas barrier properties as in the first embodiment.
  • the layer 5 of the composition (I) is excellent in flexibility and heat and humidity resistance.
  • the other base material 9 can impart properties such as strength, sealing properties, easy-opening properties at the time of sealing, design properties, and light blocking properties.
  • the laminated sheet of this invention does not need to have the gas barrier layer 3 formed from an inorganic material.
  • gas barrier layer 3 formed from an inorganic material.
  • the gas barrier layer 3 and the layer 5 of the composition (I) are laminated in this order on one surface of the substrate 1 is shown, but the arrangement of each layer is not limited to this.
  • the gas barrier layer 3 and the layer 5 of the composition (I) may be provided on both surfaces of the substrate 1, respectively, the gas barrier layer 3 is provided on one surface of the substrate 1, and the composition (I ) Layer 5 may be provided.
  • a gas barrier layer 3 is provided between the substrate 1 and the layer 5 of the composition (I).
  • the layer 7 of the composition (II) in the second embodiment and the other substrate 9 in the third embodiment may be provided on both surfaces of the substrate 1.
  • the laminated sheet of the present invention may further have an anchor coat layer between the base material 1 and the gas barrier layer 3 for the purpose of improving their adhesion.
  • the material constituting the anchor coat layer include urethane resins, epoxy resins, acrylic resins, and polyester resins.
  • other additives such as a curing agent and a silane coupling agent may be added to these depending on the application.
  • a combination of an acrylic polyol, an isocyanate compound, and a silane coupling agent is preferable. When an anchor coat layer composed of this combination is used, stable and high adhesion can be obtained between the substrate and the vapor deposition layer.
  • the thickness of the anchor coat layer is not particularly limited as long as the thickness on the surface of the substrate 1 is uniform, but is preferably 0.01 to 2 ⁇ m, more preferably 0.05 to 0.5 ⁇ m. .
  • the thickness of the anchor coat layer is not less than the lower limit (0.01 ⁇ m) of the above range, the uniformity of the thickness of the anchor coat layer is high and the adhesion of the gas barrier layer 3 to the substrate 1 is more excellent. If the thickness of the anchor coat layer is less than or equal to the upper limit (2 ⁇ m) of the above range, the anchor coat layer retains sufficient flexibility and does not easily crack due to external factors such as abuse.
  • a layer other than the layer 7 of the composition (II) is replaced with the layer 7 of the composition (II) between the gas barrier layer 3 and the layer 5 of the composition (I). Or may be further included with the layer 7 of the composition (II).
  • the laminated sheet of the present invention further has other layers other than the other substrate 9 and the adhesive layer 11 on the layer 5 of the composition (I) (on the side opposite to the substrate 1 side). May be.
  • a printing layer or a vapor deposition layer can be provided for the purpose of providing design properties, providing light blocking properties, providing moisture resistance, and the like.
  • the laminated sheet of the present invention can exhibit high gas barrier properties even under high temperature and high humidity, and can maintain gas barrier properties at a high level even after hot water treatment such as boil treatment and retort treatment.
  • post-processing such as printing process, dry lamination, melt extrusion lamination, thermocompression lamination using the laminated sheet of the present invention is used in the packaging field of foods, pharmaceuticals, etc. It is possible to provide a packaging material with a wide practical range.
  • the use of the laminated sheet of the present invention is not limited to this, and can be used for uses other than packaging materials.
  • Applications other than packaging materials include, for example, LCD substrate films, organic EL substrate films, electronic paper substrate films, electronic device sealing films, PDP films, LED films, IC tag films, solar cell bags Sheets, films related to electronic devices such as protective films for solar cells, optical communication members, flexible films for electronic devices, diaphragms for fuel cells, sealing films for fuel cells, substrate films for various functional films, and the like.
  • the packaging material according to the present invention includes the above-described laminated sheet of the present invention.
  • the packaging material of this invention may be comprised only from the lamination sheet of this invention, and the structure containing the lamination sheet of this invention and another material may be sufficient as it. Examples of other materials include a thermoplastic resin film and paper.
  • the packaging material of the present invention is not particularly limited and can be used as a packaging material for various articles.
