WO2018097161A1 - Film de polypropylène stratifié - Google Patents

Film de polypropylène stratifié Download PDF

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Publication number
WO2018097161A1
WO2018097161A1 PCT/JP2017/041940 JP2017041940W WO2018097161A1 WO 2018097161 A1 WO2018097161 A1 WO 2018097161A1 JP 2017041940 W JP2017041940 W JP 2017041940W WO 2018097161 A1 WO2018097161 A1 WO 2018097161A1
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WIPO (PCT)
Prior art keywords
film
polypropylene
surface layer
layer
laminated
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PCT/JP2017/041940
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English (en)
Japanese (ja)
Inventor
岡田一馬
久万琢也
山中康平
Original Assignee
東レ株式会社
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Application filed by 東レ株式会社 filed Critical 東レ株式会社
Priority to CN201780072183.XA priority Critical patent/CN110023086A/zh
Priority to KR1020197014060A priority patent/KR102405861B1/ko
Priority to JP2018552607A priority patent/JP7070426B2/ja
Publication of WO2018097161A1 publication Critical patent/WO2018097161A1/fr

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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
    • 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
    • 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
    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
    • 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
    • B32B7/02—Physical, chemical or physicochemical properties
    • B32B7/023—Optical properties
    • 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
    • B32B7/02—Physical, chemical or physicochemical properties
    • B32B7/027—Thermal properties
    • B32B7/028—Heat-shrinkability
    • 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
    • B32B2307/748—Releasability

Definitions

  • the present invention relates to a laminated polypropylene film that is excellent in releasability, surface smoothness, and transparency and can be suitably used as a release film.
  • Polypropylene films are excellent in transparency, mechanical properties, electrical properties, etc., and are therefore used in various applications such as packaging, mold release, tape, cable wrapping and electrical applications such as capacitors.
  • it since it has excellent surface releasability and mechanical properties, it is suitably used as a release film or process film for various members such as plastic products, building materials and optical members.
  • the required characteristics for the release film are appropriately set depending on the intended use, but in recent years, they may be used as a cover film for a resin layer having adhesiveness such as a photosensitive resin.
  • a cover film for a resin layer having adhesiveness such as a photosensitive resin.
  • the cover film is poorly releasable, it cannot be peeled cleanly when it is peeled off, and the shape of the resin layer that is the protective surface changes, or peeling marks remain on the protective surface Therefore, a film having a low surface free energy and good releasability is required.
  • the surface smoothness of a cover film is bad, when it uses, for example as a release film of an optical member, the surface unevenness
  • the cover film may interfere with a process inspection such as defect observation after bonding with the photosensitive resin.
  • a process inspection such as defect observation after bonding with the photosensitive resin.
  • Patent Document 1 As a means for improving releasability, for example, in Patent Document 1, the releasability is improved by roughening the surface such as a method of forming ⁇ crystals on the film surface layer or adding particles to the inner layer of the film. Although examples have been described, the surface smoothness and transparency were insufficient. Patent Documents 2 and 3 describe examples in which the release property is improved by adding a polymethylpentene resin to the film surface layer, but the surface smoothness and transparency are insufficient. It was. Further, Patent Document 4 describes an example in which the surface free energy is reduced by surface irregularities, but the releasability is insufficient. Moreover, since the unevenness is formed by coating or the like in post-processing, the cost may increase.
  • the object of the present invention is to solve the above-mentioned problems. That is, it is to provide a laminated polypropylene film excellent in releasability, surface smoothness, and transparency.
  • the laminated polypropylene film of the present invention is a laminated film having a surface layer (I) on at least one surface of a base material layer (II) mainly composed of polypropylene.
  • the surface free energy of the surface layer (I) is 18 to 28 mN / m, and the gloss value is 40% or more.
  • the laminated polypropylene film of the present invention is excellent in releasability, surface smoothness, and transparency, and therefore can be suitably used as a release film.
  • the laminated polypropylene film of the present invention is a laminated film having a surface layer (I) on at least one surface of a base material layer (II) mainly composed of polypropylene, and the surface free energy of the surface layer (I) is 18 to 28 mN / m.
  • the surface free energy is more preferably 18 to 27 mN / m, still more preferably 18 to 26 mN / m, and particularly preferably 18 to 25 mN / m.
  • Peeling marks may remain on the body surface.
  • it is effective to set the raw material composition of the film in the range described later and the film forming conditions in the range described later, and particularly to add a resin having a low surface free energy to the film surface layer. is there.
  • the gloss value of the surface layer (I) is 40% or more. More preferably, it is 80% or more, More preferably, it is 100% or more, Most preferably, it is 120% or more.
  • the gloss value is an index representing the glossiness, and has a high correlation with surface smoothness and transparency, and a higher value is preferable, but the upper limit is substantially about 155%.
  • the raw material composition of the film is set in the range described later, and the film forming conditions are set in the range described later.
  • the range in which the addition concentration of the low surface free energy added to the surface layer is described later
  • the compatibility between the resin with low surface free energy added to the surface layer and polypropylene resin is enhanced, the cooling conditions in casting are strengthened, and the formation of spherulites on the film surface is reduced as much as possible and the surface free energy It is effective to perform horizontal stretching and heat treatment at a temperature higher than the melting point of the low resin, to uniformly distribute the resin having a low surface free energy on the film surface layer, and to smooth the film surface.
  • the present invention improves the compatibility between the resin having a low surface free energy and the polypropylene resin, and further makes the film forming conditions described later to obtain polypropylene.
  • the present invention provides a polypropylene film having excellent releasability, surface smoothness, and transparency that cannot be achieved by conventional polypropylene films by controlling the crystal state of the film and suppressing a decrease in transparency in the stretching process. Is.
