WO2011135985A1 - 太陽電池裏面保護材用積層ポリエステルフィルム - Google Patents
太陽電池裏面保護材用積層ポリエステルフィルム Download PDFInfo
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- WO2011135985A1 WO2011135985A1 PCT/JP2011/058641 JP2011058641W WO2011135985A1 WO 2011135985 A1 WO2011135985 A1 WO 2011135985A1 JP 2011058641 W JP2011058641 W JP 2011058641W WO 2011135985 A1 WO2011135985 A1 WO 2011135985A1
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- Prior art keywords
- polyester
- layer
- film
- polyester film
- solar cell
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B10/00—Integration of renewable energy sources in buildings
- Y02B10/10—Photovoltaic [PV]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
- Y10T428/31565—Next to polyester [polyethylene terephthalate, etc.]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
- Y10T428/31573—Next to addition polymer of ethylenically unsaturated monomer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
- Y10T428/31573—Next to addition polymer of ethylenically unsaturated monomer
- Y10T428/31576—Ester monomer type [polyvinylacetate, etc.]
Definitions
- the present invention relates to a laminated polyester film for a solar battery back surface protective material.
- the base film is a white film having a high reflectance, and is excellent in hydrolysis resistance, and is sealed in solar cells. Excellent water resistance against sealing resins such as ethylene-vinyl acetate copolymer resin (hereinafter abbreviated as EVA) and polyvinyl butyral resin (hereinafter abbreviated as PVB) used as a material.
- EVA ethylene-vinyl acetate copolymer resin
- PVB polyvinyl butyral resin
- the present invention relates to a laminated polyester film for solar cell back surface protective material having adhesiveness.
- solar power generation has attracted a great deal of attention as an energy source that is clean and useful for preventing global warming, and has already begun to spread considerably.
- a solar cell using a semiconductor such as single crystal silicon, polycrystalline silicon, amorphous silicon, and the like can be given.
- a solar cell is a practical application of the principle that current can be taken out when sunlight hits a semiconductor.
- One of the recent attention is a relatively large solar cell. These solar cells are installed in unused places such as deserts and wasteland, and roofs of houses or large buildings, all of which are exposed to the sun and exposed to natural conditions outdoors. Is.
- the performance of a solar cell is significantly reduced when moisture is applied to a semiconductor cell as a heart, the solar cell is required to have a package that can withstand a natural environment with severe strength and water resistance for a long time. Moreover, since it installs in roofs, such as a house, weight reduction of a solar cell is also requested
- a solar cell module is generally a solar cell, that is, a semiconductor, by inserting a sealing material resin such as EVA between a glass substrate as a front surface side transparent protective member on the light receiving surface side and a back surface protective material film.
- a sealing material resin such as EVA
- the adhesion between the polyester film and EVA, etc. is weak, and for example, an easy-adhesive layer is applied or an adhesive is used to improve the adhesion. Is required.
- the solar cell module is assumed to be used outdoors for a long period (for example, 20 years or more), and may be exposed to a high temperature and high humidity environment.
- the polyester film as a solar cell protective material, hydrolysis of the ester bond site in the molecular chain occurs, it is considered as one problem that the mechanical properties of the film itself deteriorates over time, the other, It is speculated that the easy-adhesion layer for improving thermal adhesiveness with EVA or the like also deteriorates over time in a high-temperature and high-humidity environment, and the adhesiveness with EVA or the like cannot be maintained.
- a white film containing titanium dioxide or barium sulfate in polyester is disclosed. And as a polyester resin, the thing excellent in hydrolysis resistance is used, and the white polyester film has the suitability for solar cell back surface protection materials.
- the base film is a white film having a high reflectivity, and is excellent in hydrolysis resistance, and further provided thereon. It is to provide a laminated polyester film for a solar battery back surface protective material having excellent water resistance and adhesion to a sealing resin such as EVA or PVB that is used as a sealing material for solar cells by an application layer.
- the gist of the present invention is a laminated polyester film having the following polyester A layer in at least one outermost layer and including at least one layer of the following polyester B layer, and the amount of terminal carboxyl groups of the laminated polyester film is 26 equivalents / ton or less. And a coating layer formed of a polyurethane having at least one of a polycarbonate skeleton or a polyether skeleton and a cross-linking agent on at least one surface of the polyester A layer. It exists in the polyester film.
- Polyester A layer A layer composed of a polyester having an aromatic polyester as a main constituent and a white pigment content of less than 8% by weight.
- Polyester B layer An aromatic polyester as a main constituent and a white pigment content. Layer of polyester that is 8% by weight or more
- the film of the present invention is a laminated polyester film for solar cell back surface protective material
- the base film is a white film having a high reflectance, and is excellent in hydrolysis resistance as a base film, and further provided thereon.
- the coated layer has excellent water resistance and adhesion to sealing resins such as EVA and PVB used as a sealing material for solar cells, and its industrial utility value is high.
- the polyester film as a base material has excellent hydrolysis resistance even in a high-temperature and high-humidity environment, and at the same time, the coating layer for improving adhesion imparted thereon also has hydrolysis resistance. Therefore, it is based on the technical idea that it has hydrolysis resistance as an easy-adhesive film for the first time. If either the polyester film of the substrate or the coating layer provided on it is inferior in hydrolysis resistance, the hydrolysis resistance of the easy-adhesive film is strongly influenced by the inferior one. And become insufficient. Therefore, in order to make a polyester film excellent in hydrolysis resistance as an easily adhesive film, it is an indispensable element that both the base film and the coating layer are excellent in hydrolysis resistance. Based on this technical idea, the polyester film as the base material of the present invention and the coating layer will be roughly divided and explained in order.
- the polyester film serving as the substrate of the present invention has a layer (polyester A layer) made of polyester having an aromatic polyester as a main constituent and a white pigment content of less than 8% by weight in at least one outermost layer.
- a layer made of polyester having an aromatic polyester as a main constituent and a white pigment content of less than 8% by weight in at least one outermost layer.
- the entire film is a laminated polyester film comprising at least one layer (polyester B layer) made of polyester having an aromatic polyester as a main constituent and a white pigment content of 8% by weight or more.
- the amount of terminal carboxyl groups needs to be 26 equivalents / ton or less.
- the polyester used as the base material of the film of the present invention refers to an aromatic polyester obtained by polycondensation of an aromatic dicarboxylic acid and an aliphatic glycol.
- the aromatic dicarboxylic acid include terephthalic acid, isophthalic acid, and 2,6-naphthalenedicarboxylic acid.
- the aliphatic glycol include ethylene glycol, diethylene glycol, and 1,4-cyclohexanedimethanol.
- PET polyethylene terephthalate
- PET polyethylene terephthalate
- a polyethylene terephthalate film can be preferably used as the polyester film.
- the polyester raw material of the polyester film used as the base material of the present invention may be a metal compound polymerization catalyst such as antimony, titanium, germanium and the like that are usually used in the polymerization of polyester.
- a metal compound polymerization catalyst such as antimony, titanium, germanium and the like that are usually used in the polymerization of polyester.
- the amount of these catalysts is large, when the polyester for film formation is melted, the decomposition reaction is likely to occur, the terminal carboxylic acid concentration is increased due to the decrease in molecular weight, etc., and the hydrolysis resistance is inferior. Become.
- the amount of the polymerization catalyst is too small, the polymerization reaction rate decreases, so that the polymerization time becomes longer and the terminal carboxylic acid concentration becomes higher, resulting in deterioration of hydrolysis resistance.
- antimony is usually 50 to 400 ppm, preferably 100 to 350 ppm
- titanium is usually 1 to 20 ppm, preferably 2 to 15 ppm
- germanium is usually 3 to 50 ppm, preferably 5 It should be in the range of ⁇ 40 ppm.
- These polymerization catalysts can also be used in combination of two or more.