  • the packaging material of this embodiment is preferably used as a packaging material for articles that are easily deteriorated by the influence of oxygen, water vapor, etc., and in particular, is preferably used as a packaging material for food.
  • they can be preferably used as packaging materials for non-food products, for example, chemicals such as agricultural chemicals and pharmaceuticals, medical tools, machine parts, precision materials, and the like.
  • the laminated sheet of the present invention is excellent in heat and humidity resistance, and when subjected to hot water treatment, the gas barrier property and interlayer adhesion are not easily deteriorated. Therefore, the packaging material of the present invention is useful as a packaging material for hot water treatment. Examples of the hot water treatment include boil treatment and retort treatment.
  • the boil treatment is a method of sterilizing with wet heat to preserve foods and the like.
  • Examples of the boil treatment include a method of sterilizing a packaging material in which foods and the like are packaged at 60 to 100 ° C. and atmospheric pressure for 10 to 120 minutes, depending on the contents.
  • the boil treatment is preferably carried out using a hot water tank, and there are a batch type in which it is immersed in a hot water tank at a constant temperature and taken out after a fixed time, and a continuous type in which the hot water tank is sterilized through a tunnel type.
  • retort treatment is a method of sterilizing microorganisms such as molds, yeasts, and bacteria in order to preserve foods and the like.
  • examples of the retort treatment include a method in which a packaging material in which food or the like is packaged is subjected to a pressure sterilization treatment at 105 to 140 ° C. and 0.15 to 0.3 MPa for 10 to 120 minutes.
  • the retort apparatus used for the retort treatment includes a steam type using heated steam, a hot water type using pressurized superheated water, and the like, which are properly used depending on the sterilization conditions of food or the like as the contents.
  • the contents to be packaged with the hot water packaging material are not particularly limited, and may be food or non-food.
  • the food include curry, cooking seasoning sauce, and processed meat products.
  • non-food include medical products such as infusion preparations, and industrial products such as semiconductors and precision materials.
  • the molded product according to the present invention includes the packaging material of the present invention described above.
  • the molded article include a container, a member constituting a part of the container, and the like, and specific examples include a vertical bag filling and sealing bag, a vacuum packaging bag, a pouch with a spout, a laminate tube container, an infusion bag, and a container. Examples thereof include lid materials, paper containers, and vacuum insulators.
  • the molded product of the present invention can be manufactured by a known method.
  • vacuum packaging bags, spout pouches, laminated tube containers, infusion bags, container lids, paper containers, vacuum insulators, etc. heat sealing of packaging materials is usually performed. . Therefore, as a packaging material constituting these molded articles, one in which a heat-sealable layer is usually disposed on one or both outermost layers is preferable.
  • 0.1N hydrochloric acid is added to tetraethoxysilane (Si (OC 2 H 5 ) 4 , hereinafter referred to as “TEOS”), and the mixture is stirred for 30 minutes to be hydrolyzed to a solid content of 3% by mass (in terms of SiO 2 ).
  • TEOS hydrolysis solution was prepared.
  • 0.1N hydrochloric acid was added to 3-glycidoxypropyltrimethoxysilane (hereinafter referred to as “GPTMS”), and the mixture was stirred for 30 minutes for hydrolysis to prepare a GPTMS hydrolysis solution having a solid content of 3% by mass.
  • GPTMS hydrolysis solution having a solid content of 3% by mass.
  • a PVA solution, a GPTMS hydrolyzed solution, and a TEOS hydrolyzed solution are mixed so that PVA / GPTMS / TEOS (in terms of SiO 2 ) is 25/5/70 in terms of solid mass ratio to prepare a coating liquid (a1). did.
  • Preparation Example 2 A coating liquid (a2) was prepared in the same manner as in Preparation Example 1 except that PVA / GPTMS / TEOS (SiO 2 conversion) was 25/15/60.
  • Preparation Example 3 A coating solution (a3) was prepared in the same manner as in Preparation Example 1 except that PVA / GPTMS / TEOS (SiO 2 conversion) was 25/25/50.
  • Preparation Example 4 A coating liquid (a4) was prepared in the same manner as in Preparation Example 1 except that PVA / GPTMS / TEOS (SiO 2 conversion) was 25/30/45.
