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
  • B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
• • 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
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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  • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
  • B29C48/001—Combinations of extrusion moulding with other shaping operations
  • B29C48/0018—Combinations of extrusion moulding with other shaping operations combined with shaping by orienting, stretching or shrinking, e.g. film blowing
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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  • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
  • B29C48/001—Combinations of extrusion moulding with other shaping operations
  • B29C48/0021—Combinations of extrusion moulding with other shaping operations combined with joining, lining or laminating
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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  • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
  • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
  • B29C48/07—Flat, e.g. panels
  • B29C48/08—Flat, e.g. panels flexible, e.g. films
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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  • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
  • B29C48/25—Component parts, details or accessories; Auxiliary operations
  • B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
  • B29C48/911—Cooling
  • B29C48/9135—Cooling of flat articles, e.g. using specially adapted supporting means
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
  • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B27/00—Layered products comprising a layer of synthetic resin
  • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • 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
  • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
  • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
  • B32B7/04—Interconnection of layers
  • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • 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
• • 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
  • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
  • C08J7/04—Coating
  • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
  • C09J7/00—Adhesives in the form of films or foils
  • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
  • C09J7/22—Plastics; Metallised plastics
  • C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
• • G—PHYSICS
  • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
  • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
  • G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
  • G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
• • G—PHYSICS
  • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
  • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
  • G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
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  • G09F9/301—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements flexible foldable or roll-able electronic displays, e.g. thin LCD, OLED
• • G—PHYSICS
  • G09—EDUCATION; CRYPTOGRAPHY; DISPLAY; ADVERTISING; SEALS
  • G09F—DISPLAYING; ADVERTISING; SIGNS; LABELS OR NAME-PLATES; SEALS
  • G09F9/00—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements
  • G09F9/30—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
  • G09F9/33—Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements being semiconductor devices, e.g. diodes
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B29K2077/00—Use of PA, i.e. polyamides, e.g. polyesteramides or derivatives thereof, as moulding material
  • B29K2077/10—Aromatic polyamides [polyaramides] or derivatives thereof
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B29K2509/00—Use of inorganic materials not provided for in groups B29K2503/00 - B29K2507/00, as filler
  • B29K2509/02—Ceramics
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
  • B29K2995/0012—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular thermal properties
• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
  • B29K2995/0018—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular optical properties, e.g. fluorescent or phosphorescent
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
  • B29L2031/00—Other particular articles
  • B29L2031/34—Electrical apparatus, e.g. sparking plugs or parts thereof
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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  • B32B2255/00—Coating on the layer surface
  • B32B2255/10—Coating on the layer surface on synthetic resin layer or on natural or synthetic rubber layer
• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • B—PERFORMING OPERATIONS; TRANSPORTING
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• • C—CHEMISTRY; METALLURGY
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Definitions

• thermoplastic resin film produced by controlling conditions such as the draw ratio and temperature during film production can solve the above problems.
• the present invention has been completed. That is, the gist of the present invention is as follows.
• thermoplastic resin film of the present invention having a haze of 13% or less is The film is characterized by having a loop stiffness value of 140 mN/cm or more in at least one direction of the film plane measured by a loop stiffness tester.
• the thermoplastic resin film of the present invention preferably has a thickness of 40 ⁇ m or more.
• the thermoplastic resin constituting the thermoplastic resin film has a glass transition temperature of 60° C. or higher.
• the crystallinity of the surface layer is preferably 0.1 or more.
• the thermoplastic resin is preferably semi-aromatic polyamide.
• thermoplastic resin film of the present invention has sufficient transparency as an optical film and sufficient flexural rigidity as a support substrate. , electronic substrate materials such as flexible flat cables, cover lay films for flexible printed wiring, and the like.
• thermoplastic resin film of the present invention is a thermoplastic resin film having a haze of 13% or less, and a loop stiffness value of 140 mN/cm or more in at least one direction of the film plane measured by a loop stiffness tester. It is a thermoplastic resin film characterized by being
• the semi-aromatic polyamide may contain, as a dicarboxylic acid component, a dicarboxylic acid component other than the aromatic dicarboxylic acid component within a range that does not impair the effects of the present invention.
• dicarboxylic acids include, for example, aliphatic dicarboxylic acids such as oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, sebacic acid, dodecanedioic acid, tetradecanedioic acid, octadecanedioic acid.
• the aliphatic diamine component preferably contains an aliphatic diamine having 6 to 12 carbon atoms as a main component, more preferably an aliphatic diamine having 9 to 12 carbon atoms as a main component, and preferably contains 9 or 10 carbon atoms. of aliphatic diamine as a main component.
• the content of the aliphatic diamine having 6 to 12 carbon atoms in the aliphatic diamine component is preferably 60 mol% or more, more preferably 75 mol% or more, and even more preferably 90 mol% or more. .
• the obtained film can achieve both heat resistance and productivity.
• the aliphatic diamines having 6 to 12 carbon atoms may be used alone or in combination of two or more. In addition, when using 2 or more types together, let content be the sum total of them.
