WO2021193510A1 - Film de polypropylène à orientation biaxiale - Google Patents

Film de polypropylène à orientation biaxiale Download PDF

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Publication number
WO2021193510A1
WO2021193510A1 PCT/JP2021/011662 JP2021011662W WO2021193510A1 WO 2021193510 A1 WO2021193510 A1 WO 2021193510A1 JP 2021011662 W JP2021011662 W JP 2021011662W WO 2021193510 A1 WO2021193510 A1 WO 2021193510A1
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Prior art keywords
biaxially oriented
film
oriented polypropylene
polypropylene film
width direction
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PCT/JP2021/011662
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English (en)
Japanese (ja)
Inventor
今井　徹
山田　浩司
一仁 堀之内
麻洋 中野
健一 船城
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東洋紡株式会社
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Priority to JP2021549127A priority Critical patent/JPWO2021193510A1/ja
Publication of WO2021193510A1 publication Critical patent/WO2021193510A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
    • B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
    • B29C55/10—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial
    • B29C55/12—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets multiaxial biaxial
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets

Definitions

  • the present invention relates to a biaxially oriented polypropylene film having excellent rigidity and heat resistance. More specifically, the present invention relates to a biaxially oriented polypropylene film that can be suitably used for a packaging bag because it easily retains the shape of the packaging bag and has few wrinkles in the sealed portion when heat-sealed.
  • Biaxially oriented polypropylene film is used for packaging and industrial applications because it has moisture resistance and the required rigidity and heat resistance. In recent years, as the applications used have expanded, higher performance has been required, and in particular, improvement in rigidity is expected. Further, from the consideration of the environment, it is required to maintain the strength even if the volume is reduced (the film thickness is thinned), but for that purpose, it is indispensable to remarkably improve the rigidity. As a means for improving the rigidity, it is known that the crystallinity and melting point of the polypropylene resin are improved by improving the catalyst and the process technology at the time of polymerization of the polypropylene resin. Until now, there was no biaxially oriented polypropylene film having sufficient rigidity.
  • the first stage heat treatment is performed while relaxing the film at a temperature lower than the temperature at the time of width direction stretching, and the second stage heat treatment is performed at the first stage temperature to the width direction stretching temperature.
  • Patent Document 1 and the like a method of further stretching in the longitudinal direction after stretching in the width direction
  • Patent Document 2 and the like a method of further stretching in the longitudinal direction after stretching in the width direction
  • the film described in Patent Document 2 is excellent in rigidity, wrinkles are likely to occur in the sealed portion after heat sealing, and the heat resistance is inferior.
  • the orientation of the film described in Patent Document 1 is low, and the rigidity is not sufficient.
  • An object of the present invention is to solve the above-mentioned problems. That is, the present invention relates to a biaxially oriented polypropylene film having excellent film rigidity and heat resistance at a high temperature of 150 ° C. More specifically, it is an object of the present invention to provide a biaxially oriented polypropylene film which can easily maintain the shape of a packaging bag and has less wrinkles in and around the sealing portion when heat-sealed.
  • the present inventors have made a biaxially oriented polypropylene film satisfying the following (1) to (3), thereby increasing the rigidity of the film and heat resistance at a high temperature of 150 ° C. It has been found that a biaxially oriented polypropylene film having excellent properties can be obtained.
  • (1) When the film is constrained in all directions and the temperature is raised from 40 ° C. to 180 ° C. at a rate of 10 ° C./min, X-rays are incident in the direction perpendicular to the film surface, and wide-angle X-ray diffraction measurement is performed.
  • the ratio of the value to the maximum intensity at 40 ° C. ((110) intensity ratio) is 115% or more.
  • the degree of orientation in the width direction is 0.85 or more.
  • the heat shrinkage rate at 150 ° C. is 10% or less in the longitudinal direction and 30% or less in the width direction.
  • the ratio (E “ h / E” g ) of the maximum value (E “ h ) to the maximum value (E” g ) of the loss elastic modulus (E ") between -25 ° C and 25 ° C is 70% or more. It is preferable to have.
  • the tensile elongation at break of the biaxially oriented polypropylene film is 25% or more in the longitudinal direction and 195% or more in the width direction at 23 ° C.
  • the heat shrinkage rate of the biaxially oriented polypropylene film at 120 ° C. is 2.0% or less in the longitudinal direction, 5.0% or less in the width direction, and 120 ° C. heat shrinkage in the longitudinal direction. It is preferable that the rate is smaller than the 120 ° C. heat shrinkage rate in the width direction.
  • the refractive index Ny in the longitudinal direction of the biaxially oriented polypropylene film is 1.5230 or more and ⁇ Ny is 0.0220 or more.
  • the haze of the biaxially oriented polypropylene film is 5.0% or less.
  • the mesopentad fraction of the polypropylene resin constituting the biaxially oriented polypropylene film is 97.0% or more.
  • the polypropylene resin constituting the biaxially oriented polypropylene film has a crystallization temperature of 105 ° C. or higher and a melting point of 161 ° C. or higher.
  • the melt flow rate of the polypropylene resin constituting the biaxially oriented polypropylene film is 4.0 g / 10 minutes or more.
  • the component amount of the polypropylene resin constituting the biaxially oriented polypropylene film having a molecular weight of 100,000 or less is 35% by mass or more.
  • the biaxially oriented polypropylene film of the present invention has high rigidity and excellent heat resistance at a high temperature of 150 ° C., it is easy to maintain the bag shape when it is used as a packaging bag, and wrinkles of the sealed portion when heat-sealed.
  • a biaxially oriented polypropylene film that can be suitably used for packaging bags can be obtained.
  • the biaxially oriented polypropylene film is also excellent in rigidity, the strength can be maintained even if the thickness of the film is reduced, and it can be suitably used for applications requiring higher rigidity. ..
  • the diffraction intensity ratio-temperature curve based on is shown.
  • the elastic modulus-temperature curve in the width direction of the films obtained in Example 1, Comparative Example 1, and Comparative Example 2 is shown.
  • the biaxially oriented polypropylene film of the present invention comprises a polypropylene resin composition containing a polypropylene resin as a main component.