- the polyester film serving as the substrate of the present invention has a layer (polyester A layer) made of polyester having an aromatic polyester as a main constituent and a white pigment content of less than 8% by weight in at least one outermost layer.
- the laminated polyester film contains at least one layer (polyester B layer) made of polyester having an aromatic polyester as a main constituent and a white pigment content of 8% by weight or more.
- the white pigment examples include titanium dioxide, zinc oxide, zinc sulfide, and barium sulfate.
- titanium dioxide and barium sulfate are preferable, and furthermore, when the crystal type is anatase type titanium dioxide, it is particularly preferable because high concealability and light resistance can be obtained.
- the average particle diameter of the white pigment is usually 0.1 to 1.0 ⁇ m, preferably 0.2 to 0.5 ⁇ m.
- the optical density (OD) of the film becomes small and the light reflection performance of the polyester film is effectively improved with respect to the amount of white pigment added. Can be difficult.
- the polyester A layer constituting at least one outermost layer of the film of the present invention needs to have a content of the white pigment of less than 8% by weight.
- This content is preferably 5% by weight or less, It is preferably 3% by weight or less, and the lower limit is 0% by weight, that is, the white pigment may not be contained.
- the content of the white pigment is 8% by weight or more, it tends to be inferior in water resistance and adhesion to a coating layer provided on one surface of the polyester A layer described later and a sealing resin such as EVA or PVB. Therefore, it is not preferable.
- At least one polyester B layer provided on the polyester film for solar cell back surface protective material of the present invention is required to have a content of the white pigment of 8% by weight or more.
- This content is preferably 10% by weight or more, more preferably 15% by weight or more, and the upper limit is not particularly defined, but 30% by weight which tends to decrease the mechanical strength of the polyester B layer is a guideline. Is good.
- the content of the white pigment in the polyester B layer is less than 8 weight, the optical density (OD) of the entire polyester film becomes small, and the light reflection performance becomes insufficient when used as a film for solar cell back surface protective material. Cheap.
- particles may be blended in addition to the above-mentioned white pigment for the main purpose of imparting slipperiness.
- the type of particles to be blended is not particularly limited as long as it is a particle capable of imparting slipperiness, and specific examples thereof include, for example, silica, calcium carbonate, magnesium carbonate, barium carbonate, calcium sulfate, silicon oxide, and kaolin. And particles such as aluminum oxide.
- the heat-resistant organic particles described in JP-B-59-5216, JP-A-59-217755, etc. may be used. Examples of other heat-resistant organic particles include thermosetting urea resins, thermosetting phenol resins, thermosetting epoxy resins, benzoguanamine resins, and the like.
- precipitated particles obtained by precipitating and finely dispersing a part of a metal compound such as a catalyst during the polyester production process can also be used.
- the particles used for imparting slipperiness usually have an average particle size of preferably 0.1 to 10 ⁇ m, and the addition amount can be selected in the range of 0.005 to 5.0% by weight.
- the method for adding the white pigment and the slipperiness imparting particles to the polyester film is not particularly limited, and a conventionally known method can be adopted.
- it can be added at an arbitrary stage for producing the polyester as a raw material, but it may be added preferably after the esterification stage or after the transesterification reaction to proceed the polycondensation reaction.
- a twin screw extruder with a vent a method of kneading a slurry of particles dispersed in ethylene glycol or water and a polyester raw material, or a method of kneading dried particles and a polyester raw material, etc. Is called.
- a white pigment in the case of a white pigment, it is added to the polyester raw material as a high-concentration masterbatch, and it is used in the form of diluting it when the film is formed.
- the amount of terminal carboxylic acid groups of the polyester constituting the film It is preferable in terms of lowering.
- an ultraviolet absorber can be contained in the range of 0.01 to 5 parts by weight with respect to the polyester.
- the ultraviolet absorber include triazines, benzophenones, and benzoxazinones. Among these, benzoxazinone ultraviolet absorbers and the like are preferably used.
- a method of adding these ultraviolet absorbers to the intermediate layer can also be preferably used.
- these ultraviolet absorbers and additives can be prepared as a high-concentration master batch, and can be diluted and used during film formation.
- the film of the present invention needs to include the above-described polyester B layer as at least one outermost layer and further include the above-described polyester B layer.
- the simplest laminated structure of the film is A layer / B layer, but other than this, for example, A layer / B layer / A layer or A layer / intermediate layer / A layer B layer may be present in the inside, or the other outermost layer of the other C layer may be the A layer / B layer / C layer or the A layer / intermediate layer / C layer as the B layer in the intermediate layer
- the structure which exists may be sufficient.
- a coating layer is provided on the B layer (for example, when the B layer alone or the B layer / A layer / B layer). It is found that the water resistance and adhesion to the polyester film and the coating layer provided on the polyester film are improved compared to the case of forming both outermost surfaces with a polyester B layer with a large amount of white pigment added as in FIG. It is. The reason for this is not clear, but the polyester film containing a large amount of white pigment has a considerable effect on the white pigment at high temperatures and high humidity, and is very close to the interface between the polyester film and the coating layer. This is presumed to promote the hydrolysis of. On the other hand, when the coating layer is present on a polyester film having a small amount of white pigment, the film is hardly hydrolyzed in the vicinity of the interface between the polyester film and the coating layer. It is presumed that the adhesion is maintained.
- the thickness ratio of the polyester A layer and the polyester B layer is not particularly limited, but the minimum thickness of these layers is preferably 0.5 ⁇ m or more, more preferably 1 ⁇ m, because delamination hardly occurs. That's it.
- the method for laminating the polyester film in the present invention a so-called coextrusion method using two or three or more melt extruders is preferably used.
- the thickness of the polyester film is not particularly limited as long as it can be formed into a film, but is usually 20 to 500 ⁇ m, preferably 25 to 300 ⁇ m.
- the film of the present invention is required to have a terminal carboxylic acid amount of 26 equivalents / ton or less when the entire film (part excluding the coating layer and white pigment) is measured by the measurement method described later, preferably 24 equivalents / ton or less. If the amount of terminal carboxylic acid exceeds 26 equivalents / ton, the hydrolysis resistance of the polyester film is poor.
- the hydrolysis resistance of the polyester film is a characteristic relating to the whole film, and in the present invention, the amount of terminal carboxylic acid as the whole polyester constituting the film needs to be within the above-mentioned range.
- there is no lower limit of the amount of terminal carboxylic acid of the polyester but it is usually 10 equivalent / It is about tons.
- the process of melt extrusion of the polyester chip in film production a) avoiding hydrolysis as much as possible from the moisture contained in the polyester chip, b) It is carried out by making the residence time of the polyester in the extruder and the melt line as short as possible.
- a when a single screw extruder is used, the raw material is sufficiently dried in advance so that the water content is 50 ppm or less, preferably 30 ppm or less.
- a twin screw extruder is used.
- a method of providing a vent port and maintaining a reduced pressure of 40 hectopascals or less, preferably 30 hectopascals or less, and more preferably 20 hectopascals or less can be employed.
- the residence time from when the raw material is charged into the extruder to when the molten sheet starts to be discharged from the die is 20 minutes or less, more preferably 15 minutes or less.
- the amount of terminal carboxylic acid in the raw material polyester is preferably 20 equivalents / ton, more preferably 15 equivalents / ton or less.
- Conventionally known methods such as a method of increasing the polymerization efficiency, a method of increasing the polymerization rate, a method of suppressing the decomposition rate, and a combination of melt polymerization and solid phase polymerization are used as methods for reducing the amount of terminal carboxylic acid in the polyester chip. Can be adopted.
- a method for shortening the polymerization time a method for increasing the amount of polymerization catalyst, a method using a highly active polymerization catalyst, a method for lowering the polymerization temperature, or the like.
- solid phase polymerization in combination it may be formed into chips after melt polymerization and subjected to solid phase polymerization in a temperature range of 180 to 240 ° C. in an inert stream such as nitrogen under heating or under pressure.