• Aliphatic diamines having 6 to 12 carbon atoms include 1,6-hexanediamine, 1,7-heptanediamine, 1,8-octanediamine, 1,9-nonanediamine, 1,10-decanediamine, 1,11 - undecanediamine, linear aliphatic diamines of 1,12-dodecanediamine, 2-methyl-1,8-octanediamine, 4-methyl-1,8-octanediamine, 5-methyl-1,9-nonanediamine, 2,2,4-/2,4,4-trimethyl-1,6-hexanediamine, 2-methyl-1,5-pentanediamine, 2-methyl-1,6-hexanediamine, 2-methyl-1, Branched chain aliphatic diamines such as 7-heptanediamine are included.
• the semi-aromatic polyamide may contain, as a diamine component, a diamine component other than the aliphatic diamine component within a range that does not impair the effects of the present invention.
• diamine components include, for example, alicyclic diamines such as isophoronediamine, norbornanedimethylamine, and tricyclodecanedimethylamine, and aromatic diamines such as metaxylylenediamine, paraxylylenediamine, metaphenylenediamine, and paraphenylenediamine. is mentioned.
• the semi-aromatic polyamide may be copolymerized with lactams such as ⁇ -caprolactam, ⁇ -enantholactam, ⁇ -capryllactam, and ⁇ -laurolactam to the extent that the effects of the present invention are not impaired.
• lactams such as ⁇ -caprolactam, ⁇ -enantholactam, ⁇ -capryllactam, and ⁇ -laurolactam
• the type and copolymerization ratio of the monomers constituting the semi-aromatic polyamide are preferably selected so that the resulting semi-aromatic polyamide has a melting point (Tm) in the range of 270-350°C.
• Tm melting point
• the semi-aromatic polyamide has a Tm within the above range, thermal decomposition during processing into a film can be efficiently suppressed. If the Tm is less than 270°C, the resulting film may have insufficient heat resistance. On the other hand, if Tm exceeds 350°C, thermal decomposition may occur during film production.
• the limiting viscosity of the semi-aromatic polyamide is preferably 0.8 to 2.0 dL/g, more preferably 0.9 to 1.8 dL/g.
• the semi-aromatic polyamide has an intrinsic viscosity of 0.8 dL / g or more, it is possible to produce a film with excellent mechanical strength, but when it exceeds 2.0 dL / g, it is difficult to produce a film. can be
• thermoplastic resin film of the present invention must have a haze of 13% or less, preferably 10% or less, more preferably 5% or less, as measured according to JIS K7105. preferable. If the haze of the thermoplastic resin film exceeds 13%, the visibility is poor. Since the thermoplastic resin film has a haze of 13% or less, it has excellent visibility. For example, when used as a substrate in a bottom emission display, a light source such as an LED element can be sufficiently extracted through the substrate. can. Furthermore, even if the number of pixels increases due to the increase in display size, the increase in definition, and the aperture ratio decreases, it can be used as a substrate material while maintaining a practical light extraction efficiency. On the other hand, if it is a top emission system, it is possible to raise light extraction efficiency more.
• the thermoplastic resin film of the present invention preferably has a thickness of 40 ⁇ m or more, more preferably 45 ⁇ m or more, even more preferably 70 ⁇ m or more, and particularly preferably 75 ⁇ m or more.
• the thermoplastic resin film having a thickness of 40 ⁇ m or more can prevent the entire laminate from bending when the LED element is mounted. Such suppression of bending of the laminate not only ensures the flatness of the substrate material, but also makes it possible to make the light extraction efficiency uniform when a display is constructed. It can be made without spots in brightness.
• the thickness of the thermoplastic resin film is preferably 200 ⁇ m or less, more preferably 160 ⁇ m or less, and even more preferably 90 ⁇ m or less. Since the thermoplastic resin film has a thickness of 200 ⁇ m or less, it is easy to handle in roll-to-roll processing, and when applied to an image display device, it suppresses an increase in the thickness of the entire image display device. can be done.
• thermoplastic resin constituting the thermoplastic resin film of the present invention preferably has a glass transition temperature of 60°C or higher, more preferably 100°C or higher. Since the thermoplastic resin film has a glass transition temperature of 60° C. or higher, it can withstand the processing temperature when manufacturing the LED mounting substrate, and furthermore, it can prevent thermal expansion and deformation due to heat generation of the LED light source. can be done. Furthermore, when a display is configured, it is possible to ensure long-term durability and improve the reliability of quality maintenance, and in connection with the suppression of deflection, uniform light extraction efficiency, and a large display , the screen can be even in brightness.
• the surface layer of the thermoplastic resin film of the present invention preferably has a degree of crystallinity obtained by infrared spectroscopy of 0.1 or more, more preferably 0.15 or more, and 0.2 or more. is more preferred.
• the degree of crystallinity of the surface layer is less than 0.1, the thermoplastic resin film has low flexural rigidity, and an LED mounting substrate using the film may lack beauty.