  • the laminated polypropylene film of the present invention preferably has a haze value of 50% or less. More preferably, it is 30% or less, more preferably 10% or less, and particularly preferably 3% or less. When the haze value exceeds 50%, since the transparency of the laminated film is low, it may be an obstacle when performing process inspection such as defect observation after bonding with the photosensitive resin.
  • the lower limit of the haze value is not particularly limited, but the lower limit is substantially about 0.1%.
  • the raw material composition of the film is set in the range described below, and the film forming conditions are set in the range described below. In particular, the compatibility between the resin having low surface free energy added to the surface layer and the polypropylene resin is set. It is effective to enhance the cooling conditions in the casting and casting, and to reduce the formation of spherulites on the film surface as much as possible.
  • the laminated polypropylene film of the present invention preferably has a heat shrinkage of 2.5% or less at 120 ° C. for 15 minutes in the longitudinal direction. More preferably, it is 2.2% or less, More preferably, it is 1.8% or less.
  • a direction parallel to the film forming direction is referred to as a film forming direction, a longitudinal direction, or an MD direction
  • a direction perpendicular to the film forming direction in the film plane is referred to as a width direction or a TD direction. If the thermal shrinkage in the longitudinal direction at 120 ° C for 15 minutes exceeds 2.5%, the film will deform and peel off, for example, when passing through a drying process where heat is applied after bonding with other materials. Or wrinkles.
  • the lower limit of the heat shrinkage rate is not particularly limited, but the film may swell, and the lower limit is substantially about ⁇ 2.0%.
  • the raw material composition of the film is set in the range described later, and the film forming conditions are set in the range described below, and in particular, the heat fixing and relaxation conditions after biaxial stretching are set in the range described below. Is effective.
  • the sum of the tear strength in the film longitudinal direction and the width direction is preferably 2.5 N / mm or more. More preferably, it is 3.0 N / mm or more, More preferably, it is 3.5 N / mm or more.
  • the tear strength correlates with the interlayer adhesion (adhesion between the surface layer (I) and the base material layer (II)) of the laminated film, and the higher the value, the better the interlayer adhesion.
  • the sum of the tear strength in the film longitudinal direction and the width direction is less than 2.5 N / mm, the interlayer adhesion is low, and when the film is transported or peeled from the photosensitive resin, the interlayer peeling occurs at the laminated film interface.
  • the upper limit of the sum of the tear strengths is not particularly limited, the upper limit is substantially 10 N / mm.
  • the raw material composition of the film is in the range described later, and the film forming conditions are in the range described later.
  • the compatibility between the resin having a low surface free energy added to the surface layer and the polypropylene resin is effective to increase the orientation of the film, for example, to increase the stretching ratio or to increase the draw ratio.
  • the thickness of the laminated polypropylene film of the present invention is appropriately adjusted depending on the application and is not particularly limited, but is preferably 0.5 ⁇ m or more and 100 ⁇ m or less. When the thickness is less than 0.5 ⁇ m, handling may be difficult, and when it exceeds 100 ⁇ m, the amount of resin may increase and productivity may decrease. Since the laminated polypropylene film of the present invention is excellent in tear strength even when the thickness is reduced, the handling property can be maintained. In order to make use of such characteristics, the thickness is more preferably 1 ⁇ m or more and 40 ⁇ m or less, further preferably 1 ⁇ m or more and 30 ⁇ m or less, and particularly preferably 1 ⁇ m or more and 15 ⁇ m or less. The thickness can be adjusted by the screw speed of the extruder, the width of the unstretched sheet, the film forming speed, the stretch ratio, and the like within a range not deteriorating other physical properties.
  • the surface layer (I) of the laminated polypropylene film of the present invention preferably comprises an olefin resin as a main component. More preferably, it is 90 mass% or more, More preferably, it is 95 mass% or more, Most preferably, it is 99 mass% or more.
  • the “main component” means that the proportion of the specific component in all the components is 50% by mass or more. Addition of non-olefin resins such as fluorine resin and silicon resin can be expected to improve releasability, but non-olefin resins are particularly low in compatibility with olefin resins such as polypropylene. In some cases, it is not uniformly dispersed in the resin and the surface smoothness and transparency may be impaired. From the above viewpoint, the surface layer (I) of the laminated polypropylene film of the present invention preferably comprises an olefin resin, and more preferably comprises an olefin resin as a main component.
  • the surface layer (I) of the laminated polypropylene film of the present invention is preferably an olefin resin in which a part of the olefin resin is a 4-methylpentene-1 unit, and 4-methyl-1- A pentene / ⁇ -olefin copolymer is more preferable.
  • Resin containing 4-methylpentene-1 unit has the effect of lowering the surface free energy, and has higher affinity with polypropylene resin than non-olefin resin, so that dispersibility in polypropylene resin can be improved. it can.
  • Examples of the olefin resin examples include TPX (registered trademark) DX310, TPX (registered trademark) DX231, and TPX (registered trademark) MX004 manufactured by Mitsui Chemicals, Inc. It can be illustrated. Further, 4-methyl-1-pentene / ⁇ -olefin copolymer is particularly preferably used because of its high compatibility with polypropylene resin.
  • the ⁇ -olefin is preferably a linear or branched ⁇ -olefin having 2 to 20 carbon atoms, more preferably 2 to 10 carbon atoms, and still more preferably 2 to 5 carbon atoms.
  • ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1-octene and the like can be mentioned, but not limited thereto.
  • a 4-methyl-1-pentene / ⁇ -olefin copolymer as disclosed in JP 2013-194132 A is preferably used.
  • the surface layer (I) contains an olefin resin containing 4-methylpentene-1 unit and having a melting point of 160 ° C. or less, and the melting point is 150 ° C. or less. More preferred.