  • the "main component” means that the proportion of the polypropylene resin in the polypropylene resin composition is 90% by mass or more, more preferably 93% by mass or more, still more preferably 95% by mass or more, and particularly preferably. Is 97% by mass or more.
  • Polypropylene resin As the polypropylene resin used in the present invention, a polypropylene homopolymer or a copolymer with ethylene and / or an ⁇ -olefin having 4 or more carbon atoms can be used.
  • a propylene homopolymer substantially free of ethylene and / or an ⁇ -olefin having 4 or more carbon atoms is preferable, and even when ethylene and / or an ⁇ -olefin component having 4 or more carbon atoms is contained, ethylene and / or
  • the amount of the ⁇ -olefin component having 4 or more carbon atoms is preferably 1 mol% or less, more preferably 0.5 mol% or less, still more preferably 0.3 mol% or less, and particularly preferably 0. It is 1 mol or less. Within the above range, crystallinity tends to improve.
  • Examples of the ⁇ -olefin component having 4 or more carbon atoms constituting such a copolymer include 1-butene, 1-pentene, 3-methylpentene-1, 3-methylbutene-1, 1-hexene, and 4-methyl. Examples thereof include pentene-1,5-ethylhexene-1,1-octene, 1-decene, 1-dodecene, 1-tetradecene, 1-hexadecene, 1-heptadecene, 1-octadecene, 1-eicosene and the like.
  • the polypropylene resin two or more different polypropylene homopolymers, a copolymer with ethylene and / or an ⁇ -olefin having 4 or more carbon atoms, and a mixture thereof can be used.
  • the mesopentad fraction ([mmmm]%) which is an index of the stereoregularity of the polypropylene resin used in the present invention, is preferably in the range of 97.0 to 99.9%, preferably 97.5 to 99.7. It is more preferably in the range of%, further preferably in the range of 98.0 to 99.5%, and particularly preferably in the range of 98.5 to 99.3%.
  • it is 97.0% or more, the crystallinity of the polypropylene resin is enhanced, the melting point, crystallinity, and crystallinity of the crystals in the film are improved, and rigidity and heat resistance at high temperature can be easily obtained.
  • the mesopentad fraction is measured by a nuclear magnetic resonance method (so-called NMR method). More preferably, it is 99.5% or less.
  • the mesopentad fraction is measured by a nuclear magnetic resonance method (so-called NMR method).
  • NMR method nuclear magnetic resonance method
  • a method of washing the obtained polypropylene resin powder with a solvent such as n-heptane, selection of a catalyst and / or a co-catalyst, and a polypropylene resin composition A method of appropriately selecting the components is preferably adopted.
  • the lower limit of the melting temperature (Tm) measured by DSC of the polypropylene resin constituting the biaxially oriented polypropylene film of the present invention is preferably 160 ° C., more preferably 161 ° C., and further preferably 162 ° C. , More preferably 163 ° C, even more preferably 164 ° C.
  • Tm melting temperature
  • the upper limit of Tm is preferably 170 ° C., more preferably 169 ° C., even more preferably 168 ° C., even more preferably 167 ° C., and particularly preferably 166 ° C.
  • Tm is 170 ° C.
  • the melting temperature can be further raised by blending the crystal nucleating agent with the polypropylene resin described above.
  • Tm is a sample of 1 to 10 mg packed in an aluminum pan, set in a differential scanning calorimeter (DSC), melted at 230 ° C for 5 minutes in a nitrogen atmosphere, and up to 30 ° C at a scanning speed of -10 ° C / min. This is the main peak temperature of the endothermic peak associated with melting, which is observed when the temperature is lowered, held for 5 minutes, and the temperature is raised at a scanning speed of 10 ° C./min.
  • DSC differential scanning calorimeter
  • the lower limit of the crystallization temperature (Tc) measured by DSC of the polypropylene resin constituting the biaxially oriented polypropylene film of the present invention is 105 ° C., preferably 108 ° C., and more preferably 110 ° C.
  • Tc crystallization temperature measured by DSC of the polypropylene resin constituting the biaxially oriented polypropylene film of the present invention
  • the upper limit of Tc is preferably 135 ° C., more preferably 133 ° C., still more preferably 132 ° C., even more preferably 130 ° C., particularly preferably 128 ° C., and most preferably 127 ° C. Is.
  • Tc is 135 ° C. or lower, it is difficult to increase the cost in terms of polypropylene production, and it is difficult to break during film formation.
  • the crystallization temperature can be further raised by blending the crystal nucleating agent with the polypropylene resin described above. Tc is observed when a sample of 1 to 10 mg is packed in an aluminum pan, set in a DSC, melted at 230 ° C. for 5 minutes in a nitrogen atmosphere, and cooled to 30 ° C. at a scanning speed of -10 ° C./min. This is the main peak temperature of the exothermic peak.
  • the melt flow rate (MFR) of the polypropylene resin constituting the biaxially oriented polypropylene film of the present invention is 4 when measured in accordance with the condition M (230 ° C., 2.16 kgf) of JIS K 7210 (1995). It is preferably 0.0 to 30 g / 10 minutes, more preferably 4.5 to 25 g / 10 minutes, further preferably 4.8 to 22 g / 10 minutes, and 5.0 to 20 g / 10 minutes. It is particularly preferable to have it, and it is most preferably 6.0 to 20 g / 10 minutes.
  • melt flow rate (MFR) of the polypropylene resin is 4.0 g / 10 minutes or more, it is easy to obtain a biaxially oriented polypropylene film having a low heat shrinkage rate. Further, when the melt flow rate (MFR) of the polypropylene resin is 30 g / 10 minutes or less, it is easy to maintain the film-forming property of the film.
  • the lower limit of the melt flow rate (MFR) (230 ° C., 2.16 kgf) of the polypropylene resin constituting the film is preferably 5.0 g / 10 minutes, more preferably 5.5 g / 10 minutes. It is more preferably 6.0 g / 10 minutes, particularly preferably 6.3 g / 10 minutes, and most preferably 6.5 g / 10 minutes.