- the intrinsic viscosity is preferably 0.55 dl / g or more, and more preferably 0.60 to 0.90 dl / g.
- the amount of terminal carboxylic acid increases when a regenerated raw material that has undergone a melting step is added, it is preferable not to add such a regenerated raw material in the present invention. preferable.
- the polyester film used as the base material of the present invention preferably has an amount of phosphorus element detected by analysis using a fluorescent X-ray analyzer described later in the range of 0 to 170 ppm when the entire film is measured. More preferably, it is in the range of 0 to 140 ppm, and may be 0 ppm.
- the phosphorus element is usually derived from a phosphoric acid compound, and is added as a catalyst component during polyester production. In the present invention, when the phosphorus element amount satisfies the above range, hydrolysis resistance can be imparted to the film. If the amount of phosphorus element is too large, hydrolysis caused by the phosphate compound is promoted, which is not preferable.
- the hydrolysis resistance of the polyester film is a characteristic relating to the entire film, and in the present invention, the phosphorus content is preferably within the above-mentioned range for the entire polyester constituting the film.
- Examples of phosphoric acid compounds include known ones such as phosphoric acid, phosphorous acid or esters thereof, phosphonic acid compounds, phosphinic acid compounds, phosphonous acid compounds, and phosphinic acid compounds.
- Phosphoric acid monomethyl phosphate, dimethyl phosphate, trimethyl phosphate, monoethyl phosphate, diethyl phosphate, triethyl phosphate, ethyl acid phosphate, monopropyl phosphate, dipropyl phosphate, tripropyl phosphate, monobutyl phosphate Fate, dibutyl phosphate, tributyl phosphate, monoamyl phosphate, diamyl phosphate, triamyl phosphate, monohexyl phosphate, dihexyl phosphate, Such as re-hexyl phosphate, and the like.
- the method for producing a polyester film of the present invention will be specifically described, but the present invention is not particularly limited to the following examples as long as the gist of the present invention is satisfied.
- polyester chips dried by a known method are supplied to a single screw extruder, or undried polyester chips are supplied to a twin screw extruder, and heated and melted to a temperature equal to or higher than the melting point of each polymer.
- a known appropriate polymer filter may be passed through in order to remove foreign substances, or a method of reducing the pulsation of the molten polymer using a gear pump can be employed.
- the melted polymers are merged and laminated, extruded from the die, and rapidly cooled and solidified on the rotary cooling drum so that the temperature is equal to or lower than the glass transition temperature to obtain a substantially amorphous unoriented sheet.
- the electrostatic application adhesion method and / or the liquid application adhesion method are preferably employed.
- the sheet thus obtained is stretched in a biaxial direction to form a film.
- the unstretched sheet is preferably stretched 2 to 6 times in the machine direction (MD direction) at 70 to 145 ° C. to form a longitudinal uniaxially stretched film, and then the transverse direction (TD direction).
- MD direction machine direction
- TD direction transverse direction
- heat treatment may be performed under the same conditions.
- a method of relaxing 0.1 to 20% in the vertical direction and / or the horizontal direction in the maximum temperature zone of the heat treatment and / or the cooling zone at the heat treatment outlet is preferable. Further, it is possible to add re-longitudinal stretching and re-lateral stretching as necessary.
- the polyester film for solar cell back surface protective material of the present invention is a layer comprising at least one outermost layer of polyester having an aromatic polyester as a main constituent and a white pigment content of less than 8% by weight.
- Polyester A layer but it is necessary to have a coating layer containing a polyurethane having at least one of a polycarbonate skeleton or a polyether skeleton and a crosslinking agent on at least one surface of the polyester A layer. It is.
- coating layer / A layer / B layer (/ coating layer), coating layer / A layer / B layer / A layer (/ coating layer), coating layer / A layer / intermediate layer / A layer (/ coating layer)
- the configuration in which the B layer is present in the intermediate layer, coating layer / A layer / B layer / C layer (/ coating layer), and coating layer / A layer / intermediate layer / C layer (/ coating layer) It is a structure etc. in which the B layer exists, (/ coating layer) means a coating layer which is not essential.
- the coating layer is provided on the surface of the polyester A layer with a small amount of white pigment added, so that it is more resistant to hydrolysis than when directly provided on the surface of the polyester B layer with a large amount of white pigment added.
- the application layer for adhesive improvement is also based on the technical idea that it has hydrolysis resistance as an easily adhesive film by having hydrolysis resistance.
- the coating layer in the present invention includes various solar cell sealing resins such as EVA, PVB, ethylene-methyl acrylate copolymer (EMA), ethylene-ethyl acrylate (EEA), and ethylene- ⁇ -olefin copolymer.
- EVA ethylene-methyl acrylate copolymer
- ESA ethylene-ethyl acrylate
- ethylene- ⁇ -olefin copolymer ethylene- ⁇ -olefin copolymer.
- the polyurethane having a polycarbonate skeleton or a polyether skeleton is obtained by using a compound having a polycarbonate skeleton or a polyether skeleton as a polyol.
- the polycarbonate polyol used for the polyurethane of the coating layer can be obtained, for example, by reaction of diphenyl carbonate, dialkyl carbonate, ethylene carbonate or phosgene with a diol.
- the diol include ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 1,5-pentanediol, , 6-hexanediol, 1,4-cyclohexanediol, 1,4-cyclohexanedimethanol, 1,7-heptanediol, 1,8-octanediol, 1,9-nonanediol, 1,10-decanediol, neo
- Examples include pentyl glycol, 3-methyl-1,5-pentanediol, and 3,3-dimethyl
- Polycarbonate polyol is preferably 300 to 5000 in terms of polystyrene-reduced number average molecular weight by gel permeation chromatography (GPC).
- the polyether polyol used for the polyurethane of the coating layer includes polyoxyethylene polyol (polyethylene glycol, etc.), polyoxypropylene polyol (polypropylene glycol, etc.), polyoxytetramethylene polyol (polytetramethylene ether glycol, etc.), and copolymer polyether.
- polyols block copolymers such as polyoxyethylene glycol and polyoxypropylene glycol, random copolymers, etc.
- polyoxytetramethylene glycol is preferable because it is excellent in terms of improving adhesiveness and also has good hydrolysis resistance.
- the polyether polyol is preferably 300 to 5000 in terms of number average molecular weight in terms of polyethylene glycol by gel permeation chromatography (GPC).
- the polyurethane using the above-described polycarbonate polyol or polyether polyol has better resistance to hydrolysis than the polyurethane using polyester polyol, which is another general-purpose polyol.
- polycarbonate polyols or polyether polyols may be used alone or in combination of two or more. As described above, these polycarbonate polyols and polyether polyols can be used in combination.
- polyisocyanate used for the polyurethane of the coating layer examples include known aliphatic, alicyclic and aromatic polyisocyanates.
- aliphatic polyisocyanate examples include, for example, tetramethylene diisocyanate, dodecamethylene diisocyanate, hexamethylene diisocyanate, 2,2,4-trimethylhexamethylene diisocyanate, 2,4,4-trimethylhexamethylene diisocyanate, 2-methylpentane- Examples thereof include 1,5-diisocyanate and 3-methylpentane-1,5-diisocyanate.
- alicyclic polyisocyanate examples include, for example, isophorone diisocyanate, hydrogenated xylylene diisocyanate, hydrogenated diphenylmethane-4,4′-diisocyanate, hydrogenated biphenyl-4,4′-diisocyanate, 1,4-cyclohexane diisocyanate.
- hydrogenated tolylene diisocyanate 1,3-bis (isocyanatomethyl) cyclohexane, 1,4-bis (isocyanatomethyl) cyclohexane and the like.