• the degree of crystallinity of the surface layer of the thermoplastic resin film is preferably 0.4 or less, more preferably 0.3 or less, and even more preferably 0.25 or less. If the crystallinity of the surface layer exceeds 0.4, the thermoplastic resin film may have a high haze and poor visibility.
• the thermoplastic resin film of the present invention preferably has a coefficient of dynamic friction measured according to JIS K7125 of 0.8 or less, more preferably 0.7 or less, and even more preferably 0.5 or less. .
• a coefficient of dynamic friction measured according to JIS K7125 of 0.8 or less, more preferably 0.7 or less, and even more preferably 0.5 or less.
• the thermoplastic resin film of the present invention has a heat shrinkage rate SMD in the longitudinal direction of the film and a heat shrinkage rate S TD in the width direction measured under conditions of 250° C. for 5 minutes, respectively, of ⁇ 1.0 to 1.0. It is preferably 5%, more preferably -0.8 to 1.3%, even more preferably -0.6 to 1.0%. Since the thermoplastic resin film has a heat shrinkage rate of 1.5% or less, the dimensional stability is improved and the heat resistance is excellent. On the other hand, if the thermoplastic resin film has a heat shrinkage rate of more than 1.5%, processing troubles may occur due to a large dimensional change when the film is processed at a high temperature.
• the thermoplastic resin film of the present invention preferably has a longitudinal tensile strength of 110 MPa or more, more preferably 130 MPa or more, and even more preferably 140 MPa or more, measured according to JIS K7127. Also, the tensile strength in the width direction is preferably 200 MPa or more, more preferably 220 MPa or more, and even more preferably 230 MPa or more. When the thermoplastic resin film has a tensile strength within the above range, it is less likely to break during molding and processing.
• thermoplastic resin film of the present invention In order to further improve the properties of the thermoplastic resin film of the present invention, if necessary, a lubricant, a pigment such as titanium, a coloring agent such as a dye, and the like, as long as the properties of the film are not sacrificed.
• Anti-coloring agents, heat stabilizers, hindered phenols, antioxidants such as phosphates and phosphites, weather resistance improvers such as benzotriazole compounds, brominated and phosphorus-based flame retardants, plasticizers, Additives such as mold agents, reinforcing agents such as talc, modifiers, antistatic agents, ultraviolet absorbers, antifogging agents, and various polymer resins may be contained.
• organic particles include acrylic resin particles, melamine resin particles, silicone resin particles, and crosslinked polystyrene particles. Among them, silica particles and acrylic resin particles are preferred from the viewpoint of good dispersibility in the substrate film and good handling.
• the thermoplastic resin film of the present invention preferably contains fine particles as a lubricant.
• the content of fine particles in the thermoplastic resin film is preferably 0.01 to 0.4% by mass, more preferably 0.05 to 0.3% by mass, and more preferably 0.1 to 0.3% by mass. % is more preferred.
• the fine particles preferably have a large average particle size, preferably 0.010 ⁇ m or more, more preferably 0.5 ⁇ m or more, and 1.0 ⁇ m or more. More preferred.
• the average particle size is preferably small, preferably 5.0 ⁇ m or less, more preferably 4.0 ⁇ m or less, and 3.0 ⁇ m or less. is more preferred. If the average particle size of the fine particles is small, the voids generated between the fine particles and the resin constituting the film will be small, so that the thermoplastic resin film will have excellent transparency and bending rigidity. In addition, the smaller the particle size, the less the fine particles slide down, which is preferable.
• two or more kinds of fine particles having different average particle sizes may be used in combination, and by using them together, it is possible to adjust the balance of slipperiness, transparency, and bending rigidity.
• thermoplastic resin film Various methods can be used as a method for incorporating the additive into the thermoplastic resin film. Typical methods include the following methods.
• A) Method of adding during polymerization of thermoplastic resin (B) Masterbatch method of adding directly to thermoplastic resin and preparing melt-kneaded pellets (C) Directly adding to thermoplastic resin during film formation, extruder Method of melt-kneading (D) Method of adding directly to the extruder at the time of film formation and melt-kneading
• thermoplastic resin film of the present invention can be produced, for example, by a method of increasing the degree of crystallinity of the film by controlling production conditions such as the magnification during film stretching and subsequent temperature.
• thermoplastic resin A commercially available product can be suitably used as a thermoplastic resin for producing a thermoplastic resin film.
• examples of such commercially available products include semi-aromatic polyamide resins such as "Genestar (registered trademark)” manufactured by Kuraray Co., Ltd., "Zecot (registered trademark)” manufactured by Unitika Ltd., and "Reny (registered trademark)” manufactured by Mitsubishi Engineering Plastics.
• polyamide 6 resins include “Novamid 1022 (registered trademark)” manufactured by Mitsubishi Plastics and Unitika “A1030BRF (registered trademark)” manufactured by K.K.
• Method C and D method are preferable, and D method is more preferable.
• Method C and D can produce a crushed mixture of salt and low polymer and salt at a lower temperature, and a crushed mixture of salt and low polymer and a large amount of salt when producing salt. does not require water. Therefore, generation of a gel-like substance can be reduced, and fish eyes can be reduced.