  • MFR melt flow rate
  • the orientation crystallization of the polypropylene resin is further promoted, the degree of crystallization in the film is more likely to be increased, and the polypropylene molecular chains in the amorphous portion are less entangled with each other, resulting in heat resistance. It is easier to improve sex.
  • MFR melt flow rate
  • the lower limit of the amount of the component having a molecular weight of 100,000 or less in the GPC integration curve of the polypropylene resin constituting the film of the present invention is 35% by mass, preferably 38% by mass, and more preferably 40% by mass. It is more preferably 41% by mass, and particularly preferably 42% by mass.
  • the upper limit of the amount of the component having a molecular weight of 100,000 or less on the GPC integration curve is preferably 65% by mass, more preferably 60% by mass, and further preferably 58% by mass. When the amount of the component having a molecular weight of 100,000 or less in the GPC integration curve is 65% by mass or less, the film strength is unlikely to decrease.
  • the amount of the component having a molecular weight of 100,000 or less contained in the polypropylene resin can be easily adjusted without significantly changing the overall viscosity, so that the rigidity is increased. It is easy to improve the film-forming property without affecting the heat shrinkage.
  • the polypropylene resin used in the present invention has a lower limit of mass average molecular weight (Mw) / number average molecular weight (Mn), which is an index of the breadth of molecular weight distribution, preferably 3.5, more preferably 4, and further. It is preferably 4.5, and particularly preferably 5.
  • the upper limit of Mw / Mn is preferably 30, more preferably 25, still more preferably 23, particularly preferably 21 and most preferably 20.
  • Mw / Mn can be obtained using gel permeation chromatography (GPC). When Mw / Mn is in the above range, it is easy to increase the amount of the component having a molecular weight of 100,000 or less.
  • the shape of the molecular weight distribution obtained by GPC has a single peak in a GPC chart in which the horizontal axis is the logarithm of the molecular weight (M) (logM) and the vertical axis is the differential distribution value (weight fraction per logM). It may have a gentle molecular weight distribution, or it may have a molecular weight distribution having a plurality of peaks and shoulders.
  • the biaxially oriented polypropylene film of the present invention is preferably obtained by preparing an unstretched sheet made of the polypropylene resin composition containing the above-mentioned polypropylene resin as a main component and biaxially stretching the film.
  • a biaxial stretching method any of the inflation simultaneous biaxial stretching method, the tenter simultaneous biaxial stretching method, and the tenter sequential biaxial stretching method can be obtained, but from the viewpoint of film forming stability and thickness uniformity, the tenter sequential biaxial stretching method can be obtained.
  • a layer having another function may be laminated on at least one side. It may be laminated on one side or both sides.
  • the polypropylene resin composition described above may be used as the resin composition of the other one layer or the central layer. Further, it may be different from the polypropylene resin composition described above.
  • the number of layers to be laminated may be one layer, two layers, three layers or more per one side, but one layer or two layers is preferable from the viewpoint of production.
  • a laminating method for example, coextrusion by a feed block method or a multi-manifold method is preferable.
  • a resin layer having a heat-sealing property can be laminated within a range that does not deteriorate the characteristics.
  • one side or both sides may be subjected to corona treatment.
  • the tenter sequential biaxial stretching method is adopted as an example in the case of a single layer.
  • the resin composition containing the polypropylene resin is heated and melted by a single-screw or twin-screw extruder, extruded into a sheet from a T-die, and grounded on a cooling roll to be cooled and solidified.
  • a cooling roll For the purpose of promoting solidification, it is preferable to further cool the sheet cooled by a cooling roll by immersing it in a water tank or the like.
  • the sheet is stretched in the longitudinal direction by increasing the number of rotations of the rear stretching rolls with two pairs of stretching rolls in which the sheet is heated to obtain a uniaxially stretched film.
  • the uniaxially stretched film is stretched in the width direction at a specific temperature while grasping the end of the film with a tenter type stretching machine to obtain a biaxially stretched film.
  • This width direction stretching step will be described in detail later.
  • the biaxially stretched film is heat-treated at a specific temperature to obtain a biaxially oriented film.
  • the film may be relaxed in the width direction.
  • the biaxially oriented polypropylene film thus obtained is subjected to, for example, corona discharge treatment on at least one side, and then wound with a winder to obtain a film roll.
  • the cooling temperature is 50 ° C. or lower, the transparency of the unstretched sheet tends to increase, preferably 40 ° C. or lower, and more preferably 30 ° C. or lower.
  • the cooling temperature is preferably 40 ° C. or higher, but as described above, a propylene homopolymer having a mesopendat fraction of 97.0% or higher is used. In this case, the cooling temperature is preferably 40 ° C.
  • the thickness of the unstretched sheet is preferably 3500 ⁇ m or less, more preferably 3000 ⁇ m or less in terms of cooling efficiency, and can be appropriately adjusted according to the film thickness after sequential biaxial stretching.
  • the thickness of the unstretched sheet can be controlled by the extrusion speed of the polypropylene resin composition, the lip width of the T-die, and the like.
  • the lower limit of the longitudinal stretching ratio is preferably 3 times, more preferably 3.5 times, and particularly preferably 3.8 times. Within the above range, the strength can be easily increased and the film thickness unevenness can be reduced.
  • the upper limit of the longitudinal stretching ratio is preferably 8 times, more preferably 7.5 times, and particularly preferably 7 times. Within the above range, the width direction stretching in the width direction stretching step is easy, and the productivity is improved.
  • the lower limit of the longitudinal stretching temperature is preferably Tm-40 ° C, more preferably Tm-37 ° C, and even more preferably Tm-35 ° C. Within the above range, the subsequent stretching in the width direction becomes easy and the thickness unevenness is reduced.
  • the upper limit of the longitudinal stretching temperature is preferably Tm-7 ° C, more preferably Tm-10 ° C, and even more preferably Tm-12 ° C.
  • the longitudinal stretching may be performed by using three or more pairs of stretching rolls and stretching in two or more stages.
  • the width direction stretching step it is preferable to stretch at a temperature of Tm-10 ° C. or higher and a preheating temperature or lower.
  • the start of stretching in the width direction may be when the preheating temperature is reached, or when the temperature is lowered after reaching the preheating temperature and reaches a temperature lower than the preheating temperature.