- aromatic polyisocyanate examples include tolylene diisocyanate, 2,2′-diphenylmethane diisocyanate, 2,4′-diphenylmethane diisocyanate, 4,4′-diphenylmethane diisocyanate, 4,4′-diphenyldimethylmethane diisocyanate, Examples include 4,4′-dibenzyl diisocyanate, 1,5-naphthalene diisocyanate, xylylene diisocyanate, 1,3-phenylene diisocyanate, 1,4-phenylene diisocyanate, and the like.
- These polyisocyanates may be used alone or in combination of two or more.
- chain extenders examples include ethylene glycol, propylene glycol, butanediol, diethylene glycol, neopentyl glycol, trimethylolpropane, hydrazine, ethylenediamine, diethylenetriamine, isophoronediamine, 4,4′-diaminodiphenylmethane, 4,4 ′. -Diaminodicyclohexylmethane, water, etc.
- the polyurethane having at least one of a polycarbonate structure and a polyether structure used for the coating layer of the present invention may be one using an organic solvent as a medium, but is preferably one containing water as a medium.
- an organic solvent as a medium
- a self-emulsification type in which an ionic group is introduced into the skeleton of a polyurethane resin to form an ionomer is preferable because of excellent storage stability of the liquid and water resistance, transparency and adhesiveness of the resulting coating layer.
- examples of the anionic group include a carboxylate group, a sulfonate group, a phosphate group, and a phosphonate group
- examples of the cationic group include quaternary ammonium
- carboxylic acid groups as examples of anionic groups include dimethylolpropionic acid, dimethylolbutanoic acid, bis- (2-hydroxyethyl) propionic acid, bis- (2-hydroxyethyl) butanoic acid, trimellitic acid- Ammonium salts such as bis (ethylene glycol) ester, lower amine salts, and the like can be preferably used.
- quaternary ammonium of the cationic group a quaternized product such as N-alkyl dialkanolamine such as N-methyldiethanolamine and N-ethyldiethanolamine can be preferably used.
- the carboxylate is a base and the counter ion is an organic amine having a boiling point of 150 ° C. or lower such as ammonia or triethylamine, an oxazoline-based crosslinking agent or a carbodiimide-based crosslinking agent described later It is particularly preferable in that it has a high reactivity with and increases the crosslink density of the coating layer.
- a resin having an ionic group can be used as a copolymerization component, or a component having an ionic group can be used as one component such as a polyol or a chain extender.
- crosslinking agent in addition to the above-mentioned polyurethane, it is necessary to use a crosslinking agent in combination with the coating layer of the present invention in order to impart heat resistance, heat-resistant adhesiveness, moisture resistance, and blocking resistance to the coating layer.
- This cross-linking agent is preferably water-soluble or water-dispersible.
- melamine compounds benzoguanamine compounds, urea compounds, acrylamide compounds, which are methylolated or alkoxymethylolated, epoxy compounds
- an oxazoline-based compound or a carbodiimide-based compound, which is a polymer itself is particularly preferable because the heat and moisture resistance adhesion of the coating layer is greatly improved.
- an oxazoline-based crosslinking agent is industrially available, for example, under the trade name Epocross (registered trademark) of Nippon Shokubai Co., Ltd. .
- the amount of these crosslinking agents added is 10/90 to 90/10, preferably 20/80 to 80/20, by weight ratio to the polyurethane in the coating layer (crosslinking agent / polyurethane). Is preferred.
- the total of the polyurethane and the crosslinking agent component described above is preferably present in an amount of 50% by weight or more, and more preferably 75% by weight or more.
- other resins can be additionally added.
- the resin component that can be additionally added include polyester resins, acrylic resins, polyvinyl resins, and polyester polyurethane resins.
- polyester resins and polyester polyurethane resins are often poor in hydrolysis resistance, and these resins are preferably not added to the coating layer, or even if added, the added amount is preferably less than 10% by weight.
- fine particles for example, inorganic particles such as silica, alumina, and metal oxide, or organic particles such as crosslinked polymer particles can be used.
- the size of the fine particles is 150 nm or less, preferably 100 nm or less, and the addition amount in the coating layer is preferably selected in the range of 0.5 to 10% by weight.
- the coating layer may contain components other than those described above as necessary.
- surfactants for example, surfactants, antifoaming agents, coatability improvers, thickeners, antioxidants, antistatic agents, ultraviolet absorbers, foaming agents, dyes, pigments and the like. These additives may be used alone or in combination of two or more.
- the coating layer in the present invention is preferably coated on the polyester film as a coating solution mainly containing water.
- the polyester film to be applied may be biaxially stretched in advance, but it is preferable to use a so-called in-line coating method in which the polyester film is stretched in at least one direction after being applied and further heat-set.
- the polyester film and the coating layer are usually heat-set at a high temperature of 200 ° C. or higher at the same time, so that the thermal crosslinking reaction of the coating layer proceeds sufficiently and the adhesion to the polyester film is improved.
- the coating solution is usually an organic solvent compatible with water in an amount of 20% by weight or less for the purpose of improving the dispersibility and storage stability, or improving the coating properties and coating film properties. It is also possible to add one kind or two or more kinds.
- any known method can be applied as a method of applying the coating solution to the polyester film as the substrate. Specifically, roll coating method, gravure coating method, micro gravure coating method, reverse coating method, bar coating method, roll brush method, spray coating method, air knife coating method, impregnation method, curtain coating method, die coating method, etc. It can be applied alone or in combination.
- the coating layer in the present invention has a coating amount of 0.005 to 1.0 g as a final dry film after being dried and solidified, or after being biaxially stretched or heat-set. / M 2 , more preferably in the range of 0.01 to 0.5 g / m 2 .
- the coating amount is less than 0.005 g / m 2, there is a tendency that adhesion becomes insufficient, when it exceeds 1.0 g / m 2 is no longer the adhesive is saturated, such as blocking the reverse There is a tendency that the adverse effects of are likely to occur.
- the coating layer of the present invention may be provided only on one side of the polyester film or on both sides. Furthermore, it is also possible to provide a coating layer coating layer containing a polyurethane having at least one of the above-described polycarbonate skeleton or polyether skeleton and a crosslinking agent on one side and to provide another coating layer on the opposite side. .
- the coating layer provided on the opposite surface for example, when an antistatic coating layer, a metal or metal oxide deposition layer is formed, an easily adhesive coating layer for this deposition layer, or when a known adhesive is applied Examples thereof include an easily adhesive coating layer for the adhesive layer.
- the coating layer is provided on the surface of the polyester A layer with a small amount of white pigment added compared to the surface of the polyester B layer with a large amount of white pigment added. It shows adhesiveness.
- the laminated structure of the polyester film is the coating layer / A layer / B layer / A layer / other coating layer of the present invention, or the coating layer / A layer / intermediate layer / A layer / others of the present invention. It is preferable that the coating layer has a layer B in the intermediate layer, and that both layers have the layer A, so that an adhesive having excellent hydrolysis resistance can be exhibited.
- Amount of terminal carboxylic acid (equivalent / ton): The amount of terminal carboxylic acid was measured by a so-called titration method. That is, polyester was dissolved in benzyl alcohol, phenol red indicator was added, and titrated with a water / methanol / benzyl alcohol solution of sodium hydroxide. If there is a coating layer on the film, in order to eliminate this effect, wash the coating layer with water using a cleanser containing abrasives, rinse thoroughly with ion-exchanged water, and dry, then measure in the same way. went.
- the polyester film contains white pigments such as titanium dioxide or barium sulfate
- the polyester film can be appropriately adjusted to those obtained by removing the white pigment, which is an insoluble component in benzyl alcohol, by centrifugal sedimentation.
- the terminal carboxyl group amount (equivalent / ton) relative to the component was determined.
- the retention rate (%) of the breaking elongation before and after the treatment was calculated by the following formula (1), and judged according to the following criteria.