• the resulting semi-aromatic polyamide may be colored.
• the solid phase polymerization of the low polymer is preferably carried out under reduced pressure or under inert gas flow.
• the temperature of the solid phase polymerization is preferably 200 to 280°C. By setting the temperature of the solid-phase polymerization within this range, it is possible to suppress coloring and gelation of the obtained semi-aromatic polyamide.
• melt polymerization of the oligomer is preferably carried out at a temperature of 350°C or less. If the polymerization temperature exceeds 350°C, decomposition and thermal deterioration of the semi-aromatic polyamide may be accelerated. Therefore, films obtained from such semi-aromatic polyamides may be inferior in strength and appearance.
• melt polymerization using a melt extruder is also included in the above melt polymerization.
• a liquid mixture is obtained by stirring and mixing a suspension consisting of a molten aliphatic diamine and a solid aromatic dicarboxylic acid. Then, in this mixed solution, at a temperature below the melting point of the finally produced semi-aromatic polyamide, a reaction of the aromatic dicarboxylic acid and the aliphatic diamine to form a salt, and polymerization of the produced salt to produce a low polymer.
• a production reaction is performed to obtain a mixture of the salt and the low polymer.
• the crushing may be performed while reacting, or the crushing may be performed after taking out once after the reaction.
• the resulting reaction product is solid-phase polymerized at a temperature below the melting point of the final semi-aromatic polyamide to be polymerized to a predetermined molecular weight to obtain a semi-aromatic polyamide.
• Solid state polymerization is preferably carried out at a polymerization temperature of 180 to 270° C. for a reaction time of 0.5 to 10 hours in an inert gas stream such as nitrogen.
• the aromatic dicarboxylic acid powder is heated in advance to a temperature above the melting point of the aliphatic diamine and below the melting point of the aromatic dicarboxylic acid, and the aromatic dicarboxylic acid powder at this temperature is added to the aromatic dicarboxylic acid.
• the salt is made by adding the aliphatic diamine substantially free of water so that it remains powdery.
• the obtained salt is subjected to solid-phase polymerization at a temperature below the melting point of the semi-aromatic polyamide to be finally produced to increase the molecular weight to a predetermined molecular weight, thereby obtaining the semi-aromatic polyamide.
• Solid state polymerization is preferably carried out at a polymerization temperature of 180 to 270° C. for a reaction time of 0.5 to 10 hours in an inert gas stream such as nitrogen.
• the raw material for the semi-aromatic polyamide film may be a mixture of the above-mentioned virgin raw materials, a non-standard film generated during the production of the semi-aromatic polyamide film, a scrap mixture generated as edge trim, or the like. It may be prepared by adding virgin raw materials to a scrap mixture. These can be mixed by a known method such as a method of dry blending using a known device, or a kneading method of melt-kneading and mixing using a single-screw or twin-screw extruder.
• the unstretched thermoplastic resin film used in the biaxial stretching step is obtained by melt mixing the thermoplastic resin in an extruder at a temperature of 280 to 340 ° C. for 3 to 15 minutes. After that, it can be produced by extruding into a sheet through a T-die, contacting the sheet on a cooling roll whose temperature is adjusted to 30 to 40° C., and cooling it.
• the unstretched film is biaxially stretched, and the thermoplastic resin is oriented and crystallized by stretching.
• the stretching method is not particularly limited, but a flat sequential biaxial stretching method, a flat simultaneous biaxial stretching method, a tubular method, or the like can be used. Among them, the flat sequential biaxial stretching method and the flat simultaneous biaxial stretching method are most suitable since a film with good thickness accuracy can be obtained.
• Stretching devices for adopting the flat simultaneous biaxial stretching method include, for example, a screw type tenter, a pantograph type tenter, and a linear motor driven clip type tenter.
• the draw ratio is preferably 2.0 to 3.5 times in the longitudinal direction and 2.0 to 4.0 times in the width direction. It is more preferably 0 to 3.5 times. If the stretching ratio in the longitudinal direction exceeds 3.5 times, the resulting stretched film may be excessively crystallized, resulting in reduced stretchability in the width direction. Even when the film can be stretched in the width direction, the resulting stretched film is likely to be stretched unevenly, resulting in a decrease in thickness accuracy, a decrease in tensile strength in the longitudinal direction, and a decrease in transparency. On the other hand, if the stretch ratio in the width direction exceeds 4.0 times, the transparency may decrease, the heat shrinkage rate may increase, the dimensional stability may decrease, and the tensile strength may decrease.
• the resulting stretched film has a reduced loop stiffness value and tensile strength, and is likely to be stretched unevenly, resulting in unevenness in thickness and flatness. It may reduce sexuality.
• the stretching speed preferably exceeds 400%/min in both the longitudinal direction and the transverse direction, more preferably 800 to 12000%/min, and further preferably 1200 to 6000%/min. preferable. If the strain rate is 400%/min or less, crystals may grow during stretching and the film may be broken. , may break.