  • Preparation Example 5 A coating liquid (a5) was prepared in the same manner as in Preparation Example 1, except that PVA / GPTMS / TEOS (SiO 2 conversion) was 27.5 / 5 / 67.5.
  • Preparation Example 6 A coating liquid (a6) was prepared in the same manner as in Preparation Example 1, except that PVA / GPTMS / TEOS (SiO 2 equivalent) was 27.5 / 7 / 65.5.
  • Preparation Example 7 A coating solution (a7) was prepared in the same manner as in Preparation Example 1, except that PVA / GPTMS / TEOS (SiO 2 conversion) was 27.5 / 30 / 42.5.
  • Preparation Example 8 A coating solution (a8) was prepared in the same manner as in Preparation Example 1, except that PVA / GPTMS / TEOS (SiO 2 conversion) was set to 30/5/65.
  • Preparation Example 9 A coating solution (a9) was prepared in the same manner as in Preparation Example 1, except that PVA / GPTMS / TEOS (SiO 2 equivalent) was 30 / 17.5 / 52.5.
  • Preparation Example 10 A coating solution (a10) was prepared in the same manner as in Preparation Example 1, except that PVA / GPTMS / TEOS (SiO 2 equivalent) was 30/30/40.
  • Preparation Example 11 A coating solution (a11) was prepared in the same manner as in Preparation Example 1, except that GPTMS was changed to 3-glycidoxypropyltriethoxysilane (hereinafter referred to as “GPTES”).
  • GPTES 3-glycidoxypropyltriethoxysilane
  • Preparation Example 12 The PVA solution and the TEOS hydrolysis solution were mixed so that the PVA / TEOS (SiO 2 conversion) was 25/75 in terms of solid content, and the same as in Preparation Example 1 except that the GPTMS hydrolysis solution was not added. Thus, a coating liquid (b1) was prepared.
  • a coating solution (b2) was prepared in the same manner as in Preparation Example 1, except that PVA / GPTMS / TEOS (SiO 2 equivalent) was 20 / 17.5 / 62.5.
  • a coating solution (b3) was prepared in the same manner as in Preparation Example 1, except that PVA / GPTMS / TEOS (SiO 2 equivalent) was 35 / 17.5 / 47.5.
  • a coating liquid (b4) was prepared in the same manner as in Preparation Example 1 except that PVA / GPTMS / TEOS (SiO 2 equivalent) was 27.5 / 35 / 37.5.
  • a coating solution (b5) was prepared in the same manner as in Preparation Example 1, except that GPTMS was changed to 3-aminopropyltrimethoxysilane (hereinafter referred to as “APTMS”).
  • Example 1 On a biaxially stretched polyethylene terephthalate film (PET: manufactured by Toray, Lumirror (registered trademark) P60, thickness 12 ⁇ m, inner corona treatment), metal aluminum is evaporated by an electron beam heating vacuum deposition apparatus, and oxygen gas is present there. Then, aluminum oxide was vapor-deposited to form a vapor-deposited film (gas barrier layer) having a thickness of 20 nm.
  • PET biaxially stretched polyethylene terephthalate film
  • Lumirror registered trademark
  • a coating liquid (a1) is applied onto the gas barrier layer with a bar coater, and dried at 120 ° C. for 1 minute with a dryer to form a film (layer (a1)) having a film thickness of about 0.3 ⁇ m.
  • a laminated sheet having the configuration of [PET / gas barrier layer / layer (a1)] was obtained.
  • Example 2 [PET / gas barrier layer / layer (a2)] was performed in the same manner as in Example 1 except that the coating liquid (a2) was used instead of the coating liquid (a1) to form a film (layer (a2)). A laminated sheet having the structure is obtained.
  • Example 3 [PET / gas barrier layer / layer (a3)] was performed in the same manner as in Example 1 except that the coating liquid (a3) was used instead of the coating liquid (a1) to form a film (layer (a3)). A laminated sheet having the structure is obtained.
  • Example 4 [PET / gas barrier layer / layer (a4)] The same operation as in Example 1 was performed except that the coating liquid (a4) was used instead of the coating liquid (a1) to form a film (layer (a4)). A laminated sheet having the structure is obtained.