- Breaking elongation retention rate breaking elongation after treatment ⁇ breaking elongation before treatment ⁇ 100 (1) ⁇ : Retention rate is 80% or more ⁇ : Retention rate is less than 60-80% ⁇ : Retention rate is less than 30-60% ⁇ : Retention rate is less than 30%
- Adhesive strength with EVA Two pieces of polyester film having a length of 300 mm and a width of 25 mm were cut out so that the longitudinal direction was the MD direction. On the other hand, one piece of the EVA film having a length of 50 mm and a width of 25 mm was cut out and stacked so that the EVA film was sandwiched between the application layer surfaces of the two pieces of the polyester film. This was laminated using a heat seal device (TP-701, manufactured by Tester Sangyo Co., Ltd.). The EVA film used was 485.00 (standard curing type, thickness 0.5 mm) manufactured by Etimex, Germany, and the heat seal conditions were a temperature of 150 ° C. and a pressure of 0.13 MPa for 20 minutes.
- a sample having a length of 300 mm and a width of 15 mm is cut out from a polyester film / EVA film laminate piece having a width of 25 mm.
- the non-laminated end of this 15 mm wide polyester film piece is mounted in a tensile / bending tester (EZGraph manufactured by Shimadzu Corporation).
- EZGraph tensile / bending tester
- the force (adhesive strength) required to separate the polyester film / EVA film laminate at an angle of 180 ° and a speed of 100 mm / min was measured for 10 samples, and the average values were classified as follows. did.
- A Adhesive strength of 50 N / 15 mm width or more
- B Adhesive strength of 30 N / 15 mm width to less than 50 N / 15 mm width
- ⁇ Adhesive strength of 10 N / 15 mm width to less than 30 N / 15 mm width
- ⁇ Adhesive strength of less than 10 N / 15 mm width
- Adhesive strength retention rate (%) (Adhesive strength after wet heat treatment) / (Adhesive strength before wet heat treatment) ⁇ : Retention rate is 70% or more ⁇ : Retention rate is 50 to less than 70% ⁇ : Retention rate is less than 50% ⁇ : Degradation of the polyester film itself is significant, and tearing or damage occurs
- Adhesiveness with polyvinyl butyral (PVB) -Creation of PVB sheet for evaluation: Powdered PVB (molecular weight about 110,000, butyralization degree 65 mol%, hydroxyl group amount about 34 mol%) 6 parts by weight, tri (ethylene glycol) -bis-2-ethylhexanoate (plasticizer) 4 parts by weight After mixing with 45 parts by weight of toluene and swelling, 45 parts by weight of ethanol was added and dissolved. This solution was put into a petri dish made of Teflon (registered trademark) and dried in a hot air oven at 100 ° C. for 1 hour to prepare a PVB sheet having a thickness of about 0.4 mm.
- Teflon registered trademark
- Adhesion evaluation The PVB sheet is cut into a width of 1 cm and a length of 10 cm, sandwiched between two test films so that the easy adhesion surface faces the sheet, and thermocompression bonded with a heat seal tester (TP-701, manufactured by Tester Sangyo Co., Ltd.). The conditions are as follows. Pressure: 0.13 MPa Temperature: 140 ° C Time: 3 minutes After the whole day and night, the pressure-bonded portion was peeled off by hand, and the adhesion was judged according to the following criteria.
- Adhesive strength is good (the test film or PVB sheet is damaged or peels off at the adhesive interface but has strong force)
- Adhesive strength is normal (peeling at the bonding interface but light response)
- Adhesive strength is poor (There is almost no response at the adhesive interface, and it peels easily)
- XX Degradation of the polyester film itself is significant and tearing or damage occurs
- polyester raw material used in the following examples will be described.
- Method for producing polyester (1) Using 100 parts by weight of dimethyl terephthalate and 60 parts by weight of ethylene glycol as starting materials, 0.09 parts by weight of magnesium acetate tetrahydrate as a catalyst is placed in the reactor, the reaction start temperature is set to 150 ° C., and the methanol is distilled off gradually. The reaction temperature was raised to 230 ° C. after 3 hours. After 4 hours, the transesterification reaction was substantially terminated. 0.04 part by weight of antimony trioxide was added to this reaction mixture, and a polycondensation reaction was performed for 4 hours. That is, the temperature was gradually raised from 230 ° C. to 280 ° C.
- the obtained polyester (1) had an intrinsic viscosity of 0.61, and the terminal carboxylic acid content of the polymer was 32 equivalents / ton.
- Polyester (1) was used as a starting material, and solid phase polymerization was performed at 220 ° C. under vacuum to obtain polyester (2).
- the intrinsic viscosity of the polyester (2) was 0.81, and the terminal carboxylic acid content of the polymer was 8 equivalents / ton.
- polyester (3) was obtained in the same manner except that 0.1 part by weight of silica particles having an average particle diameter of 2.6 ⁇ m dispersed in ethylene glycol was added after the transesterification reaction. .
- the obtained polyester (3) had an intrinsic viscosity of 0.61, and the terminal carboxylic acid content of the polymer was 28 equivalents / ton.
- Polyester (3) was used as a starting material, and solid phase polymerization was performed at 220 ° C. under vacuum to obtain polyester (4).
- the intrinsic viscosity of the polyester (4) was 0.73, and the terminal carboxylic acid content of the polymer was 10 equivalents / ton.
- polyester (5) ⁇ Method for producing polyester (5)>
- the same method except that 0.047 part by weight of orthophosphoric acid (0.015 part as phosphorus element) was added after the transesterification and then 0.04 part by weight of antimony trioxide was added.
- polyester (5) was obtained.
- the obtained polyester (5) had an intrinsic viscosity of 0.61, and the terminal carboxylic acid content of the polymer was 29 equivalents / ton.
- Polyester (5) was used as a starting material, and solid phase polymerization was performed at 220 ° C. under vacuum to obtain polyester (6).
- the intrinsic viscosity of the polyester (6) was 0.73, and the amount of terminal carboxylic acid in the polymer was 10 equivalents / ton.
- the polyester (2) is subjected to a twin screw extruder with a vent, and barium sulfate particles (particle diameter 0.8 ⁇ m) are supplied so as to be 50% by weight to form chips, and a white pigment master batch (WMB1) is obtained. Obtained.
- the polyester (6) is subjected to a twin screw extruder with a vent, and a titanium oxide (particle size: 0.3 ⁇ m) having an anatase crystal form of 50% by weight is supplied to make a chip, and a white pigment master batch (WMB3) was obtained.
- the coating composition of the coating layer is shown in Table 2 below. In addition, all the addition amount of Table 2 represents solid content weight%.
- the coating agent used is as shown below.
- U-1 polyurethane water dispersion which is a polyurethane (the counter ion of carboxylic acid is ammonia) made of polytetramethylene glycol having a number average molecular weight of about 1000, dimethylolpropionic acid and isophorone diisocyanate
- U-2 A water dispersion which is a polyurethane composed of a polycarbonate polyol of hexamethylene diol (number average molecular weight of about 1000), dimethylolpropionic acid and hydrogenated diphenylmethane-4,4′-diisocyanate (the counter ion of carboxylic acid is triethylamine).
- U-3 DIC Corporation trade name Hydran (registered trademark) AP-40F, which is an aqueous polyester polyurethane dispersion of aromatic polyester and aliphatic diisocyanate.
- E-1 Aqueous dispersion of aromatic polyester, DIC Corporation Trade name Finetech (registered trademark) ES-670
- Oxazoline-based water-soluble resin crosslinking agent Nippon Shokubai Co., Ltd. Trade name Epocross (registered trademark) WS-500
- X-3 Water-soluble epoxy-based cross-linking agent Nagase ChemteX Corporation Brand name Denacol (registered trademark) EX-521 D-1: Silica fine particle aqueous dispersion (average particle diameter 60 nm)
- Example 1 The polyester obtained by mixing the polyester (2) and the polyester (4) in a weight ratio of 70:30 is used as the raw material for the polyester A layer, and the weight of the polyester (2) and the white pigment masterbatch 1 (WMB1) is 70:30.
- the polyester mixed in the ratio was used as the raw material for the polyester B layer.