  • An olefinic resin comprising 4-methylpentene-1 unit and a polypropylene resin have high affinity but are not compatible with each other, and thus form a domain like a sea-island structure. Due to the presence of this sea-island structure, unevenness in releasability may occur or transparent smoothness may be impaired.
  • the melting point of the olefin resin containing 4-methylpentene-1 unit is 160 ° C. or higher, voids are stretched at the domain interface of the sea-island structure by the olefin resin containing 4-methylpentene-1 unit and the polypropylene resin. May occur, and smoothness and transparency may be deteriorated.
  • the content of the olefin resin comprising 4-methylpentene-1 unit in the resin composition of the surface layer (I) is 0.1 to 15% by mass, or 85 to 100%. % By mass is preferable, and 0.1 to 10% by mass, or 90 to 100% by mass is more preferable.
  • the content of the olefin resin comprising 4-methylpentene-1 unit is higher than 15 mass% and lower than 85 mass%, the transparency and smoothness of the film may be impaired. The reason is estimated below. Transparency and smoothness are high when a polypropylene resin and an olefin-based resin containing 4-methylpentene-1 units are not blended and formed into films independently.
  • an olefin resin and a polypropylene resin containing 4-methylpentene-1 unit have high affinity but are not compatible with each other, and thus form a domain like a sea-island structure. Moreover, since both resin also differs in refractive index, it can be estimated that transparency and smoothness of a laminated film are impaired.
  • the olefin resin containing 4-methylpentene-1 unit should be 15% by mass or less, or conversely 85% by mass. This is achieved by the above.
  • each case will be described.
  • the thickness of the surface layer (I) it is preferable to set the thickness of the surface layer (I) to be thin so that an olefin-based resin containing many 4-methylpentene-1 units appears on the surface of the film of the surface layer (I). Further, by adding an olefin resin containing 4-methylpentene-1 unit having a melting point of 160 ° C.
  • the domain of the olefin resin comprising 4-methylpentene-1 unit is deformed flatly and distributed uniformly, so that no voids are formed at the interface. It becomes possible to improve releasability.
  • a technique in which an olefin resin containing 4-methylpentene-1 unit is kneaded with a polypropylene resin in advance to form a chip is also preferably used from the viewpoint of improving dispersibility.
  • the olefin-based resin containing 4-methylpentene-1 unit is 85% by mass or more, there is a concern that interfacial delamination may occur at the interface between the inner layer and the surface layer. It is preferable to use a technique for improving the above.
  • a technique for improving the above For example, in order to enhance the compatibility with the polypropylene resin used in the base material layer (II), a 4-methyl-1-pentene / ⁇ -olefin copolymer is used, or a butene polymer is used as the third component. The method to add is mentioned. Since the butene polymer has a high affinity for both polypropylene and 4-methylpentene-1 polymer, it is possible to improve the adhesive strength at the interface between the inner layer and the surface layer.
  • the surface layer (I) contains an olefin resin containing 4-methylpentene-1 unit having a melting point of 160 ° C. or less, and is subjected to transverse stretching at a temperature equal to or higher than the melting point to be melted by heat treatment.
  • voids hardly occur during stretching, and it becomes possible to improve transparency, smoothness and releasability.
  • a technique in which a polypropylene resin is preliminarily kneaded with an olefin resin containing 4-methylpentene-1 unit to form a chip is also preferably used from the viewpoint of improving dispersibility.
  • the raw materials used for the polypropylene laminated film of the present invention include antioxidants, heat stabilizers, antistatic agents, lubricants composed of inorganic or organic particles, and further anti-blocking agents and fillers as long as the effects of the present invention are not impaired.
  • Various additives such as an incompatible polymer may be contained.
  • an antioxidant for the purpose of suppressing oxidative deterioration of polypropylene or a resin having a low surface free energy. It is preferable that antioxidant content shall be 2 mass parts or less with respect to 100 mass parts of polypropylene compositions, More preferably, it is 1 mass part or less, More preferably, it is 0.5 mass part or less.
  • the polypropylene raw material is preferably polypropylene having a cold xylene soluble part (hereinafter CXS) of 4% by mass or less and a mesopentad fraction of 0.95 or more. If these conditions are not satisfied, the film-forming stability may decrease, and the tear strength of the film may decrease.
  • CXS cold xylene soluble part
  • the cold xylene soluble part refers to a polypropylene component dissolved in xylene when the film is completely dissolved in xylene and then deposited at room temperature, and has low stereoregularity. It is considered that the component which is difficult to crystallize due to a low molecular weight is applicable. If many such components are contained in the resin, the tear strength of the film may be reduced. Therefore, CXS is preferably 4% by mass or less, more preferably 3% by mass or less, and particularly preferably 2% by mass or less. CXS is preferably as low as possible, but about 0.1% by mass is the lower limit. In order to bring the CXS of the polypropylene resin within the above range, a method of increasing the catalytic activity in obtaining the resin, a method of washing the obtained resin with a solvent or propylene monomer itself, and the like can be used.
  • the mesopentad fraction of the polypropylene raw material is preferably 0.95 or more, more preferably 0.97 or more.
  • the mesopentad fraction is an index indicating the stereoregularity of the crystal phase of polypropylene measured by a nuclear magnetic resonance method (NMR method). The higher the numerical value, the higher the crystallinity, the higher the melting point, and the higher the temperature. It is preferable because it is suitable for use.
  • the upper limit of the mesopentad fraction is not particularly specified.
  • a method of washing resin powder obtained with a solvent such as n-heptane there are a method of appropriately selecting a catalyst and / or a promoter, and a composition. Preferably employed.