• the stretching temperature is preferably equal to or higher than the glass transition temperature (Tg) of the thermoplastic resin, more preferably higher than Tg and equal to or lower than (Tg+50°C). If the stretching temperature is lower than Tg, the film is likely to break and stable production cannot be performed.
• the heat setting temperature is preferably 260 to 280°C, more preferably 263 to 278°C, even more preferably 265 to 275°C. If the heat setting treatment temperature is lower than 260°C, the obtained film will have a high heat shrinkage rate.
• the resulting film has a reduced tensile strength, is likely to have poor appearance due to wrinkles caused by heat loss, and may break during the heat setting treatment, resulting in a poor biaxially stretched film. becomes difficult.
• Examples of the heat setting method include known methods such as a method of blowing hot air, a method of irradiating with infrared rays, and a method of irradiating with microwaves.
• the method of blowing hot air is preferable because it can be heated uniformly and accurately.
• the film may be subjected to relaxation treatment at the same temperature as the heat setting treatment temperature while being held by the clip.
• the relaxation rate is preferably 10.0% or less in the longitudinal direction and preferably 1.0 to 12.0% in the width direction. If the relaxation rate in the longitudinal direction exceeds 10.0%, the film may sag.
• thermoplastic resin film of the present invention As one method for suitably producing the thermoplastic resin film of the present invention, the film after heat setting treatment, or when heat relaxation treatment is performed, the film after heat relaxation treatment is attached to a clip.
• a method of cooling treatment at a temperature lower than the temperature in the heat setting treatment or heat relaxation treatment while being held is exemplified.
• the cooling treatment it is possible to prevent the rapid temperature drop (quenching) from the high temperature in the heat setting treatment or heat relaxation treatment to room temperature, and increase the crystallinity of the resulting thermoplastic resin film, which can be easily bent. Rigidity can be increased. That is, the method for producing a thermoplastic resin film of the present invention needs to include a step of performing a cooling treatment after biaxially stretching an unstretched thermoplastic resin film.
• the cooling treatment temperature is preferably 110° C. or higher, more preferably 120° C. or higher.
• the cooling treatment temperature is preferably 150° C. or lower, more preferably 140° C. or lower.
• the holding time is preferably 0.5 to 25 seconds, more preferably 1 to 20 seconds, even more preferably 2 to 15 seconds.
• the surface of the cylinder, the melting part of the barrel, the weighing part, the single tube, the filter, the T-die, etc. is prevented from stagnation. It is preferable that a treatment for reducing roughness is applied.
• a treatment for reducing roughness for example, a method of modifying with a substance having low polarity can be mentioned.
• the obtained thermoplastic resin film may be in the form of a sheet, or may be in the form of a film roll by being wound up on a take-up roll. From the viewpoint of productivity when used for various purposes, it is preferable to use the form of a film roll. When made into a film roll, it may be slit to a desired width.
• the thermoplastic resin film may be a single-layer film composed of one layer, or a multilayer structure composed of two or more layers laminated.
• a multilayer structure for example, in a film with a two-layer structure, any one of the two layers contains a lubricant, and in a film with a three-layer structure, a lubricant is contained in each of the three layers located on both surfaces. can be done.
• the type and content of the lubricant to be contained can be designed independently. With such a multilayer structure, the surface roughness of each surface of the thermoplastic resin film can be controlled independently.
• At least one surface of the thermoplastic resin film may be laminated with an easy-adhesion layer or subjected to corona treatment, plasma treatment, acid treatment, flame treatment, etc. in order to improve adhesion with other materials.
• the resin that constitutes the easy-adhesion layer is not particularly limited, and various resins can be used.
• resins include polyamide-based resins, polyurethane-based resins, polyester-based resins, acrylic-based resins, and epoxy-based resins.
• polyurethane-based resins, and acrylic resins are preferable, and from the viewpoint of heat resistance, polyamide-based resins, polyurethane-based resins, and acrylic-based resins are more preferable.
• the polyamide-based resin constituting the easy-adhesion layer is not particularly limited, and may include aliphatic polyamide, alicyclic polyamide, aromatic polyamide, and the like.
• Aromatic polyamides include semi-aromatic polyamides and wholly aromatic polyamides (aramids). From the viewpoint of improving adhesion to the semi-aromatic polyamide used as the base material, the same kind of semi-aromatic polyamide can be used as the easy-adhesion layer.
• these polyamide-based resins dimer acid-based polyamides are preferable from the viewpoint of excellent balance between heat resistance and adhesiveness.
• an aqueous dispersion of a polyamide resin can be used to form the easy-adhesion layer.
• Commercially available polyamide resin aqueous dispersions include, for example, Sepolsion PA-150 and PA-200 (manufactured by Sumitomo Seika Co., Ltd.).
• polyurethane resin aqueous dispersions include, for example, Hydran series (manufactured by DIC Corporation), Superflex series (manufactured by Daiichi Kogyo Seiyaku Co., Ltd.), Takelac series (manufactured by Mitsui Chemicals, Inc.), and Adeka Bontiter series (manufactured by Adeka Corporation). (manufactured by Sanyo Chemical Industries, Ltd.).