  • the lower limit of the temperature in the width direction stretching step is more preferably Tm-9 ° C, further preferably Tm-7 ° C, and particularly preferably Tm-5 ° C.
  • the upper limit of the temperature in the width direction stretching step is preferably Tm + 10 ° C., more preferably Tm + 7 ° C., and particularly preferably Tm + 5 ° C.
  • the cooling temperature at this time is preferably not more than the temperature of stretching in the width direction and preferably Tm-80 ° C. or higher and Tm-15 ° C. or lower, and is preferably Tm-80 ° C. or higher and Tm-20 ° C. or lower. It is more preferable to set the temperature to Tm-80 ° C.
  • the temperature at the end of stretching in the width direction can be gradually lowered to the temperature at the time of cooling, but it can also be lowered stepwise or in one step. It is preferable to lower the temperature stepwise or stepwise because the crystal orientation in the film tends to be increased.
  • the lower limit of the final width direction stretching ratio in the width direction stretching step is preferably 10 times, more preferably 11 times. If it is 12 times or more, the rigidity is likely to be increased and the film thickness unevenness is likely to be reduced.
  • the upper limit of the stretching ratio in the width direction is preferably 20 times, more preferably 17 times, and further preferably 15 times. When it is 20 times or less, the heat shrinkage rate is likely to be reduced, and it is difficult to break during stretching.
  • the molecules of the polypropylene resin are highly oriented in the main orientation direction (the above-mentioned width).
  • the width direction is applicable.
  • the crystal orientation in the obtained biaxially oriented film is very strong, and crystals having a high melting point are easily generated.
  • the orientation of the amorphous part between the crystals also increases in the main orientation direction (the width direction corresponds to the width direction stretching step described above), and many crystals having a high melting point exist around the amorphous part.
  • the elongated polypropylene molecule in the amorphous part is difficult to relax and tends to maintain its tense state. Therefore, the entire biaxially oriented film can maintain high rigidity even at high temperatures.
  • the heat shrinkage rate at a high temperature of 150 ° C. is likely to be further reduced. The reason is that since there are more crystals with a high melting point around the amorphous part, the elongated polypropylene resin molecules in the amorphous part are difficult to relax at a temperature lower than the melting point of the crystals, and the molecules are less entangled with each other. It is in.
  • the crystallinity of the film is more likely to be increased, and the polypropylene resin molecular chains in the amorphous portion are less entangled with each other, resulting in less heat shrinkage stress.
  • the heat shrinkage rate can be further reduced. Conventionally, it can be said that it is epoch-making considering that if either the strength or the heat shrinkage rate is improved, the other property tends to be lowered.
  • the biaxially stretched film can be heat-treated to further reduce the heat shrinkage rate.
  • the upper limit of the heat treatment temperature is preferably Tm + 10 ° C, more preferably Tm + 7 ° C, and particularly preferably Tm + 5 ° C. By setting the temperature to Tm + 10 ° C. or lower, rigidity is likely to be developed, the roughness of the film surface does not become too large, and the film is less likely to whiten.
  • the lower limit of the heat treatment temperature is preferably Tm-5 ° C, more preferably Tm-2 ° C, and particularly preferably Tm ° C. If it is less than Tm-5 ° C, the heat shrinkage rate may increase.
  • the highly oriented crystals produced in the stretching step are difficult to melt, and the rigidity of the obtained film is reduced.
  • the heat shrinkage rate can be made smaller without lowering.
  • the film may be relaxed (relaxed) in the width direction during heat treatment for the purpose of adjusting the heat shrinkage rate, but the upper limit of the relaxation rate is preferably 4%. When it is within the above range, the film strength is unlikely to decrease, and the fluctuation in film thickness tends to be small. It is more preferably 3%, even more preferably 2%, even more preferably 1%, and particularly preferably 0%.
  • the thickness of the biaxially oriented polypropylene film of the present invention is set according to each application, but in order to obtain the strength of the film, the lower limit of the film thickness is preferably 2 ⁇ m, more preferably 3 ⁇ m, still more preferably. It is 4 ⁇ m, particularly preferably 8 ⁇ m, and most preferably 10 ⁇ m. When the film thickness is 2 ⁇ m or more, the rigidity of the film can be easily obtained.
  • the upper limit of the film thickness is preferably 100 ⁇ m, more preferably 80 ⁇ m, further preferably 60 ⁇ m, particularly preferably 50 ⁇ m, and most preferably 40 ⁇ m.
  • the biaxially oriented polypropylene film of the present invention is usually formed as a roll having a width of 2000 to 12000 mm and a length of about 1000 to 50000 m, and is wound into a film roll. Further, it is slit according to each application and is provided as a slit roll having a width of 300 to 2000 mm and a length of about 500 to 5000 m.
  • the biaxially oriented polypropylene film of the present invention can obtain a longer film roll.
  • the lower limit of the thickness uniformity of the biaxially oriented polypropylene film of the present invention is preferably 0%, more preferably 0.1%, still more preferably 0.5%, and particularly preferably 1%.
  • the upper limit of the thickness uniformity is preferably 20%, more preferably 17%, still more preferably 15%, particularly preferably 12%, and most preferably 10%. Within the above range, defects are less likely to occur during post-processing such as coating and printing, and it is easy to use for applications that require precision.
  • the measurement method was as follows. A test piece having a width of 40 mm is cut out from a steady region where the physical properties of the film are stable in the length direction of the film, and a film feeder manufactured by Micrometer Measuring Instruments Co., Ltd.
  • Thickness uniformity (%) [(maximum thickness-minimum thickness) / average thickness] x 100
  • the (110) strength ratio is preferably 120% or more, more preferably 123% or more, further preferably 125% or more, and particularly preferably 126% or more.
  • the width direction is applicable in the above-mentioned width direction stretching step
  • the main orientation direction is obtained. Secondary crystallization is likely to proceed along the line, and the degree of crystallinity increases. This is contributed by the large number of polypropylene molecules having a low molecular weight and high stereoregularity, which are easy to move and crystallize.
  • the biaxially stretched polypropylene film of the present invention has preferable characteristics of excellent rigidity and low heat shrinkage.