  • the polypropylene raw material is more preferably a melt flow rate (MFR) of 1 to 10 g / 10 minutes (230 ° C., 21.18 N load), particularly preferably 2 to 5 g / 10 minutes (230 ° C., 21.18 N load).
  • MFR melt flow rate
  • a method of controlling the average molecular weight or the molecular weight distribution is employed.
  • the polypropylene raw material may contain other unsaturated hydrocarbon copolymerization components or the like as long as the object of the present invention is not impaired, or may be blended with a polymer that is not propylene alone.
  • a copolymer component and a monomer component constituting the blend include ethylene, propylene (in the case of a copolymer blend), 1-butene, 1-pentene, 3-methylpentene-1, 3- Methylbutene-1,1-hexene, 4-methylpentene-1,5-ethylhexene-1,1-octene, 1-decene, 1-dodecene, vinylcyclohexene, styrene, allylbenzene, cyclopentene, norbornene, 5-methyl-2 -Norbornene and the like.
  • the copolymerization amount or blend amount is preferably less than 1 mol% in terms of copolymerization amount and less
  • the laminated polypropylene film of the present invention has a laminated structure having a surface layer (I) on at least one surface of a base material layer (II) containing polypropylene as a main component.
  • the thickness of the T 1 of the surface layer (I) when the base layer a thickness of (II) was T 2, it is preferable the value of T 1 / T 2 is 0.3 or less. More preferably, it is 0.2 or less, More preferably, it is 0.12 or less.
  • T 1 / T 2 exceeds 0.3, interfacial peeling at the laminated interface between the inner layer and the surface layer may occur or the transparent smoothness may be impaired.
  • the thickness T 1 of the front layer (I) is determined by measuring the surface free energy of each film surface of the A layer and the C layer, the thickness of the surface layer (a layer or C layer) of the lower layer to T 1.
  • raw materials for the surface layer (I) and the base material layer (II) are supplied to each single-screw extruder, and melt extrusion is performed at 200 to 260 ° C. Then, after removing foreign substances and modified polymer with a filter installed in the middle of the polymer tube, a multi-manifold type A layer / B layer / A layer composite T die has a lamination thickness ratio of 1/15/1, for example. And discharged onto a cast drum to obtain a laminated unstretched sheet having a layer configuration of A layer / B layer / A layer. At this time, the cast drum preferably has a surface temperature of 15 to 50 ° C.
  • any method among an electrostatic application method, an adhesion method using the surface tension of water, an air knife method, a press roll method, an underwater casting method, etc. may be used.
  • the air knife method is preferable.
  • the air temperature of the air knife is preferably 20 to 50 ° C.
  • the blowing air speed is preferably 130 to 150 m / s, and a double tube structure is preferable in order to improve the uniformity in the width direction. Further, it is preferable to appropriately adjust the position of the air knife so that air flows downstream of the film formation so as not to cause vibration of the film.
  • the obtained unstretched sheet is allowed to cool in the air and then introduced into the longitudinal stretching step.
  • an unstretched sheet is first brought into contact with a plurality of metal rolls maintained at 100 ° C. or more and less than 150 ° C., preheated to the stretching temperature, stretched 3 to 8 times in the longitudinal direction, and then cooled to room temperature. If the stretching temperature is 150 ° C. or more, stretching unevenness may occur or the film may break. On the other hand, if the draw ratio is less than 3 times, stretch unevenness may occur, the orientation of the film becomes weak, and the tear strength may decrease.
  • the longitudinally uniaxially stretched film is guided to a tenter, the end of the film is held with a clip, and the transverse stretching is stretched 7 to 13 times in the width direction at a temperature of 120 to 180 ° C, preferably 120 to 170 ° C.
  • the stretching temperature is low, the film may break, and it is preferable to stretch at a temperature equal to or higher than the melting point of the olefin resin containing 4-methyl-1-unit contained in the surface layer (I). Melting
  • the stretching temperature is too high, the rigidity of the film may decrease.
  • the magnification is high, the film may be broken, and when the magnification is low, the orientation of the film is weak and the tear strength may be lowered. Therefore, the upper limit is about 180 ° C.
  • the clip is heat-set at a temperature of 100 ° C. or more and less than 160 ° C. while being relaxed at a relaxation rate of 2 to 20% in the width direction while holding the clip in the width direction.
  • the film is guided to the outside of the tenter through a cooling process at 100 ° C., the clip at the film end is released, the film edge is slit in the winder process, and the film product roll is wound up.
  • Control of the conditions of the heat treatment and relaxation process is very important in adjusting the heat shrinkage rate.
  • the relaxation rate is more preferably 5 to 18%, still more preferably 8 to 15%.
  • the heat setting temperature is more preferably 120 ° C. or more and less than 160 ° C., and further preferably 140 ° C.
  • heat treatment is preferably performed at a temperature equal to or higher than the melting point of the olefin resin including 4-methyl-1-unit included in the surface layer (I), more preferably melting point + 10 ° C. or higher, and melting point + 20 ° C. or higher. Further preferred.
  • the laminated polypropylene film of the present invention obtained as described above can be used in various applications such as packaging films, release films, process films, sanitary products, agricultural products, building products, medical products, In particular, since it is excellent in releasability, it can be preferably used as a release film and a process film. Since it is excellent in especially transparent smoothness, it is preferably used as release films, such as a cover film of an adhesive resin layer.
  • ⁇ S, ⁇ Sd, ⁇ Sp, and ⁇ Sh are the surface free energy, dispersion force component, polar force component, and hydrogen bond component of the film surface, respectively
  • ⁇ L, ⁇ Ld, ⁇ Lp, and ⁇ Lh are the surface free energy and dispersion force of the measurement solution used, respectively. It represents a component, a polar force component, and a hydrogen bond component.