• polyester resin The polyester-based resin that constitutes the easy-adhesion layer is not particularly limited, and examples thereof include those composed of a polybasic acid component and a polyhydric alcohol component and produced by a known polymerization method.
• the polybasic acid component and the polyhydric alcohol component may be used alone or in combination of two or more.
• an aqueous dispersion of a polyester resin can be used to form the easy-adhesion layer.
• Commercially available polyester resin aqueous dispersions include, for example, Elitel KA-5034, KZA-0134, KZA-3556 (all manufactured by Unitika), Plascoat Z-730, RZ-142 (all manufactured by Goo Chemical Industry Co., Ltd.). etc. can be mentioned.
• the acrylic resin constituting the easy-adhesion layer is not particularly limited, and is mainly composed of ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, etc., and vinyl compounds such as styrene, methyl methacrylate, acrylonitrile, etc. and functional group monomers such as acrylic It is a copolymer of acid, methacrylic acid, itaconic acid, acrylamide, methylol acrylamide, hydroxyethyl acrylate, hydroxyethyl methacrylate, and the like.
• An aqueous acrylic resin dispersion can be used to form the easy-adhesion layer.
• aqueous acrylic resin dispersions include the Nikasol series (manufactured by Nippon Carbide Co., Ltd.), the Nanocryl series, the Lyocryl series (all manufactured by Toyochem), the Ultrasol series (manufactured by Aica Kogyo Co., Ltd.), and the Boncoat series (DIC company) and the like.
• thermoplastic resin film of the present invention may be laminated with inorganic substances such as metals or oxides thereof, other types of polymers, paper, woven fabrics, non-woven fabrics, wood, and the like.
• thermoplastic resin film of the present invention A laminate obtained by laminating the easy-adhesion layer on at least one side of the thermoplastic resin film of the present invention can be used for an LED mounting substrate, and the LED mounting substrate can be used for a flexible LED display. Further, the thermoplastic resin film of the present invention has excellent dimensional stability while having heat resistance, and thus can be used for various electronic materials, optical parts and other uses.
• packaging materials for pharmaceuticals packaging materials for foods such as retort food; packaging materials for electronic components such as semiconductor packages; electrical insulating materials for motors, transformers, cables, etc.; Materials: cassette tapes, magnetic tapes for digital data storage, magnetic tape materials for video tapes; solar cell substrates, liquid crystal panels, conductive films, protective plates for display devices, etc.; substrates for flexible printed wiring , flexible flat cables and other electronic substrate materials; coverlay films for flexible printed wiring, heat-resistant masking tapes, industrial process tapes and other heat-resistant tapes; heat-resistant barcode labels; heat-resistant reflectors; insulating tapes; Agricultural materials; medical materials; civil engineering and construction materials; filtration membranes, etc., and household and industrial materials.
• thermoplastic resin film of the present invention is excellent in the above properties, that is, heat resistance, dimensional stability, and transparency, so that it can be used for applications such as display materials and display devices in mobile devices and the like. Specifically, it is used as an optical substrate for various displays such as liquid crystal and organic EL, as a base film for various functional materials such as polarizing plates and retardation plates, and as a protective and sealing film for light emitting elements and display devices. can do.
• thermoplastic resin Melting point of thermoplastic resin, glass transition temperature Using a differential scanning calorimeter (PerkinElmer DSC-7), the thermoplastic resin is heated from 20 ° C. to 350 ° C. at 10 ° C./min under a nitrogen atmosphere. After the temperature was raised and held for 5 minutes (1st Scan), it was cooled from 350° C. to 20° C. at 100° C./min and held for 5 minutes. Further, the glass transition temperature in the process (2nd Scan) in which the temperature was reheated from 20° C. to 350° C. at 10° C./min was defined as the Tg of the thermoplastic resin. Similarly, the peak top temperature of the crystal melting peak observed in the 2nd Scan was taken as Tm.
• thermoplastic resin film The front and back surfaces of the thermoplastic resin film obtained by stretching are measured using an infrared spectrophotometer (manufactured by JASCO Corporation, infrared spectrophotometer FT/IR-6100). , FT-IR ATR measurements were performed. The ATR prism was diamond, the incident angle was 45°, the resolution was 4 cm ⁇ 1 , and the number of times of integration was 128.
• infrared spectrophotometer manufactured by JASCO Corporation, infrared spectrophotometer FT/IR-6100.
• the degree of crystallinity is, of the peaks in the range of 1100 to 1250 cm ⁇ 1 , the peak area present on the low wavelength side is P1 (peak derived from crystallization), and the peak area present on the high wavelength side is P2 (amorphous portion and the area ratio determined by P1/(P1+P2) was taken as the degree of crystallinity.
• thermoplastic resin film was cut into a piece having a width of 20 mm and a length of 120 mm.
• An etching mask patterned in the shape of a wiring pattern was formed on the metal foil surface of the obtained metal laminate. After that, the metal foil was removed with an immersion liquid at the portions not covered with the etching mask, and then the etching mask was removed with an alkaline peeling liquid. Finally, an LED element was soldered onto the obtained metal foil in the form of a wiring pattern to fabricate a simple LED mounting module.