  • the lower limit of the degree of orientation calculated from Wh of the biaxially oriented polypropylene film of the present invention by the following formula is preferably 0.850, more preferably 0.855, and even more preferably 0.861. It is easy to increase the rigidity by setting it to 0.850 or more.
  • Orientation (180-Wh) / 180
  • the upper limit of the degree of orientation is preferably 0.928, more preferably 0.922, and even more preferably 0.917. When it is 0.928 or less, the film formation is easy to stabilize.
  • the biaxially oriented polypropylene film of the present invention is characterized by the following characteristics.
  • the "longitudinal direction" in the biaxially oriented polypropylene film of the present invention is a direction corresponding to the flow direction in the film manufacturing process
  • the "width direction” is a direction orthogonal to the flow direction in the film manufacturing process.
  • wide-angle X-rays are incident in the direction perpendicular to the film surface, and the scattering peaks derived from the (110) plane of the ⁇ -type crystal are scanned in the circumferential direction.
  • the direction in which the obtained diffraction intensity distribution has the largest diffraction intensity is referred to as the "longitudinal direction", and the direction orthogonal to it is referred to as the "width direction”.
  • the upper limit of the heat shrinkage in the longitudinal direction of the biaxially oriented polypropylene film of the present invention at 150 ° C. is preferably 10%, more preferably 7.0%, still more preferably 6.0%, and more. It is more preferably 5.0%, and particularly preferably 4.0% or less.
  • the upper limit of the heat shrinkage rate in the width direction at 150 ° C. is preferably 30%, more preferably 24%, further preferably 21%, and particularly preferably 18% or less.
  • the strain when the chuck portion is fused to the open portion is small, which is preferable.
  • the lower limit of the amount of components having a molecular weight of 100,000 or less when measuring the gel permeation chromatography (GPC) integration curve of the polypropylene resin constituting the film is set to 35% by mass. It is effective to adjust the stretching ratio, stretching temperature, and heat fixing temperature.
  • the biaxially oriented polypropylene film of the present invention uses polypropylene having high stereoregularity, and by adopting the above-mentioned stretching step in the width direction, the crystallinity and crystal distribution height in the film having a large contribution to rigidity are high.
  • relaxation due to melting of the crystal near the glass transition temperature of the polypropylene resin is less likely to occur, and relaxation of the amorphous portion is also suppressed due to the effect.
  • the melting of crystals with a high degree of orientation is completed, and the relaxation of the amorphous parts, which had been suppressed until then, also progresses, so that large relaxation occurs at high temperatures.
  • the biaxially oriented polypropylene film of the present invention has a small elastic modulus near the glass transition temperature, and conversely has a large elastic modulus at high temperatures (particularly at 100 ° C. or higher). Therefore, in the temperature dependence of the loss elastic modulus (E ′′) in the width direction obtained by the dynamic viscoelasticity measurement (DMA) of the biaxially oriented polypropylene film of the present invention, the loss elastic modulus (E ′′) at 100 ° C. or higher.
  • the ratio (E “ h / E" g ) of the maximum value (E " h ) to the maximum value (E” g ) of the loss elastic modulus (E ") between -25 ° C and 25 ° C is preferably 70.
  • Ratio (E " h / E” g ) Is 70% or more, the rigidity and heat resistance in the practical temperature range close to room temperature are more likely to be improved.
  • the polypropylene resin constituting the film is used. It is effective to set the lower limit of the amount of the component having a molecular weight of 100,000 or less when measuring the gel permeation chromatography (GPC) integration curve to 35% by mass, and adjust the draw ratio, the draw temperature, and the heat fixation temperature.
  • the lower limit of the tensile elongation at break in the longitudinal direction of the biaxially oriented polypropylene film of the present invention at 23 ° C. is preferably 195%, more preferably 200%, still more preferably 210%, and particularly preferably. It is 220% or more. If it is 195% or more, the breakage of the film and the breakage of the packaging bag are likely to decrease.
  • the upper limit of the tensile elongation at break in the longitudinal direction at 23 ° C. is preferably 300% as a realistic value, and more preferably 280%.
  • the lower limit of the tensile elongation at break in the width direction of the biaxially oriented polypropylene film of the present invention at 23 ° C. is preferably 25%, more preferably 30%, still more preferably 32%, and particularly preferably. It is 35%. If it is 25% or more, the breakage of the film and the breakage of the packaging bag are likely to occur.
  • the upper limit of the tensile elongation at break in the width direction at 23 ° C. is preferably 60%, more preferably 55%, and even more preferably 50%. If it is 60% or less, the printing pitch shift when transferring the printing ink is less likely to occur, and the durability of the packaging bag is likely to be excellent.
  • the tensile elongation at break can be within the range by adjusting the draw ratio, the draw temperature, and the heat fixation temperature.
  • the lower limit of the tensile breaking strength in the longitudinal direction of the biaxially oriented polypropylene film of the present invention at 23 ° C. is preferably 90 MPa, more preferably 100 MPa, still more preferably 110 MPa, and particularly preferably 120 MPa. If it is 90 MPa or more, the printing pitch shift when transferring the printing ink is less likely to occur, and the durability of the packaging bag is likely to be excellent.
  • the upper limit of the tensile breaking strength in the longitudinal direction at 23 ° C. is preferably 200 MPa, more preferably 180 MPa, and further preferably 160 MPa as a realistic value.
  • the lower limit of the tensile breaking strength in the width direction of the biaxially oriented polypropylene film of the present invention at 23 ° C. is preferably 380 MPa, more preferably 400 MPa, further preferably 430 MPa, and particularly preferably 450 MPa. If it is 380 MPa or more, the printing pitch shift when transferring the printing ink is less likely to occur, and the durability of the packaging bag is likely to be excellent.
  • the upper limit of the tensile breaking strength in the width direction at 23 ° C. is preferably 550 MPa, more preferably 520 MPa, and further preferably 500 MPa as a realistic value.
  • the breakage of the film and the breakage of the packaging bag are likely to decrease.
  • the lower limit of the amount of components having a molecular weight of 100,000 or less when the gel permeation chromatography (GPC) integration curve of the polypropylene resin constituting the film is measured is set to 35% by mass, and the draw ratio is set to 35% by mass. It is effective to adjust the stretching temperature and the heat fixing temperature.