  • Panzer J. Panzer, J. Colloid Interface Sci., 44, 142 (1973)
  • Thermal shrinkage 120 ° C
  • the test piece is sandwiched between papers and taken out after heating for 15 minutes in an oven kept at 120 ° C. with zero load. After cooling at room temperature, the dimension (l 1 ) is measured with a universal projector and measured as follows.
  • Thermal contraction rate ⁇ (l 0 ⁇ l 1 ) / l 0 ⁇ ⁇ 100 (%)
  • the average value of the five samples was taken as the heat shrinkage rate.
  • Polyester adhesive tape NO. 31B was pasted with a roller, and it was cut into a width of 19 mm to prepare a sample. The sample was peeled off at a speed of 500 mm / min using a tensile tester and evaluated according to the following criteria.
  • C delamination occurs between the surface layer (I) and the base material layer (II), Alternatively, peeling is very heavy, and peeling marks remain on the adherend surface.
  • Acrylic adhesive (SK Dyne (registered trademark) 1310, manufactured by Soken Chemical Co., Ltd.) is diluted with ethyl acetate, toluene, and MEK on one side of the laminated polypropylene film, and the solid content of the adhesive is 100.
  • the coating material in which 2.0 parts by mass of a curing agent (Coronate D-90, manufactured by Nippon Polyurethane Industry Co., Ltd.) is mixed with the part by mass is hand-coated, dried in an oven at 80 ° C. for 30 seconds, and the adhesive layer thickness Produced a 1000 nm adhesive film.
  • a 40 ⁇ m thick “Zeonor Film” (registered trademark) manufactured by Nippon Zeon Co., Ltd. is sampled into a square with a width of 100 mm and a length of 100 mm, and the back surface of the adhesive film and the “Zeonor film” are placed in contact with each other. Then, it was sandwiched between two acrylic plates having a thickness of 5 mm, applied with a load of 2 kgf, and allowed to stand in an atmosphere at 23 ° C. for 24 hours. After 24 hours, the surface of the “ZEONOR film” (the surface on which the adhesive film was in contact) was visually observed and evaluated according to the following criteria. A: It is clean and is the same as before weighting. B: Weak unevenness is confirmed. C: Strong unevenness is confirmed.
  • Example 1 4 parts by mass of homopolypropylene (Prime Polymer Co., Ltd., TF850H, MFR: 2.9 g / 10 min) and 96 parts by mass of 4-methyl-1-pentene / propylene copolymer (melting point: 130 ° C.)
  • the raw material is supplied from the weighing hopper to the twin screw extruder so that it is mixed at a ratio, melt kneaded at 260 ° C, discharged from the die in a strand shape, cooled and solidified in a 25 ° C water bath, and cut into chips.
  • a polypropylene raw material (A) for the surface layer (I) was obtained.
  • the 4-methyl-1-pentene / propylene copolymer had a copolymerization ratio of 73 mol% for 4-methyl-1-pentene and 27 mol% for propylene.
  • the above-mentioned polypropylene raw material (A) is supplied to a uniaxial melt extruder for the surface layer (I), and the above-mentioned homopolypropylene ( TF850H) 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II), melt extruded at 260 ° C., foreign matter is removed with a 60 ⁇ m cut sintered filter, and feed block type A /
  • the laminate was laminated at a thickness ratio of 1/25/1 with a B / A composite T die, discharged onto a casting drum whose surface temperature was controlled at 18 ° C., and closely adhered to the casting drum with an air knife.
  • the uncooled drum surface of the sheet on the casting drum was cooled by injecting compressed air at a temperature of 25 ° C. and a pressure of 0.3 MPa to obtain an unstretched sheet.
  • the sheet was preheated to 125 ° C. using a ceramic roll, and stretched 4.5 times in the longitudinal direction of the film between 125 ° C. rolls provided with a peripheral speed difference.
  • the end is held by a clip and introduced into a tenter type stretching machine, preheated at 165 ° C. for 3 seconds, stretched 7.8 times in the width direction at 155 ° C., and given 13% relaxation in the width direction.
  • a heat treatment is performed at 158 ° C., followed by a cooling process at 100 ° C., and then led to the outside of the tenter, the film end clip is released, the film is wound around the core, and a laminated polypropylene film having a thickness of 11 ⁇ m (surface layer 0.4 ⁇ m) is obtained. Obtained.
  • Table 1 shows the physical properties and evaluation results of the laminated polypropylene film.
  • Example 2 94 parts by mass of the homopolypropylene (TF850H) and 6 parts by mass of the 4-methyl-1-pentene / propylene copolymer (melting point: 130 ° C.) were fed to a twin screw extruder and melt kneaded at 260 ° C. Then, it was discharged from the die in a strand shape, cooled and solidified in a 25 ° C. water bath, and cut into a chip shape to obtain a polypropylene raw material (B) for the surface layer (I).
  • TF850H homopolypropylene
  • 4-methyl-1-pentene / propylene copolymer melting point: 130 ° C.
  • the polypropylene raw material for the surface layer (I) is supplied to a uniaxial melt extruder for the surface layer (I), and the polypropylene raw material for the base layer (II) is used as the homopolypropylene ( TF850H) 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II), melt extruded at 260 ° C., foreign matter is removed with a 60 ⁇ m cut sintered filter, and feed block type A / The B / A composite T-die was laminated at a thickness ratio of 1/13/1, discharged onto a casting drum whose surface temperature was controlled at 23 ° C., and closely adhered to the casting drum with an air knife.
  • the uncooled drum surface of the sheet on the casting drum was cooled by injecting compressed air at a temperature of 25 ° C. and a pressure of 0.3 MPa to obtain an unstretched sheet.
