WO2017061545A1 - ポリビニルアセタール樹脂組成物、接着シート、タッチパネル用層間充填材料及び積層体 - Google Patents
ポリビニルアセタール樹脂組成物、接着シート、タッチパネル用層間充填材料及び積層体 Download PDFInfo
- Publication number
- WO2017061545A1 WO2017061545A1 PCT/JP2016/079799 JP2016079799W WO2017061545A1 WO 2017061545 A1 WO2017061545 A1 WO 2017061545A1 JP 2016079799 W JP2016079799 W JP 2016079799W WO 2017061545 A1 WO2017061545 A1 WO 2017061545A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- touch panel
- polyvinyl acetal
- filling material
- resin composition
- interlayer
- Prior art date
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- 238000011049 filling Methods 0.000 title claims abstract description 126
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 title abstract 5
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims abstract description 117
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- AMIMRNSIRUDHCM-UHFFFAOYSA-N Isopropylaldehyde Chemical compound CC(C)C=O AMIMRNSIRUDHCM-UHFFFAOYSA-N 0.000 description 2
- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 description 2
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Images
Classifications
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- C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
- C08F261/12—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated acetals or ketals
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- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10761—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing vinyl acetal
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- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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- C08F16/38—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an acetal or ketal radical
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
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- 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
- C09J129/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Adhesives based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Adhesives based on derivatives of such polymers
- C09J129/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
-
- 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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
-
- 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
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
-
- 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
- C09J7/29—Laminated material
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
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- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1339—Gaskets; Spacers; Sealing of cells
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- G06F3/00—Input arrangements for transferring data to be processed into a form capable of being handled by the computer; Output arrangements for transferring data from processing unit to output unit, e.g. interface arrangements
- G06F3/01—Input arrangements or combined input and output arrangements for interaction between user and computer
- G06F3/03—Arrangements for converting the position or the displacement of a member into a coded form
- G06F3/041—Digitisers, e.g. for touch screens or touch pads, characterised by the transducing means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2457/00—Electrical equipment
- B32B2457/20—Displays, e.g. liquid crystal displays, plasma displays
- B32B2457/208—Touch screens
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- G06F2203/00—Indexing scheme relating to G06F3/00 - G06F3/048
- G06F2203/041—Indexing scheme relating to G06F3/041 - G06F3/045
- G06F2203/04103—Manufacturing, i.e. details related to manufacturing processes specially suited for touch sensitive devices
Definitions
- the present invention provides a polyvinyl acetal resin composition that is excellent in thermal stability and can be molded by an extrusion method and can exhibit a high storage elastic modulus even at high temperatures, an adhesive sheet comprising the polyvinyl acetal resin composition, and the polyvinyl acetal
- the present invention relates to an interlayer filling material for a touch panel made of a resin composition, and a laminate manufactured using the interlayer filling material for a touch panel.
- Polyvinyl acetal is widely used for applications such as paints, wash primers, binders for ceramics, interlayer films for laminated glass, etc. because of its excellent toughness, adhesion to inorganic materials, and solubility in organic solvents. ing.
- polyvinyl acetal has a high storage elastic modulus at a room temperature of about 20 ° C., there is a problem that the storage elastic modulus is greatly reduced at a high temperature.
- Patent Document 1 discloses a polymer film obtained by forming a polymer solution comprising a polyvinyl acetal, a cross-linking agent, and an organic solvent into a film shape by a solvent casting method, and the organic solvent in the polymer solution.
- a polymer film obtained by crosslinking a polyvinyl acetal to a crosslinking degree of 1 to 60% in the step of volatilizing and / or the step after obtaining the polymer film is described.
- polyvinyl acetal is crosslinked using boric acid or the like as a crosslinking agent.
- a polymer film made of crosslinked polyvinyl acetal can exhibit a high storage elastic modulus even at high temperatures.
- the present invention is a polyvinyl acetal resin composition that is excellent in thermal stability, can be molded by an extrusion method, and can exhibit a high storage elastic modulus even at high temperatures, and an adhesive comprising the polyvinyl acetal resin composition It aims at providing the laminated body manufactured using the sheet
- the present invention is a polyvinyl acetal resin composition containing a polyvinyl acetal, a radical photopolymerization initiator, and a monomer or oligomer having a radical polymerizable double bond.
- the present invention is described in detail below.