  • the lower limit of the stress (F5) of the biaxially oriented polypropylene film of the present invention at 5% elongation in the longitudinal direction at 23 ° C. is preferably 40 MPa, more preferably 42 MPa, still more preferably 44 MPa, and further. It is preferably 46 MPa, particularly preferably 48 MPa. At 40 MPa or more, since the rigidity is high, it is easy to maintain the bag shape when it is used as a packaging bag, and the film is less likely to be deformed during processing such as printing.
  • the lower limit of F5 in the width direction of the biaxially oriented polypropylene film of the present invention at 23 ° C. is preferably 160 MPa, more preferably 170 MPa, still more preferably 180 MPa, and particularly preferably 190 MPa. At 160 MPa or more, since the rigidity is high, it is easy to maintain the bag shape when it is used as a packaging bag, and the film is less likely to be deformed during processing such as printing.
  • F5 can be set within the range by adjusting the stretching ratio and the relaxing rate, and adjusting the temperature at the time of film formation.
  • the upper limit of the heat shrinkage in the longitudinal direction of the biaxially oriented polypropylene film of the present invention at 120 ° C. is preferably 2.0%, more preferably 1.5%, and even more preferably 1.2%. , Particularly preferably 1.0%. When it is 2.0% or less, the printing pitch shift when transferring the printing ink is less likely to occur.
  • the upper limit of the heat shrinkage rate in the width direction at 120 ° C. is 5.0%, preferably 4.0%, more preferably 3.5%, and particularly preferably 2.5%. If it is 5.0% or less, wrinkles during heat sealing are unlikely to occur.
  • the balance between the heat shrinkage rate at 120 ° C. and the heat shrinkage rate in the longitudinal direction to the width direction can be within the range by adjusting the draw ratio, the draw temperature, and the heat fixation temperature.
  • the lower limit of the refractive index (Nx) in the longitudinal direction of the biaxially oriented polypropylene film of the present invention is preferably 1.4950, more preferably 1.4970, and even more preferably 1.4980. If it is 1.4950 or more, it is easy to increase the rigidity of the film.
  • the upper limit of the refractive index (Nx) in the longitudinal direction is preferably 1.5100, more preferably 1.5070, and even more preferably 1.5050. If it is 1.5100 or less, the balance of the characteristics in the longitudinal direction and the width direction of the film tends to be excellent.
  • the lower limit of the refractive index (Ny) in the width direction of the biaxially oriented polypropylene film of the present invention is 1.5230, preferably 1.5235, and more preferably 1.5240. If it is 1.5230 or more, it is easy to increase the rigidity of the film.
  • the upper limit of the refractive index (Ny) in the width direction is preferably 1.5280, more preferably 1.5275, and even more preferably 1.5270. If it is 1.5280 or less, the balance of the characteristics in the longitudinal direction and the width direction of the film tends to be excellent.
  • the lower limit of the refractive index (Nz) in the thickness direction of the biaxially oriented polypropylene film of the present invention is preferably 1.4960, more preferably 14965, and even more preferably 1.4970. If it is 1.4960 or more, it is easy to increase the rigidity of the film.
  • the upper limit of the refractive index (Nz) in the thickness direction is preferably 1.5020, more preferably 1.5015, and even more preferably 1.5010. If it is 1.5020 or less, the heat resistance of the film can be easily increased.
  • the refractive index can be set within the range by adjusting the stretching ratio, stretching temperature, and heat fixing temperature.
  • the lower limit of ⁇ Ny of the biaxially oriented polypropylene film of the present invention of the present invention is 0.0220, preferably 0.0225, more preferably 0.0228, and further preferably 0.0230. If it is 0.0220 or more, the rigidity of the film tends to increase.
  • the upper limit of ⁇ Ny is preferably 0.0270, more preferably 0.0265, still more preferably 0.0262, and particularly preferably 0.0260 as a realistic value. If it is 0.0270 or less, the thickness unevenness tends to be good.
  • ⁇ Ny can be set within the range by adjusting the stretching ratio, stretching temperature, and heat fixing temperature of the film.
  • ⁇ Ny is calculated by the following formula, where the refractive indexes along the longitudinal direction, the width direction, and the thickness direction of the film are Nx, Ny, and Nz, respectively. It means the degree of orientation in the direction.
  • ⁇ Ny Ny ⁇ [(Nx + Nz) / 2]
  • the lower limit of the plane orientation coefficient ( ⁇ P) of the biaxially oriented polypropylene film of the present invention is preferably 0.0135, more preferably 0.0138, and even more preferably 0.0140. When it is 0.0135 or more, the balance in the surface direction of the film is good, and the thickness unevenness is also good.
  • the upper limit of the plane orientation coefficient ( ⁇ P) is preferably 0.0155, more preferably 0.0152, and even more preferably 0.0150 as a realistic value. If it is 0.0155 or less, the heat resistance at high temperature is likely to be excellent.
  • the plane orientation coefficient ( ⁇ P) can be set within the range by adjusting the stretching ratio, stretching temperature, and heat fixing temperature. The plane orientation coefficient ( ⁇ P) was calculated using (Equation) [(Nx + Ny) / 2] -Nz.
  • the oriented crystal in the width direction of the film.
  • the upper limit of the half-value width (Wh) of the diffraction peak derived from is 27 °, preferably 26 °, more preferably 25 °, particularly preferably 24 °, and most preferably 23 °.
  • Wh half-value width
  • the lower limit of Wh is preferably 13 °, more preferably 14 °, and even more preferably 15 °.
  • the upper limit of the haze of the biaxially oriented polypropylene film of the present invention is preferably 5.0%, more preferably 4.5%, further preferably 4.0%, and particularly preferably 3.5%. Yes, most preferably 3.0%. If it is 5.0% or less, it is easy to use in applications where transparency is required.
  • the lower limit of the haze is preferably 0.1%, more preferably 0.2%, still more preferably 0.3%, and particularly preferably 0.4% as a realistic value. If it is 0.1% or more, it is easy to manufacture.