- the longest residence time in this melt extrusion was 12 minutes.
- the obtained sheet was stretched 3.6 times in the longitudinal direction at 85 ° C. by a roll stretching method.
- the coating agent 1 shown in Table 2 was applied to the treated surface with a bar coater, and the coating amount on the final film was 0.02 g. It was adjusted to / m 2.
- the film was guided to a tenter, dried at 100 ° C., stretched 3.9 times in the transverse direction at 110 ° C., further heat-treated at 220 ° C., and then shrunk 4% in the width direction at 200 ° C.
- the thickness of the obtained film was 50 ⁇ m.
- the properties and evaluation results of this film are shown in Table 3.
- WMB2 white pigment masterbatch 2
- the longest residence time in this melt extrusion was 14 minutes.
- the obtained sheet was stretched 3.6 times in the longitudinal direction at 85 ° C. by a roll stretching method.
- the coating agent 1 shown in Table 2 was applied to the treated surface with a bar coater, and the coating amount on the final film was 0.02 g. It was adjusted to / m 2.
- the film was guided to a tenter, dried at 100 ° C., stretched 3.9 times in the transverse direction at 110 ° C., further heat-treated at 220 ° C., and then shrunk 4% in the width direction at 200 ° C.
- the thickness of the obtained film was 50 ⁇ m.
- the properties and evaluation results of this film are shown in Table 3.
- Example 3 In Example 2, except that polyester (2), polyester (4), and white pigment masterbatch 2 (WMB2) mixed in a weight ratio of 56:30:14 were changed to a polyester A layer raw material in Example 2. A film having a thickness of 50 ⁇ m was obtained in the same manner as in Example 2. The longest residence time in this melt extrusion was 14 minutes. The properties and evaluation results of this film are shown in Table 3.
- Example 4 In Example 2, polyester obtained by mixing polyester (2), polyester (4), and white pigment masterbatch 2 (WMB2) in a weight ratio of 60:30:10 was used as a raw material for the polyester A layer. Further, polyester obtained by mixing polyester (2) and white pigment masterbatch 2 (WMB2) at a weight ratio of 70:30 was used as a raw material for the polyester B layer. Other than that, the longest residence time in this melt extrusion, in which a film having a thickness of 50 ⁇ m was obtained in the same manner as in Example 2, was 14 minutes. The properties and evaluation results of this film are shown in Table 3.
- Example 2 a film having a thickness of 50 ⁇ m was obtained in the same manner as in Example 1 except that the surface on which the corona discharge treatment and the coating liquid 1 were applied was changed to the polyester B surface. The longest residence time in this melt extrusion was 12 minutes. The properties and evaluation results of this film are shown in Table 4 below.
- Example 2 polyester (2) and white pigment masterbatch 2 (WMB2) were mixed at a weight ratio of 70:30 as a raw material, and polyester (2) and white pigment masterbatch 2 ( A film having a thickness of 50 ⁇ m was obtained in the same manner as in Example 2 except that the polyester mixed with WMB2) at a weight ratio of 86:14 was changed to the raw material for the polyester B layer. The longest residence time in this melt extrusion was 14 minutes. Table 4 shows the properties and evaluation results of this film.
- Comparative Example 3 In Example 2, the raw material was polyester (2), polyester (4), and white pigment masterbatch 2 (WMB2) mixed in a weight ratio of 50:30:20 except that polyester was changed to a raw material for the polyester A layer. A film having a thickness of 50 ⁇ m was obtained in the same manner as in Example 2. The longest residence time in this melt extrusion was 14 minutes. Table 4 shows the properties and evaluation results of this film.
- Example 3 a film was obtained in the same manner as in Example 3, except that the coating agent used in the coating layer was changed to coating agent 2 to coating agent 10 shown in Table 2. The properties and evaluation results of this film are shown in Tables 5 and 6 below. In the film lamination structures in Tables 3 to 6, “coating” means any coating layer.
- the film of the present invention can be suitably used for, for example, a solar cell back surface protective material.
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Abstract
Description
・ポリエステルA層:芳香族ポリエステルを主構成成分として、白色顔料の含有量が8重量%未満であるポリエステルからなる層