  • the sheet was preheated to 130 ° C. using a ceramic roll, and stretched 4.7 times in the longitudinal direction of the film between 130 ° C. rolls provided with a peripheral speed difference.
  • the end is held by a clip and introduced into a tenter type stretching machine, preheated at 170 ° C. for 3 seconds, and then stretched 8.0 times in the width direction at 160 ° C., giving a relaxation of 12% in the width direction.
  • a heat treatment is performed at 155 ° C., and then a cooling process at 100 ° C.
  • Example 3 88 parts by mass of the homopolypropylene (TF850H) and 12 parts by mass of 4-methyl-1-pentene resin (manufactured by Mitsui Chemicals, DX310, melting point 232 ° C.) are fed to a twin screw extruder and melted at 260 ° C. Kneading was carried out, the strand was discharged from the die, solidified by cooling in a water bath at 25 ° C., and cut into chips to obtain a polypropylene raw material (C) for the surface layer (I).
  • TF850H homopolypropylene
  • 4-methyl-1-pentene resin manufactured by Mitsui Chemicals, DX310, melting point 232 ° C.
  • the polypropylene raw material (C) is supplied as a polypropylene raw material for the surface layer (I) to a uniaxial melt extruder for the surface layer (I), and the polypropylene raw material for the base layer (II) is the homopolypropylene ( TF850H) 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II), melt extruded at 260 ° C., foreign matter is removed with a 60 ⁇ m cut sintered filter, and feed block type A /
  • the layers were laminated at a thickness ratio of 1/25/1 by a B / A composite T die, discharged onto a casting drum whose surface temperature was controlled at 33 ° C., and adhered to the casting drum with an air knife.
  • the uncooled drum surface of the sheet on the casting drum was cooled by injecting compressed air at a temperature of 30 ° C. and a pressure of 0.3 MPa to obtain an unstretched sheet.
  • the sheet was preheated to 138 ° C. using a ceramic roll, and stretched 4.8 times in the longitudinal direction of the film between 138 ° C. rolls provided with a peripheral speed difference.
  • the end is held by a clip and introduced into a tenter-type stretching machine, preheated at 171 ° C. for 3 seconds, stretched 8.0 times in the width direction at 166 ° C., and given 10% relaxation in the width direction.
  • a heat treatment is performed at 143 ° C., and then a cooling process at 100 ° C.
  • Example 4 5 parts by mass of the homopolypropylene (TF850H), 90 parts by mass of 4-methyl-1-pentene resin (manufactured by Mitsui Chemicals, MX004, melting point 228 ° C.), polybutene-1 resin (manufactured by Mitsui Chemicals, P5050N) ) 5 parts by mass of raw material is fed to a twin screw extruder, melt kneaded at 260 ° C., discharged from a die in a strand shape, cooled and solidified in a 25 ° C. water tank, cut into a chip shape, and surface layer (I Polypropylene raw material (D) was obtained.
  • TF850H homopolypropylene
  • 4-methyl-1-pentene resin manufactured by Mitsui Chemicals, MX004, melting point 228 ° C.
  • polybutene-1 resin manufactured by Mitsui Chemicals, P5050N
  • the polypropylene raw material (D) is supplied as a polypropylene raw material for the surface layer (I) to a uniaxial melt extruder for the surface layer (I), and the polypropylene raw material for the base layer (II) is the homopolypropylene ( TF850H) 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II), melt extruded at 260 ° C., foreign matter is removed with a 60 ⁇ m cut sintered filter, and feed block type A / They were laminated with a B / A composite T die at a thickness ratio of 1/14/1, discharged onto a casting drum whose surface temperature was controlled at 23 ° C., and adhered to the casting drum with an air knife.
  • TF850H homopolypropylene
  • the uncooled drum surface of the sheet on the casting drum was cooled by injecting compressed air at a temperature of 25 ° C. and a pressure of 0.3 MPa to obtain an unstretched sheet.
  • the sheet was preheated to 135 ° C. using a ceramic roll, and stretched 5.2 times in the longitudinal direction of the film between 135 ° C. rolls provided with a difference in peripheral speed.
  • the end part is introduced into a tenter type stretching machine by holding a clip, preheated at 168 ° C. for 3 seconds, and then stretched 8.0 times in the width direction at 163 ° C., giving a relaxation of 6% in the width direction.
  • a heat treatment is performed at 138 ° C., and then a cooling process at 100 ° C. is conducted to the outside of the tenter.
  • a clip at the end of the film is released, the film is wound around a core, and a laminated polypropylene film having a thickness of 18 ⁇ m (surface layer: 1.3 ⁇ m) is obtained. Obtained.
  • Table 1 shows the physical properties and evaluation results of the laminated polypropylene film.
  • Example 5 9 parts by mass of the homopolypropylene (TF850H), 86 parts by mass of 4-methyl-1-pentene resin (Mitsui Chemicals, MX004, melting point 228 ° C.), polybutene-1 resin (Mitsui Chemicals, P5050N) ) 5 parts by mass of raw material is fed to a twin screw extruder, melt kneaded at 260 ° C., discharged from a die in a strand shape, cooled and solidified in a 25 ° C. water tank, cut into a chip shape, and surface layer (I ) Polypropylene raw material (E) was obtained.
  • the polypropylene raw material (E) is supplied as a polypropylene raw material for the surface layer (I) to a uniaxial melt extruder for the surface layer (I), and the polypropylene raw material for the base layer (II) is the homopolypropylene ( TF850H) 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II), melt extruded at 260 ° C., foreign matter is removed with a 60 ⁇ m cut sintered filter, and feed block type A / A B / A composite T die was laminated at a thickness ratio of 1/6/1, discharged onto a casting drum whose surface temperature was controlled at 52 ° C., and adhered to the casting drum with an air knife.