• the sample was fixed on a horizontal surface plate so that the tip of the sample protruded by 100 mm, and the amount of deflection of the tip portion from the surface of the surface of the plate was measured, and stiffness was evaluated according to the following criteria. Practically, A to C are preferred, A and B are more preferred, and A is even more preferred. A: 25 mm or less B: More than 25 mm and less than 30 mm C: More than 30 mm and less than 35 mm D: More than 35 mm
• Thermoplastic resin Thermoplastic resin A The one manufactured by the following method was used. Terephthalic acid (TA) 3289 parts by mass, 1,9-nonanediamine (NDA) 2533 parts by mass, 2-methyl-1,8-octanediamine (MODA) 633 parts by mass, benzoic acid (BA) 48.9 parts by mass, the following 6.5 parts by mass of sodium phosphite monohydrate (0.1% by mass with respect to the total of the above four polyamide starting materials) and 2200 parts by mass of distilled water were placed in a reaction vessel and purged with nitrogen. The molar ratio (TA/BA/NDA/MODA) of these raw materials is 99/2/80/20.
• the internal temperature was raised to 210° C. over 2 hours.
• the pressure inside the reactor was increased to 2.12 MPa (22 kg/cm 2 ).
• the temperature was raised to 230°C, and then the temperature was kept at 230°C for 2 hours, and the reaction was carried out while gradually removing water vapor and maintaining the pressure at 2.12 MPa (22 kg/cm 2 ).
• the pressure was lowered to 0.98 MPa (10 kg/cm 2 ) over 30 minutes, and the reaction was continued for 1 hour to obtain a prepolymer. This was dried at a temperature of 100° C.
• Thermoplastic resin A had a melting point of 290, a glass transition temperature of 125° C., and an intrinsic viscosity of 1.17 dL/g.
• Thermoplastic resin B The one manufactured by the following method was used. Terephthalic acid (TA) 489 parts by mass, 1,10-decanediamine (DDA) 507 parts by mass, benzoic acid (BA) 2.8 parts by mass, sodium hypophosphite monohydrate 1.0 parts by mass (the above 0.1% by mass with respect to the total of the three raw materials for polyamide) and 1000 parts by mass of distilled water were placed in a reaction vessel and purged with nitrogen. The molar ratio (TA/BA/DDA) of these raw materials is 99/2/100. The contents of the reactor were stirred at 80°C for 0.5 hours at 28 revolutions per minute, and then heated to 230°C. After that, it was heated at 230° C. for 3 hours.
• TA Terephthalic acid
• DDA 1,10-decanediamine
• BA benzoic acid
• sodium hypophosphite monohydrate 1.0 parts by mass (the above 0.1% by mass with respect to the total of the three raw materials for polyamide)
• Thermoplastic resin B had a melting point of 316° C., a glass transition temperature of 150° C., and an intrinsic viscosity of 1.24 dL/g.
• Thermoplastic resin C Polyamide 6 resin (manufactured by Unitika, A1030BRF, monomer content of 1.0% or less, melting point of 223°C, glass transition temperature of 52°C, intrinsic viscosity of 3.10 dL/g)
• Thermoplastic resin D Polyethylene terephthalate resin (manufactured by Nippon Ester Co., Ltd., UT-CBR, melting point 255 ° C., glass transition temperature 78 ° C., intrinsic viscosity 0.67 dL / g)
• ⁇ Master chip (M3) 98 parts by mass of thermoplastic resin A and 2 parts by mass of silica Cs (manufactured by Fuji Silysia Chemical Ltd., average particle size 2.3 ⁇ m) were melt-kneaded.
• ⁇ Master chip (M4) 98 parts by mass of thermoplastic resin A, 1 part by mass of silica As, and 1 part by mass of silica Bs were melt-kneaded.
• ⁇ Master chip (M5) 98 parts by mass of thermoplastic resin A and 2 parts by mass of acrylic Da (manufactured by ENEOS Liquid Crystal, NMB-0220C, average particle size 2.0 ⁇ m) were melt-kneaded.
• ⁇ Master chip (M6) 98 parts by mass of thermoplastic resin A and 2 parts by mass of acrylic Ea (manufactured by ENEOS Liquid Crystal, NMB-0320C, average particle size 3.0 ⁇ m) were melt-kneaded.
• ⁇ Master chip (M7) 98 parts by mass of thermoplastic resin A, 1 part by mass of acrylic Da and 1 part by mass of acrylic Ea were melt-kneaded.
• ⁇ Master chip (M8) 98 parts by mass of thermoplastic resin A and 2 parts by mass of acrylic Fa (manufactured by ENEOS Liquid Crystal Co., Ltd., NMB-0520C, average particle size 5.0 ⁇ m) were melt-kneaded.
• ⁇ Master chip (M9) 98 parts by mass of thermoplastic resin A, 1 part by mass of acrylic Da, and 1 part by mass of acrylic Fa were melt-kneaded.