・ポリエステルB層:芳香族ポリエステルを主構成成分として、白色顔料の含有量が8重量%以上であるポリエステルからなる層
a)の具体的な例としては、一軸押出機を使用する場合は、原料をあらかじめ水分量が50ppm以下、好ましくは30ppm以下になるように十分乾燥すること、二軸押出機を使用する場合は、ベント口を設け、40ヘクトパスカル以下、好ましくは30ヘクトパスカル以下、さらに好ましくは20ヘクトパスカル以下の減圧を維持すること等の方法を採用することができる。
b)の具体的な例としては、押出機への原料投入から溶融シートが口金から吐出し始めるまでの滞留時間として、20分以下、さらには15分以下とすることが好ましい。
いわゆる滴定法によって、末端カルボン酸の量を測定した。すなわちポリエステルをベンジルアルコールに溶解し、フェノールレッド指示薬を加え、水酸化ナトリウムの水/メタノール/ベンジルアルコール溶液で滴定した。フィルムに塗布層が設けてある場合には、この影響を無くすため、研磨剤入りクレンザーを使って塗布層を水で洗い流してから、イオン交換水で十分にすすいで乾燥した後、同様に測定を行った。また、ポリエステルフィルム中に二酸化チタンや硫酸バリウム等の白色顔料が含まれている場合は、ベンジルアルコールに対する不溶成分である白色顔料を、遠心沈降法により取り除いたものに対し適定することで、ポリエステル成分に対する末端カルボキシル基量(当量/トン)を求めた。
蛍光X線分析装置(株式会社島津製作所製 型式「XRF-1500」)を用いて、下記表1に示す条件下で、フィルム中の元素量を求めた。積層フィルムの場合はフィルムを溶融してディスク状に成型して測定することにより、フィルム全体に対する含有量を測定した。また、フィルムに塗布層が設けてある場合には、この影響を無くすため、研磨剤入りクレンザーを使って塗布層を水で洗い流してから、イオン交換水で十分にすすいで乾燥した後、同様に測定を行った。なお、この方法での検出限界は、通常1ppm程度である。
測定試料1gを精秤し、フェノール/テトラクロロエタン=50/50(重量部)の溶媒に溶解させて濃度c=0.01g/cm3の溶液を調製し、30℃にて溶媒との相対粘度ηrを測定し、極限粘度[η]を求めた。
平山製作所製 パーソナルプレッシャークッカーPC-242HS-Eを用いて、120℃、100%RHの雰囲気にてフィルムを35時間処理した。次いで、23℃、50%RHの雰囲気にて24時間調温・調湿した後、フィルムの機械的特性として、製膜方向(MD方向)の破断伸度を測定した。測定には株式会社島津製作所製 万能試験機AUTOGRAPHを使用し、幅15mmのサンプルで、チャック間50mmとして、引張り速度200mm/分の条件で行った。処理前後での破断伸度の保持率(%)を下記の式(1)にて算出し、下記の基準で判断した。
破断伸度保持率=処理後の破断伸度÷処理前の破断伸度×100 …(1)
◎:保持率が80%以上
○:保持率が60~80%未満
△:保持率が30~60%未満
×:保持率が30%未満
長手方向がMD方向となるように、長さ300mm、幅25mmのポリエステルフィルムの小片を2本切り取った。一方で長さ50mm、幅25mmであるEVAフィルムの1本の小片を切り取り、2本のポリエステルフィルムの小片の塗布層面でEVAフィルムを挟むように重ねた。これをヒートシール装置(テスター産業株式会社製 TP-701)を用いてラミネートした。使用したEVAフィルムは、ドイツ Etimex社製 485.00(標準硬化タイプ、厚み0.5mm)で、ヒートシール条件は、温度150℃、圧力0.13MPaで、20分間の条件を用いた。EVAとの接着強度を測定するため、まず25mmの幅のポリエステルフィルム/EVAフィルムラミネート小片から、長さ300mm、幅15mmのサンプルを切り取る。この15mm幅のポリエステルフィルムの小片のラミネートされていない端部を、引張/曲げ試験機(株式会社島津製作所製 EZGraph)の中に取り付ける。引き続き、角度180°、速度100mm/分でこのポリエステルフィルム/EVAフィルムラミネートを分離するために必要な力(接着強度)を10個の試料について測定して、その平均値を下記のように分類にした。
◎:接着強度が50N/15mm幅以上
○:接着強度が30N/15mm幅~50N/15mm幅未満
△:接着強度が10N/15mm幅~30N/15mm幅未満
×:接着強度が10N/15mm幅未満
上記(5)で作成したポリエステルフィルム/EVAフィルムラミネートの25mm幅の試験片を用いて、上記(4)と同様に120℃、100%RHの雰囲気にて35時間の湿熱処理を行った。次いで、23℃、50%RHの雰囲気にて24時間調温・調湿した後、サンプルから15mm幅の測定サンプルを切り取り、上記(5)と同様に、ポリエステルフィルム/EVAフィルムラミネートを分離するために必要な力(接着強度)の平均値を求めた。この値と、湿熱処理を行う前の接着強度から、接着強度保持率を次式にて算出し、下記の基準で判断した。
接着強度保持率(%)=(湿熱処理後の接着強度)/(湿熱処理前の接着強度)
◎:保持率が70%以上
○:保持率が50~70%未満
△:保持率が50%未満
×:ポリエステルフィルム自体の劣化が著しく、破れや損傷が発生する
・評価用PVBシートの作成:
粉末状のPVB(分子量約11万、ブチラール化度65モル%、水酸基量約34モル%)6重量部、トリ(エチレングリコール)-ビス-2-エチルヘキサノエート(可塑剤)4重量部を45重量部のトルエンと混合し膨潤させた後、45重量部のエタノールを加え溶解させた。この溶液をテフロン(登録商標)製のシャーレに入れ、熱風オーブンにて100℃、1時間乾燥して厚さ約0.4mmのPVBシートを作成した。
・接着性評価:
上記PVBシートを幅1cm、長さ10cmに切り出し、2枚の供試フィルムで易接着面が該シートに向くように挟み、ヒートシールテスター(テスター産業株式会社製 TP-701)で熱圧着する。条件は以下のとおりである。
圧力:0.13MPa
温度:140℃
時間:3分
一昼夜の放冷後、圧着部分を手で剥離し下記の基準により接着性を判定した。
○:接着強度が良好(供試フィルムまたはPVBシートが損傷するまたは接着界面で剥離するが強い力がいる)
△:接着強度が普通(接着界面で剥離するが軽い手応えがある)
×:接着強度が不良(接着界面でほとんど手応えがなく、簡単に剥離する)
××:ポリエステルフィルム自体の劣化が著しく、破れや損傷が発生する
上記(7)で作成した接着性評価試験サンプルを、ESPEC株式会社製 恒温恒湿槽PR-2KPを用いて、85℃、85%RHの雰囲気にて500時間湿熱処理を行った。このサンプルを恒温恒湿槽から取り出した後、一昼夜放冷してから、(7)と同様に接着性の評価を行った。
<ポリエステル(1)の製造法>
テレフタル酸ジメチル100重量部とエチレングリコール60重量部とを出発原料とし、触媒として酢酸マグネシウム・四水塩0.09重量部を反応器にとり、反応開始温度を150℃とし、メタノールの留去とともに徐々に反応温度を上昇させ、3時間後に230℃とした。4時間後、実質的にエステル交換反応を終了させた。この反応混合物に三酸化アンチモン0.04重量部を加えて、4時間重縮合反応を行った。すなわち、温度を230℃から徐々に昇温し280℃とした。一方、圧力は常圧より徐々に減じ、最終的には40パスカルとした。反応開始後、反応槽の攪拌動力の変化により、極限粘度0.61に相当する時点で反応を停止し、窒素加圧下ポリマーを吐出させた。得られたポリエステル(1)の極限粘度は0.61、ポリマーの末端カルボン酸量は32当量/トンであった。
ポリエステル(1)を出発原料とし、真空下220℃にて固相重合を行ってポリエステル(2)を得た。ポリエステル(2)の極限粘度は0.81、ポリマーの末端カルボン酸量は8当量/トンであった。
ポリエステル(1)の製造において、エステル交換反応後に、エチレングリコールに分散させた平均粒子径2.6μmのシリカ粒子0.1重量部を加えた以外は同様の方法で、ポリエステル(3)を得た。得られたポリエステル(3)の極限粘度は0.61、ポリマーの末端カルボン酸量は28当量/トンであった。
ポリエステル(3)を出発原料とし、真空下220℃にて固相重合を行ってポリエステル(4)を得た。ポリエステル(4)の極限粘度は0.73、ポリマーの末端カルボン酸量は10当量/トンであった。
ポリエステル(1)の製造において、エステル交換反応後に正リン酸0.047重量部(リン元素として0.015部)を添加した後、三酸化アンチモン0.04重量部を加えた以外は同様の方法で、ポリエステル(5)を得た。得られたポリエステル(5)の極限粘度は0.61、ポリマーの末端カルボン酸量は29当量/トンであった。
ポリエステル(5)を出発原料とし、真空下220℃にて固相重合を行ってポリエステル(6)を得た。ポリエステル(6)の極限粘度は0.73、ポリマーの末端カルボン酸量は10当量/トンであった。
上記ポリエステル(2)をベント付き二軸押出機に供して、硫酸バリウム粒子(粒子径0.8μm)を50重量%となるように供給してチップ化を行い、白色顔料マスターバッチ(WMB1)を得た。
上記ポリエステル(2)をベント付き二軸押出機に供して、結晶型がアナターゼの酸化チタン(粒子径0.3μm)を50重量%となるように供給してチップ化を行い、白色顔料マスターバッチ(WMB2)を得た。
上記ポリエステル(6)をベント付き二軸押出機に供して、結晶型がアナターゼの酸化チタン(粒子径0.3μm)を50重量%となるように供給してチップ化を行い、白色顔料マスターバッチ(WMB3)を得た。
塗布層の塗布剤配合は下記表2に示す。なお、表2中の添加量は、全て固形分重量%を表す。用いた塗布剤は下記に示すとおりである。
・D-1:シリカ微粒子水分散体(平均粒子径60nm)