  • the uncooled drum surface of the sheet on the casting drum was cooled by injecting compressed air at a temperature of 30 ° C. and a pressure of 0.3 MPa to obtain an unstretched sheet.
  • the sheet was preheated to 140 ° C. using a ceramic roll, and the film was stretched 4.6 times in the longitudinal direction of the film between 140 ° C. rolls provided with a peripheral speed difference.
  • the end is held by a clip and introduced into a tenter type stretching machine, preheated at 171 ° C. for 3 seconds, stretched 7.6 times in the width direction at 166 ° C., and given 15% relaxation in the width direction.
  • a heat treatment is performed at 156 ° C., and then a cooling process at 100 ° C.
  • Example 6 10 parts by mass of homopolypropylene (Prime Polymer Co., Ltd., TF850H, MFR: 2.9 g / 10 min) and 90 parts by mass of 4-methyl-1-pentene / propylene copolymer (melting point: 130 ° C.)
  • the raw material is supplied from the weighing hopper to the twin screw extruder so that it is mixed at a ratio, melt kneaded at 260 ° C, discharged from the die in a strand shape, cooled and solidified in a 25 ° C water bath, and cut into chips.
  • a polypropylene raw material (A) for the surface layer (I) was obtained.
  • the 4-methyl-1-pentene / propylene copolymer had a copolymerization ratio of 73 mol% for 4-methyl-1-pentene and 27 mol% for propylene.
  • the above-mentioned polypropylene raw material (A) is supplied to a uniaxial melt extruder for the surface layer (I), and the above-mentioned homopolypropylene ( TF850H) 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II), melt extruded at 260 ° C., foreign matter is removed with a 60 ⁇ m cut sintered filter, and feed block type A /
  • the layers were laminated at a thickness ratio of 1/22/1 with a B / A composite T die, discharged onto a casting drum whose surface temperature was controlled at 24 ° C., and adhered to the casting drum with an air knife.
  • the uncooled drum surface of the sheet on the casting drum was cooled by injecting compressed air at a temperature of 25 ° C. and a pressure of 0.3 MPa to obtain an unstretched sheet.
  • the sheet was preheated to 130 ° C. using a ceramic roll, and stretched 4.4 times in the longitudinal direction of the film between 130 ° C. rolls provided with a peripheral speed difference.
  • the end is held by a clip and introduced into a tenter type stretching machine, preheated at 138 ° C. for 3 seconds, stretched 7.7 times in the width direction at 138 ° C., and given 7% relaxation in the width direction.
  • a heat treatment is performed at 139 ° C., and then a cooling process at 100 ° C.
  • the above-mentioned polypropylene raw material (F) is supplied to a uniaxial melt extruder for the surface layer (I), and the above-mentioned homopolypropylene ( RF1342B) 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II), melt extruded at 230 ° C., foreign matter is removed with a 60 ⁇ m cut sintered filter, and feed block type A /
  • the layers were laminated with a B / A composite T die at a thickness ratio of 1/10/1, discharged onto a casting drum whose surface temperature was controlled at 30 ° C., and adhered to the casting drum with an air knife.
  • the uncooled drum surface of the sheet on the casting drum was cooled by injecting compressed air at a temperature of 30 ° C. and a pressure of 0.3 MPa to obtain an unstretched sheet.
  • sequential biaxial stretching was performed using a batch type biaxial stretching machine KARO IV manufactured by Bruckner.
  • the stretching conditions were a preheating temperature of 165 ° C., a preheating time of 1 minute, a stretching temperature of 165 ° C., a stretching speed of 100% / sec, and a heat setting condition of 165 ° C. and 30 sec.
  • the laminated polypropylene film having a thickness of 12 ⁇ m was obtained by stretching 4.5 times and a stretching ratio in the width direction of 9 times.
  • Table 1 shows the physical properties and evaluation results of the laminated polypropylene film.
  • the above-mentioned polypropylene raw material (G) is supplied to a uniaxial melt extruder for the surface layer (I)
  • the above-mentioned homopolypropylene ( RF1342B) 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II)
  • melt extruded at 230 ° C., foreign matter is removed with a 60 ⁇ m cut sintered filter, and feed block type A /
  • the layers were laminated at a thickness ratio of 1/23/1 with a B / A composite T die, discharged onto a casting drum whose surface temperature was controlled at 30 ° C., and adhered to the casting drum with an air knife.
  • the uncooled drum surface of the sheet on the casting drum was cooled by injecting compressed air at a temperature of 30 ° C. and a pressure of 0.3 MPa to obtain an unstretched sheet.
  • sequential biaxial stretching was performed using a batch type biaxial stretching machine KARO IV manufactured by Bruckner. Stretching conditions are a preheating temperature of 162 ° C, a preheating time of 2 minutes, a stretching temperature of 162 ° C, a stretching speed of 100% / sec, and a heat setting condition of 162 ° C and 30 sec.
  • the biaxially stretched polypropylene film having a thickness of 20 ⁇ m was obtained by stretching 5 times and a stretching ratio in the width direction of 9 times.
  • Table 1 shows the physical properties and evaluation results of the laminated polypropylene film.
  • the mixture was melt-kneaded at 300 ° C., discharged from a die in a strand shape, cooled and solidified in a water bath at 25 ° C., and cut into chips to obtain a polypropylene raw material (H) for the surface layer (I).
  • the polypropylene raw material (H) is supplied to the uniaxial melt extruder for the surface layer (I) as the polypropylene raw material for the surface layer (I), and homopolypropylene (TF850H is used as the polypropylene raw material for the base layer (II).