  • the haze adjusts the cooling roll (CR) temperature, the stretching temperature in the width direction, the preheating temperature before stretching in the tenter width direction, the stretching temperature in the width direction, or the heat fixing temperature, or the amount of components having a molecular weight of 100,000 or less of the polypropylene resin.
  • it may increase due to the addition of an antiblocking agent or the addition of a seal layer.
  • the pre-made bag is filled with the contents and heated to melt the film, fuse it and seal it.
  • a sealant film made of polyethylene, polypropylene, or the like is laminated on the base film, and the sealant film surfaces are fused to each other.
  • pressure is applied from the base film side with a heating plate to press the film to seal it, but the sealing width is often about 10 mm.
  • the base film is also heated, and the shrinkage at that time causes wrinkles. It is better to have less wrinkles in the durability of the bag, and it is better to have less wrinkles in order to increase purchasing motivation.
  • the sealing temperature may be about 120 ° C., but in order to increase the bag making processing speed, a higher sealing temperature is required, and even in that case, it is preferable that the shrinkage is small.
  • the chuck is fused to the opening portion of the bag, it is required to seal at a higher temperature.
  • Print pitch shift As a basic structure of the packaging film, it is often composed of a laminated film of a printed base film and a sealant film.
  • a bag making machine is used to manufacture bags, and there are three-sided bags, standing bags, gusset bags, etc., and various bag making machines are used. It is considered that the printing pitch shift occurs because the base material of the film expands and contracts because tension and heat are applied to the film during the printing process. Eliminating defective products due to printing pitch deviation is important in terms of effective use of resources, and is also important in increasing purchasing motivation.
  • the biaxially oriented polypropylene film of the present invention can be printed by letterpress printing, lithographic printing, intaglio printing, stencil printing, and transfer printing, depending on the application.
  • low-density polyethylene, linear low-density polyethylene, ethylene-vinyl acetate copolymer, polypropylene, unstretched sheet made of polyester, uniaxially stretched film, and biaxially stretched fill are bonded as a sealant film to impart heat sealability. It can also be used as a laminated body.
  • aluminum foil polyvinylidene chloride, nylon, ethylene-vinyl alcohol copolymer, unstretched sheet made of polyvinyl alcohol, uniaxially stretched film, and biaxially stretched film as biaxially oriented polypropylene film. It can be provided as an intermediate layer between the and the sealant film.
  • An adhesive applied by a dry lamination method or a hot melt lamination method can be used for laminating the sealant film.
  • aluminum or an inorganic oxide can be vapor-deposited on a biaxially oriented polypropylene film, an intermediate layer film, or a sealant film. Vacuum vapor deposition, sputtering, and ion plating methods can be adopted as the vapor deposition method, but silica, allumina, or a mixture thereof is particularly preferable.
  • the biaxially oriented polypropylene film of the present invention contains, for example, antifogging agents such as fatty acid esters of polyhydric alcohols, amines of higher fatty acids, amides of higher fatty acids, amines of higher fatty acids and ethylene oxide adducts of amide.
  • antifogging agents such as fatty acid esters of polyhydric alcohols, amines of higher fatty acids, amides of higher fatty acids, amines of higher fatty acids and ethylene oxide adducts of amide.
  • additives for improving quality such as slipperiness and antistatic property
  • lubricants such as wax and metal soap for improving productivity
  • plasticizers for example, plasticizers.
  • agents, processing aids, heat stabilizers, antioxidants, antistatic agents, ultraviolet absorbers and the like are also possible.
  • the biaxially oriented polypropylene film of the present invention has excellent properties as described above, it can be preferably used for packaging bags, and the thickness of the film can be made thinner than before.
  • insulating films for capacitors and motors such as insulating films for capacitors and motors, back sheets for solar cells, barrier films for inorganic oxides, and base films for transparent conductive films such as ITO, and to have rigidity such as separate films. It is also suitable for various applications.
  • melt flow rate The melt flow rate (MFR) was measured at a temperature of 230 ° C. and a load of 2.16 kgf in accordance with JIS K7210.
  • the mesopentad fraction ([mmmm]%) of the polypropylene resin was measured using 13C-NMR.
  • the mesopentad fraction was calculated according to the method described in Zambelli et al., Macromolecules, Vol. 6, p. 925 (1973).
  • the 13C-NMR measurement was carried out at 110 ° C. by dissolving 200 mg of a sample in an 8: 2 mixture of o-dichlorobenzene and heavy benzene using AVANCE500 manufactured by Bruker.
  • the number average molecular weight (Mn) and the mass average molecular weight (Mw) are each defined by the following equations by the number of molecules (Ni) of the molecular weight (Mi) at each elution position of the GPC curve obtained via the molecular weight calibration curve.
  • Number average molecular weight: Mn ⁇ (Ni ⁇ Mi) / ⁇ Ni
  • Mass average molecular weight: Mw ⁇ (Ni ⁇ Mi 2 ) / ⁇ (Ni ⁇ Mi)
  • the molecular weight distribution can be obtained by Mw / Mn.
  • the ratio of the components having a molecular weight of 100,000 or less was obtained from the integral curve of the molecular weight distribution obtained by GPC.
  • Crystallization temperature (Tc), melting temperature (Tm) Heat measurement was performed in a nitrogen atmosphere using a Q1000 differential scanning calorimeter manufactured by TA Instruments. Approximately 5 mg was cut out from polypropylene resin pellets and sealed in an aluminum pan for measurement. The temperature was raised to 230 ° C. and held for 5 minutes, then cooled to 30 ° C. at a rate of ⁇ 10 ° C./min, and the exothermic peak temperature was defined as the crystallization temperature (Tc). The amount of heat of crystallization ( ⁇ Hc) was determined by setting a baseline so that the area of the exothermic peak could be smoothly connected from the start of the peak to the end of the peak. The temperature was kept as it was at 30 ° C. for 5 minutes, the temperature was raised to 230 ° C. at 10 ° C./min, and the main endothermic peak temperature was defined as the melting temperature (Tm).