  • Example 5 [PET / gas barrier layer / layer (a5)] was performed in the same manner as in Example 1 except that the coating liquid (a5) was used instead of the coating liquid (a1) to form a film (layer (a5)). A laminated sheet having the structure is obtained.
  • Example 6 [PET / gas barrier layer / layer (a6)] was performed in the same manner as in Example 1 except that the coating liquid (a6) was used instead of the coating liquid (a1) to form a film (layer (a6)). A laminated sheet having the structure is obtained.
  • Example 7 [PET / gas barrier layer / layer (a7)] The same operation as in Example 1 was performed except that the coating liquid (a7) was used instead of the coating liquid (a1) to form a film (layer (a7)). A laminated sheet having the structure is obtained.
  • Example 8 [PET / gas barrier layer / layer (a8)] was performed in the same manner as in Example 1 except that the coating liquid (a8) was used instead of the coating liquid (a1) to form a film (layer (a8)). A laminated sheet having the structure is obtained.
  • Example 9 [PET / gas barrier layer / layer (a9)] was performed in the same manner as in Example 1 except that the coating liquid (a9) was used instead of the coating liquid (a1) to form a film (layer (a9)). A laminated sheet having the structure is obtained.
  • Example 10 [PET / gas barrier layer / layer (a10)] was performed in the same manner as in Example 1 except that the coating liquid (a10) was used instead of the coating liquid (a1) to form a film (layer (a10)). A laminated sheet having the structure is obtained.
  • Example 11 [PET / gas barrier layer / layer (a11)] The same operation as in Example 1 was performed except that the coating liquid (a11) was used instead of the coating liquid (a1) to form a film (layer (a11)). A laminated sheet having the structure is obtained.
  • Example 12 [PET / gas barrier layer / layer (b1)] The same operation as in Example 1 was performed except that the coating liquid (b1) was used instead of the coating liquid (a1) to form a film (layer (b1)). The laminated body which has a structure of] was obtained. Next, the coating liquid (a9) is applied onto the layer (b1) of the obtained laminate by a bar coater, and dried at 120 ° C. for 1 minute with a dryer to form a 0.3 ⁇ m-thick film (layer (a9 )) To form a laminated sheet having a structure of [PET film / gas barrier layer / layer (b1) / layer (a9)].
  • Comparative Example 1 On a biaxially stretched polyethylene terephthalate film (PET: manufactured by Toray, Lumirror (registered trademark) P60, thickness 12 ⁇ m, inner corona treatment), metal aluminum is evaporated by an electron beam heating vacuum deposition apparatus, and oxygen gas is present there. Then, aluminum oxide was vapor-deposited to form a vapor-deposited film (gas barrier layer) having a thickness of 20 nm.
  • PET polyethylene terephthalate film
  • Lumirror registered trademark
  • the coating liquid (b1) is applied onto the gas barrier layer with a bar coater, and dried at 120 ° C. for 1 minute with a dryer to form a film (layer (b1)) having a film thickness of about 0.6 ⁇ m.
  • a laminated sheet having the configuration of [PET / gas barrier layer / layer (b1)] was obtained.
  • Comparative Example 2 A laminated sheet was obtained in the same manner as in Comparative Example 1 except that the coating liquid (b2) was used instead of the coating liquid (b1) to form a film (layer (b2)).
  • Comparative Example 3 A laminated sheet was obtained in the same manner as in Comparative Example 1 except that the coating liquid (b3) was used instead of the coating liquid (b1) to form a film (layer (b3)).
  • Comparative Example 4 A laminated sheet was obtained in the same manner as in Comparative Example 1 except that the coating liquid (b4) was used instead of the coating liquid (b1) to form a film (layer (b4)).
  • Comparative Example 5 A laminated sheet was obtained by performing the same operation as in Comparative Example 1 except that the coating liquid (b5) was used instead of the coating liquid (b1) to form a film (layer (b5)).
  • LLDPE linear low density polyethylene
  • a two-component curable adhesive Takelac A525 (main agent) / Takenate A52 (hardener) manufactured by Mitsui Chemicals, Inc. was used.
  • Ny a stretched nylon film, Emblem ONMB (15 ⁇ m) manufactured by Unitika Ltd. was used.