  • 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II), melt extruded at 240 ° C., foreign matter is removed with a 60 ⁇ m cut sintered filter, and then a feed block type A / B A cast sheet was obtained by laminating with a composite T die at a thickness ratio of 8/1 and discharging onto a cast drum whose surface temperature was controlled at 90 ° C.
  • the film was preheated to 125 ° C. using a plurality of ceramic rolls and stretched 4.6 times in the longitudinal direction of the film.
  • the end portion was introduced into a tenter-type stretching machine by holding it with a clip, preheated at 165 ° C. for 3 seconds, and then stretched 8.0 times at 160 ° C.
  • heat treatment is performed at 160 ° C while giving 10% relaxation in the width direction, and then the cooling process is performed at 130 ° C, leading to the outside of the tenter, releasing the clip at the end of the film, and winding the film around the core
  • a laminated polypropylene film having a thickness of 15 ⁇ m (surface layer 1.7 ⁇ m) was obtained.
  • the polypropylene raw material (J) is supplied to the uniaxial melt extruder for the base material layer (II) as the polypropylene raw material for the base material layer (II), and homopolypropylene is used as the polypropylene raw material for the surface layer (I).
  • TF850H 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II), melt extruded at 240 ° C., and foreign matter is removed by a 60 ⁇ m cut sintered filter. / B composite T-die was laminated at a thickness ratio of 8/1, and discharged onto a cast drum whose surface temperature was controlled at 30 ° C. to obtain a cast sheet.
  • the film was preheated to 125 ° C. using a plurality of ceramic rolls and stretched 4.6 times in the longitudinal direction of the film.
  • the end portion was introduced into a tenter-type stretching machine by holding it with a clip, preheated at 165 ° C. for 3 seconds, and then stretched 8.0 times at 160 ° C.
  • the sheet was preheated to 140 ° C. using a ceramic roll, and the film was stretched 4.6 times in the longitudinal direction of the film between 140 ° C. rolls provided with a peripheral speed difference.
  • the end is held by a clip and introduced into a tenter type stretching machine, preheated at 165 ° C. for 3 seconds, stretched 8 times in the width direction at 160 ° C., and 155 ° C. while giving 10% relaxation in the width direction.
  • the film was then subjected to a heat treatment and then led to the outside of the tenter through a cooling process at 100 ° C., the clip at the end of the film was released, and the film was wound around a core to obtain a laminated polypropylene film having a thickness of 19 ⁇ m.
  • Table 1 shows the physical properties and evaluation results of the laminated polypropylene film.
  • the above-mentioned polypropylene raw material (A) is supplied to a uniaxial melt extruder for the surface layer (I), and the above-mentioned homopolypropylene ( (FL1105C) 100 parts by mass is supplied to a uniaxial melt extruder for the base material layer (II), melt extruded at 260 ° C., and foreign matter is removed by a 60 ⁇ m cut sintered filter.
  • the layers were laminated with a B / A composite T die at a thickness ratio of 1/10/1, discharged onto a casting drum whose surface temperature was controlled at 25 ° C., and adhered to the casting drum with an air knife.
  • the uncooled drum surface of the sheet on the casting drum was cooled by injecting compressed air at a temperature of 25 ° C. and a pressure of 0.3 MPa to obtain an unstretched sheet.
  • the sheet was preheated to 140 ° C. using a ceramic roll, and stretched 4.8 times in the longitudinal direction of the film between 140 ° C. rolls provided with a peripheral speed difference.
  • the end of the tenter type stretching machine is introduced by gripping with a clip, preheated at 160 ° C. for 3 seconds, and then stretched 9.0 times in the width direction at 160 ° C., giving 5% relaxation in the width direction.
  • the laminated polypropylene film of the present invention can be used in various applications such as a packaging film, a release film, a process film, a sanitary product, an agricultural product, a building product, and a medical product.
  • a packaging film a release film
  • a process film a sanitary product
  • an agricultural product a building product
  • a medical product a medical product.
  • it since it is excellent in transparent smoothness, it can be preferably used as a release film and process film for applications requiring surface smoothness of products, and since it is excellent in releasability, it also covers an adhesive resin layer. It is preferably used as a release film such as a film.

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  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Laminated Bodies (AREA)
  • Shaping By String And By Release Of Stress In Plastics And The Like (AREA)

Abstract

L'invention a pour objet de fournir un film de polypropylène stratifié doté d'excellentes propriétés de décollage, de lissé de surface et de transparence. Plus précisément, l'invention concerne un film de polypropylène stratifié qui consiste en un film stratifié possédant une couche superficielle (I) sur au moins une surface d'une couche de matériau de base (II) ayant un polypropylène pour composant principal, et qui est telle que la tension superficielle de la couche superficielle (I) est comprise entre １８ et ２８ｍＮ／ｍ, et la valeur de brillance est supérieure ou égale à 40%.
PCT/JP2017/041940 2016-11-25 2017-11-22 Film de polypropylène stratifié WO2018097161A1 (fr)

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CN115243890B (zh) * 2020-03-27 2024-08-20 三井化学株式会社 层叠体、使用其的辊体和包装体
KR102413401B1 (ko) * 2020-05-08 2022-06-27 주식회사 아랑씨엔에이치 후지를 포함하지 않는 라미네이팅 필름 및 그 제조방법
WO2021256347A1 (fr) * 2020-06-17 2021-12-23 東洋紡株式会社 Film de polypropylène à orientation biaxiale
CN115698148B (zh) * 2020-06-17 2024-05-24 东洋纺株式会社 双轴取向聚丙烯薄膜
CN114425897A (zh) * 2022-04-06 2022-05-03 广东德冠薄膜新材料股份有限公司 可模压可镀金属聚丙烯薄膜及其制备方法和应用

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