  • Tensile test The tensile strength of the film in the longitudinal direction and the width direction was measured at 23 ° C. according to JIS K 7127. The sample was cut out from a film to a size of 15 mm ⁇ 200 mm, had a chuck width of 100 mm, and was set in a tensile tester (dual column desktop tester Instron 5965 manufactured by Instron Japan Company Limited). A tensile test was performed at a tensile speed of 200 mm / min. From the obtained strain-stress curve, the stress at 5% elongation was defined as F5. The tensile breaking strength and the tensile breaking elongation were taken as the strength and elongation at the time when the sample broke, respectively.
  • F5 at 80 ° C. was determined by performing the measurement in a constant temperature bath at 80 ° C. The measurement was carried out by setting the chuck in a constant temperature bath set to 80 ° C. in advance, mounting the sample until the measurement was performed, and then holding the sample for 1 minute.
  • Heat shrinkage rate Measured by the following method in accordance with JIS Z 1712. The film was cut with a width of 20 mm and a length of 200 mm in the longitudinal direction and the width direction of the film, respectively, and hung in a hot air oven at 120 ° C. or 150 ° C. and heated for 5 minutes. The length after heating was measured, and the heat shrinkage rate was determined by the ratio of the contracted length to the original length.
  • Refractive index, ⁇ Ny, plane orientation coefficient Measured at a wavelength of 589.3 nm and a temperature of 23 ° C. using an Abbe refractometer manufactured by Atago Co., Ltd.
  • the refractive indexes along the longitudinal direction and the width direction of the film were Nx and Ny, respectively, and the refractive indexes in the thickness direction were Nz.
  • ⁇ Ny was determined using (formula) Ny ⁇ [(Nx + Nz) / 2] using Nx, Ny, and Nz.
  • the plane orientation coefficient ( ⁇ P) was calculated using (Equation) [(Nx + Ny) / 2] -Nz.
  • the wide-angle X-ray (WAXS) measurement of the film is owned by the Frontier Soft Matter Development Industry-Academia Union (FSBL) in the large radiation facility SPring-8. It was done at the second hatch of the beam line BL03XU.
  • the X-ray wavelength was 0.1 nm
  • a two-dimensional detector SOPHIAS was used as a detector, and the transmittance was calculated from the values of the ion chambers set before and after the sample.
  • the film is sandwiched between two non-slip SUS plates with a hole with a diameter of 4 mm in the center, placed in a self-made holder, restrained in all directions, and blown with temperature-controlled air from 40 ° C to 180 ° C. While raising the temperature at a rate of 10 ° C./min, X-rays were incident on the film surface in the direction perpendicular to the film surface to obtain wide-angle X-ray diffraction images at each temperature. Air scattering correction was performed on the obtained two-dimensional image in consideration of the transmittance.
  • Cerium oxide (CeO 2 ) was used to measure the camera length, and Fit2D (software made by European Synchrotron Radiation Facility [http://www.esrf.eu/computing/scientific/FIT2D/]) was used to measure polypropylene ⁇ .
  • the azimuth profile of the (110) plane of the type crystal was calculated.
  • the maximum value of the maximum intensity in the range of 40 ° C. to 130 ° C. the maximum intensity at 40 ° C.
  • the ratio (diffraction intensity ratio) to the ratio (diffraction intensity ratio) (%) was calculated.
  • DMA Dynamic Viscoelasticity Measurement
  • PP-1 Suditomo Chemical Co., Ltd.
  • Table 1 shows the structure of the polypropylene resin
  • Table 2 shows the film forming conditions
  • Table 3 shows the physical properties. As shown in Table 3, its physical properties were inferior in rigidity and heat shrinkage at 150 ° C.
  • the film was heated with a tenter at a preheating temperature of 173 ° C., and subsequently stretched 8.2 times in the width direction at a stretching temperature of 165 ° C., and then. , Heat fixation was performed at 171 ° C. with 6.6% relaxation.
  • the thickness of the obtained film was 20.9 ⁇ m.
  • Table 1 shows the structure of the polypropylene resin
  • Table 2 shows the film forming conditions
  • Table 3 shows the physical properties. As shown in Table 3, its physical properties were inferior in rigidity.

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Abstract

La présente invention concerne un film de polypropylène à orientation biaxiale qui présente une rigidité élevée et une excellente résistance à la chaleur même à une température aussi élevée que 150 °C, et qui maintient facilement la forme du sac lorsqu'il est formé dans un sac d'emballage, tout en subissant un faible décalage de pas pendant l'impression et ayant peu de plis dans une partie d'étanchéité lorsqu'il est scellé à la chaleur.　Un film de polypropylène à orientation biaxiale satisfait les exigences (1) à (3) décrites ci-dessous. (1) Par rapport à la dépendance à la température de l'intensité maximale du profil azimutal telle qu'obtenue par balayage, dans la direction circonférentielle, de la diffusion associée au plan (110) d'un cristal de forme α du polypropylène dans une mesure de diffraction des rayons X à grand angle qui est réalisée en restreignant le film dans quatre directions et en irradiant le film avec un rayon X dans une direction qui est perpendiculaire à la surface du film, tout en chauffant le film de 40 °C à 180 °C à une vitesse de 10 °C/minute, le ratio de la valeur maximale de l'intensité maximale dans la plage de 40 °C à 130 °C par rapport à l'intensité maximale à 40 °C (à savoir, le ratio d'intensité (110)) est de 115 % ou plus. (2) Le degré d'orientation dans la direction de la largeur est de 0,85 ou plus. (3) Le rapport de retrait thermique à 150 °C est inférieur ou égal à 10 % dans la direction longitudinale, tout en étant de 30 % ou moins dans la direction de la largeur.
PCT/JP2021/011662 2020-03-24 2021-03-22 Film de polypropylène à orientation biaxiale WO2021193510A1 (fr)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013111779A1 (fr) * 2012-01-24 2013-08-01 東洋紡株式会社 Film de polypropylène étiré
WO2017221781A1 (fr) * 2016-06-23 2017-12-28 東洋紡株式会社 Film de polypropylène stratifié

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013111779A1 (fr) * 2012-01-24 2013-08-01 東洋紡株式会社 Film de polypropylène étiré
WO2017221781A1 (fr) * 2016-06-23 2017-12-28 東洋紡株式会社 Film de polypropylène stratifié

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