上記のポリエステル(2)およびポリエステル(4)を70:30の重量比で混合したポリエステルをポリエステルA層用原料とし、さらにポリエステル(2)と白色顔料マスターバッチ1(WMB1)を70:30の重量比で混合したポリエステルをポリエステルB層用原料とした。これらの各原料を別々に二台のベント付き二軸押出機に投入して、290℃で溶融押出し、A/B=2/3の層構成比になるようにマルチマニホールドダイで合流積層させた後、静電印加密着法を用いて表面温度を40℃に設定したキャスティングドラム上で急冷固化させて未延伸シートを得た。この溶融押出での最も長い滞留時間は12分であった。得られたシートをロール延伸法により、縦方向に85℃で3.6倍延伸した。ここで、ポリエステルA層表面にコロナ放電処理を施した後、その処理面に、上記表2に示した塗布剤1をバーコーターで塗布し、最終的なフィルムでの塗工量が0.02g/m2となるように調整した。この後テンターに導き、100℃で乾燥した後、110℃で横方向に3.9倍延伸し、さらに220℃で熱処理を行った後、200℃で幅方向に4%縮めた。得られたフィルムの厚さは50μmであった。このフィルムの特性および評価結果を表3に示す。
実施例1において、原料をポリエステル(2)およびポリエステル(4)を70:30の重量比で混合したポリエステルをポリエステルA層用原料として、さらにポリエステル(2)と白色顔料マスターバッチ2(WMB2)を70:30の重量比で混合したポリエステルをポリエステルB層用原料とした。これらの各原料を別々に二台のベント付き二軸押出機に投入して、290℃で溶融押出し、A/B/A=3/44/3の層構成比になるようにマルチマニホールドダイで合流積層させた後、静電印加密着法を用いて表面温度を40℃に設定したキャスティングドラム上で急冷固化させて未延伸シートを得た。この溶融押出での最も長い滞留時間は14分であった。得られたシートをロール延伸法により、縦方向に85℃で3.6倍延伸した。ここで、ポリエステルA層表面にコロナ放電処理を施した後、その処理面に、上記表2に示した塗布剤1をバーコーターで塗布し、最終的なフィルムでの塗工量が0.02g/m2となるように調整した。この後テンターに導き、100℃で乾燥した後、110℃で横方向に3.9倍延伸し、さらに220℃で熱処理を行った後、200℃で幅方向に4%縮めた。得られたフィルムの厚さは50μmのであった。このフィルムの特性および評価結果を表3に示す。
実施例2において、原料をポリエステル(2)、ポリエステル(4)、および白色顔料マスターバッチ2(WMB2)を56:30:14の重量比で混合したポリエステルをポリエステルA層用原料に変更した以外は、実施例2と全く同様の方法で厚さ50μmのフィルムを得た。この溶融押出での最も長い滞留時間は14分であった。このフィルムの特性および評価結果を表3に示す。
実施例2において、原料をポリエステル(2)、ポリエステル(4)、および白色顔料マスターバッチ2(WMB2)を60:30:10の重量比で混合したポリエステルをポリエステルA層用原料とした。さらにポリエステル(2)および白色顔料マスターバッチ2(WMB2)を70:30の重量比で混合したポリエステルをポリエステルB層用原料とした。それ以外は、実施例2と全く同様の方法で厚さ50μmのフィルムを得たこの溶融押出での最も長い滞留時間は14分であった。このフィルムの特性および評価結果を表3に示す。
実施例2において、原料をポリエステル(6)およびポリエステル(4)を70:30の重量比で混合したポリエステルをポリエステルA層用原料とし、更にポリエステル(2)と白色顔料マスターバッチ3(WMB3)を50:50の重量比で混合したポリエステルをポリエステルB層用原料とした。ポリエステルA層とポリエステルB層の層構成比をA/B/A=15/20/15となるように変更した以外は、実施例2と全く同様の方法で厚さ50μmのフィルムを得た。この溶融押出での最も長い滞留時間は14分であった。このフィルムの特性および評価結果を表3に示す。
実施例2において、コロナ放電処理および塗布液1を塗布する面をポリエステルB面に変更した以外は、実施例1と全く同様の方法で厚さ50μmのフィルムを得た。この溶融押出での最も長い滞留時間は、12分であった。このフィルムの特性および評価結果を下記表4に示す。
実施例2において、原料をポリエステル(2)と白色顔料マスターバッチ2(WMB2)を70:30の重量比で混合したポリエステルをポリエステルA層用原料とし、ポリエステル(2)と白色顔料マスターバッチ2(WMB2)を86:14の重量比で混合したポリエステルをポリエステルB層用原料と変更した以外は、実施例2と全く同様の方法で厚さ50μmのフィルムを得た。この溶融押出での最も長い滞留時間は14分であった。このフィルムの特性および評価結果を表4に示す。
実施例2において、原料をポリエステル(2)、ポリエステル(4)、および白色顔料マスターバッチ2(WMB2)を50:30:20の重量比で混合したポリエステルをポリエステルA層用原料に変更した以外は、実施例2と全く同様の方法で厚さ50μmのフィルムを得た。この溶融押出での最も長い滞留時間は14分であった。このフィルムの特性および評価結果を表4に示す。
実施例3において、同じポリエステル原料を用いて溶融押出しをして、A/B/A=3/44/3の層構成比の未延伸フィルムを得たが、この際に吐出量を下げて行い、溶融押出での最も長い滞留時間は23分とした。その後は実施例3と全く同様の方法により、厚さ50μmのフィルムを得た。このフィルムの特性および評価結果を表4に示す。
実施例3において、塗布層に用いる塗布剤を、表2に記載の塗布剤2~塗布剤10に変更する以外は、実施例3と全く同様の方法でフィルムを得た。このフィルムの特性および評価結果を下記表5および6に示す。なお、表3~6中のフィルム積層構成に「塗」とあるのは、いずれも塗布層を意味する。
Claims (5)
- 少なくとも一方の最外層に下記ポリエステルA層を有し、下記ポリエステルB層を少なくとも一層含む積層ポリエステルフィルムあり、当該積層ポリエステルフィルムの末端カルボキシル基量が26当量/トン以下であり、前記ポリエステルA層の少なくとも一方の表面に、ポリカーボネート骨格またはポリエーテル骨格の少なくとも一種を有するポリウレタンと、架橋剤とから形成された塗布層を有することを特徴とする太陽電池裏面保護材用ポリエステルフィルム。
・ポリエステルA層:芳香族ポリエステルを主構成成分として、白色顔料の含有量が8重量%未満であるポリエステルからなる層
・ポリエステルB層:芳香族ポリエステルを主構成成分として、白色顔料の含有量が8重量%以上であるポリエステルからなる層 - 架橋剤/ポリウレタン(重量比)が10/90~90/10である請求項1に記載の太陽電池裏面保護材用ポリエステルフィルム。
- 架橋剤がオキサゾリン系ポリマーまたはカルボジイミド系ポリマーの少なくとも一種である請求項1に記載の太陽電池裏面保護材用ポリエステルフィルム。
- 少なくとも一つの塗布層上にエチレン-酢酸ビニル共重合体樹脂層を積層した請求項1~3の何れかに記載の太陽電池裏面保護材用ポリエステルフィルム。
- 少なくとも一つの塗布層上にポリビニルブチラール樹脂層を積層した請求項1~3の何れかに記載の太陽電池裏面保護材用ポリエステルフィルム。
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- 2011-04-05 WO PCT/JP2011/058641 patent/WO2011135985A1/ja active Application Filing
- 2011-04-05 EP EP11774769.1A patent/EP2565936B1/en active Active
- 2011-04-05 KR KR1020127028188A patent/KR101765483B1/ko active IP Right Grant
- 2011-04-05 US US13/643,155 patent/US20130065063A1/en not_active Abandoned
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Cited By (5)
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EP2335924A1 (en) * | 2008-10-06 | 2011-06-22 | Mitsubishi Plastics, Inc. | Multilayer polyester film |
EP2335924A4 (en) * | 2008-10-06 | 2013-03-06 | Mitsubishi Plastics Inc | MULTILAYER POLYESTER FILM |
US20150068601A1 (en) * | 2012-03-14 | 2015-03-12 | Toyobo Co., Ltd. | Sealing sheet for back surface of solar cell, and solar cell module |
US10896987B2 (en) * | 2012-03-14 | 2021-01-19 | Toyobo Co., Ltd. | Sealing sheet for back surface of solar cell, and solar cell module |
CN115536995A (zh) * | 2022-10-11 | 2022-12-30 | 苏州易昇光学材料股份有限公司 | 一种光伏背板用pet膜及其制备方法 |
Also Published As
Publication number | Publication date |
---|---|
CN102859716B (zh) | 2016-08-24 |
US20130065063A1 (en) | 2013-03-14 |
JP2011249756A (ja) | 2011-12-08 |
KR101765483B1 (ko) | 2017-08-08 |
EP2565936A1 (en) | 2013-03-06 |
EP2565936A4 (en) | 2014-06-11 |
JP5615130B2 (ja) | 2014-10-29 |
CN102859716A (zh) | 2013-01-02 |
KR20130097061A (ko) | 2013-09-02 |
EP2565936B1 (en) | 2017-03-29 |
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