• ⁇ Master chip (M10) 98 parts by mass of thermoplastic resin B and 2 parts by mass of acrylic Da were melt-kneaded.
• ⁇ Master chip (M11) 98 parts by mass of thermoplastic resin C and 2 parts by mass of acrylic As were melt-kneaded.
• ⁇ Master chip (M12) 98 parts by mass of thermoplastic resin D and 2 parts by mass of acrylic As were melt-kneaded.
• ⁇ Master chip (M13) 98 parts by mass of thermoplastic resin D, 1 part by mass of acrylic Ea and 1 part by mass of acrylic Fa were melt-kneaded.
• Hindered phenol heat stabilizer GA 3,9-bis[2- ⁇ 3-(3-t-butyl-4-hydroxy-5-methylphenyl)propionyloxy ⁇ -1,1-dimethylethyl] -2,4,8,10-tetraoxaspiro[5.5]undecane (Sumilizer GA-80 manufactured by Sumitomo Chemical Co., thermal decomposition temperature 392 ° C.)
• Example 1 Thermoplastic resin A, GA and master chip (M1) were mixed so that 0.2 parts by mass of GA and 0.1 parts by mass of As silica were mixed with 100 parts by mass of thermoplastic resin A. This mixture is put into a 65 mm single-screw extruder with a cylinder temperature set to 320 ° C., melted, extruded into a sheet from a T-die set at 320 ° C., and electrostatically placed on a cooling roll with a surface temperature of 40 ° C. After contact and cooling, a substantially non-oriented, unstretched film having a thickness of 650 ⁇ m was obtained.
• Examples 2-28, Comparative Examples 1-7 Thermoplastic resin was prepared in the same manner as in Example 1 except that the type of thermoplastic resin, the type and content of fine particles, the thickness of the unstretched film, the stretch ratio, and the cooling treatment temperature were changed as shown in Tables 1 and 2. got the film. In Comparative Example 1, no cooling treatment was performed.
• Example 29 The thermoplastic resin C and the master chip (M11) were mixed so that the amount of silica As was 0.1 parts by mass with respect to 100 parts by mass of the thermoplastic resin C.
• This mixture is put into a 65 mm single screw extruder with a cylinder temperature set to 240 ° C., melted, supplied to a T die set to 240 ° C. and discharged in a sheet, and transferred to a metal drum whose temperature is adjusted to 20 ° C.
• a substantially non-oriented, unstretched film having a thickness of 780 ⁇ m was produced by winding, cooling and winding. Next, while holding both ends of this unstretched film with clips, it was led to a tenter-type sequential biaxial stretching machine, and sequential biaxial stretching was performed.
• the stretching conditions were a preheating zone temperature of 65° C., a stretching zone temperature of 96° C., a stretching strain rate of 3200%/min in the longitudinal direction and the transverse direction, a draw ratio of 2.8 times in the longitudinal direction and the transverse direction, respectively. was seven times.
• heat setting treatment is performed at 202 ° C. for 5 seconds
• relaxation treatment is performed at a relaxation rate of 3.0% in the width direction
• cooling treatment is performed at a temperature of 130 ° C. for 3 seconds
• a thermoplastic resin film having a thickness of 75 ⁇ m is obtained. Obtained.
• Example 30 The thermoplastic resin C and the master chip (M12) were mixed so that the amount of silica As was 0.1 parts by mass with respect to 100 parts by mass of the thermoplastic resin D. This mixture is put into a 65 mm single-screw extruder with a cylinder temperature set to 280 ° C., melted, supplied to a T-die set to 280 ° C., discharged in a sheet, and transferred to a metal drum whose temperature is adjusted to 20 ° C. A substantially non-oriented, unstretched film having a thickness of 780 ⁇ m was produced by winding, cooling and winding.
• Example 31 A thermoplastic resin film was obtained in the same manner as in Example 30, except that the type and content of fine particles and the thickness of the unstretched film were changed as shown in Table 2.
• Example 32 A thermoplastic resin film was obtained in the same manner as in Example 1, except that the relaxation treatment was performed at a relaxation rate of 3.0% in the width direction and at a relaxation rate of 1.0% in the longitudinal direction.
• Tables 1 and 2 show the composition of the thermoplastic resin film, the film manufacturing conditions, and the properties of the obtained thermoplastic resin film.
• thermoplastic resin films of Examples 1 to 32 satisfy all of the characteristic values defined in the present invention, have low haze, excellent transparency, high loop stiffness, sufficient stiffness, and bending resistance. It was also excellent in quality.
• the thermoplastic resin films of Comparative Examples 1-5 had low loop stiffness values, and the thermoplastic resin films of Comparative Examples 6-7 were inferior in haze.
• Comparative Example 1 is a thermoplastic resin film obtained under the same conditions as the film formation and stretching of Patent Document 1 (Example 12) cited as a prior art document, but cooling after stretching and heat setting. Since no treatment was performed, the crystallinity was 0.06 and the loop stiffness value was less than 140 mN/cm.

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• 2022
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