  • CPP a polypropylene film manufactured by Toray Film Processing Co., Ltd., Treffan ZK93FM (60 ⁇ m) was used.
  • LLDPE a linear low-density polyethylene film, TUX-TCS (60 ⁇ m) manufactured by Mitsui Chemicals, Inc., Toro Cello Co., Ltd. was used.
  • the oxygen permeability of the sample was measured under the conditions of a temperature of 30 ° C. and a relative humidity of 70% using an oxygen permeation tester (OXTRAN 2/20, manufactured by Modern Control). The measurement method was expressed in units of cm 3 (STP) / (m 2 ⁇ day ⁇ MPa) in accordance with JIS K-7126 “Method B (isobaric method)” and ASTM D3985-81. .
  • (STP) means standard conditions (0 ° C., 1 atm) for defining the volume of oxygen.
  • a laminate film (configuration: laminated sheet / adhesive / LLDPE) was cut into a size of 200 mm long ⁇ 150 mm wide to prepare a sample.
  • the sample was subjected to the following abuse test.
  • the sample was stretched 5% in the machine direction at a speed of 100 ⁇ m / second using Tensilon manufactured by Toyo Baldwin, and the stretched state was maintained for 1 minute. Then, the film was returned to the original position at the same speed and stretched. .
  • the oxygen permeability and the water vapor permeability were measured by the measurement method described above.
  • (A) component represents a hydroxyl group-containing polymer compound (A)
  • Si agent represents a silane coupling agent
  • (C) component represents a silicon compound (C).
  • the laminated sheets of Examples 1 to 12 had high gas barrier properties in the state of the base paper. Further, the difference between the oxygen permeability and water vapor permeability of the base paper and the values of oxygen permeability and water vapor permeability after stretching and after retorting were small, and the film was excellent in flexibility and heat and humidity resistance.
  • the coating liquid used for forming the coating does not contain an epoxy group-containing silane coupling agent (B), Comparative Example 1, a polymer compound (A), an epoxy group-containing silane coupling agent (B), and a silicon compound (C )
  • the laminated sheet of the present invention has a high gas barrier property even under high temperature and high humidity, and can maintain the gas barrier property at a high level even after hot water treatment such as boil treatment and retort treatment. In addition, gas barrier properties are unlikely to deteriorate even after abuse such as bending or stretching. Therefore, by using the laminated sheet of the present invention, post-processing such as a printing process, dry lamination, melt extrusion lamination, thermocompression lamination, etc. is provided to provide a packaging material with a wide practical range used in the packaging field of foods, pharmaceuticals, etc. It is possible.
  • the laminated sheet of the present invention can be used for applications other than packaging materials.
  • Applications other than packaging materials include, for example, LCD substrate films, organic EL substrate films, electronic paper substrate films, electronic device sealing films, PDP films, LED films, IC tag films, solar cell bags Sheets, films related to electronic devices such as protective films for solar cells, optical communication members, flexible films for electronic devices, diaphragms for fuel cells, sealing films for fuel cells, substrate films for various functional films, and the like.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Wrappers (AREA)
  • Laminated Bodies (AREA)

Abstract

L'invention concerne une feuille en couches, qui comprend : un substrat ; et une couche formée d'une composition renfermant un composé de polymère comprenant un groupe hydroxyle (A), un agent de couplage au silane comprenant un groupe époxy (B), et un autre composé de silicium (C) autre que l'agent de couplage au silane comprenant un groupe époxy (B) ; le rapport du composé de polymère comprenant un groupe hydroxyle (A) étant de 25-30 % en masse et le rapport du composé d'agent de couplage au silane comprenant un groupe époxy (B) étant de 5-30 % en masse par rapport au total de la masse du composé de polymère comprenant un groupe hydroxyle (A), de la masse de l'agent de couplage au silane comprenant un groupe époxy (B) et d'une quantité équivalente de SiO2 du composé de silicium (C).
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JP7072117B1 (ja) 2021-11-22 2022-05-19 東京インキ株式会社 ガスバリア性グラビア積層体、ガスバリア用グラビアインキセット、およびガスバリア性グラビア積層体の製造方法
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