- a polyvinyl acetal resin composition containing a polyvinyl acetal, a radical photopolymerization initiator, and a monomer or oligomer having a radical polymerizable double bond can be obtained even at a high temperature during extrusion molding. While not reacting or gelling, it was found that it can be cross-linked by irradiating light after molding, and can exhibit a high storage elastic modulus even at high temperature, and the present invention has been completed.
- Photo radical polymerization initiators are highly stable even at high temperatures and are not activated at the normal extrusion temperature (about 100 to 220 ° C.) of polyvinyl acetal.
- the photo radical polymerization initiator is irradiated with light, it is activated to generate radicals, which pulls C—H hydrogen in the polyvinyl acetal and crosslinks via monomers or oligomers having radical polymerizable double bonds. Therefore, it was considered that high storage stability can be exhibited even at high temperatures.
- the polyvinyl acetal resin composition of the present invention contains a polyvinyl acetal, a radical photopolymerization initiator, and a monomer or oligomer having a radical polymerizable double bond.
- the polyvinyl acetal can be prepared, for example, by acetalizing polyvinyl alcohol obtained by saponifying polyvinyl acetate with an aldehyde in the presence of a catalyst.
- the saponification degree of the polyvinyl alcohol is not particularly limited, but is generally in the range of 70 to 99.9 mol%, preferably 70 to 99.8 mol%, more preferably 80 to 99.8 mol%.
- the average degree of polymerization of the polyvinyl alcohol is not particularly limited, but polyvinyl acetal having a high molecular weight is preferable from the viewpoint of exhibiting more excellent performance. Therefore, it is preferable to use polyvinyl alcohol having a high average degree of polymerization.
- the preferable lower limit of the average degree of polymerization of the polyvinyl alcohol is 200, and the preferable upper limit is 4000.
- the average degree of polymerization of the polyvinyl alcohol is within this range, the reaction when acetalizing the polyvinyl alcohol is easy, and the obtained polyvinyl acetal can exhibit high mechanical strength. Moreover, when using the polyvinyl acetal resin composition of this invention for the interlayer filling material for touch panels mentioned later, when a portable information terminal is damaged, scattering of fragments can be suppressed.
- the more preferable lower limit of the average degree of polymerization of the polyvinyl alcohol is 600, the more preferable upper limit is 3800, the still more preferable lower limit is 800, and the still more preferable upper limit is 3600.
- the average degree of polymerization of polyvinyl alcohol means the viscosity average degree of polymerization calculated
- the polyvinyl alcohol resin When two or more kinds of polyvinyl alcohol resins are mixed and used as the polyvinyl alcohol resin, it means the apparent viscosity average polymerization degree of the whole polyvinyl alcohol resin after mixing.
- a solution containing the polyvinyl alcohol may be used.
- a solvent used for the solution containing the said polyvinyl alcohol water etc. are mentioned, for example.
- the aldehyde is not particularly limited, but in general, an aldehyde having 1 to 10 carbon atoms is preferably used.
- the aldehyde having 1 to 10 carbon atoms is not particularly limited, and may be a linear aldehyde or a branched aldehyde such as n-butyraldehyde, isobutyraldehyde, n- Examples include valeraldehyde, 2-ethylbutyraldehyde, n-hexylaldehyde, n-octylaldehyde, n-nonylaldehyde, n-decylaldehyde, formaldehyde, acetaldehyde, benzaldehyde and the like.
- aldehydes may be used alone or in combination of two or more.
- n-butyraldehyde, n-hexylaldehyde, and n-valeraldehyde are preferable, and n-butyraldehyde is more preferable.
- the polyvinyl acetal is preferably polyvinyl butyral (when the aldehyde is n-butyraldehyde, the polyvinyl acetal is referred to as polyvinyl butyral).
- the polyvinyl butyral exhibits an appropriate adhesion to glass or the like, and is excellent in light resistance, weather resistance, and the like. Moreover, you may use together 2 or more types of polyvinyl acetal as needed.
- the polyvinyl acetal resin composition of the present invention is used for an interlayer filling material for a touch panel described later
- the polyvinyl acetal is a molecule before being cross-linked by light irradiation because of excellent step following ability and defoaming property. It is preferable that there is little intercrosslinking. If the intermolecular crosslinking of the polyvinyl acetal is small, it is possible to obtain an interlayer filling material for a touch panel that is more excellent in step following ability even if the molecular weight, acetyl group amount, degree of acetalization, etc. of the polyvinyl acetal are the same.
- the molecular weight of the polyvinyl acetal is large, more excellent anti-scattering properties can be obtained.
- As a method for obtaining such a polyvinyl acetal with little intermolecular crosslinking for example, so as not to crosslink the main chain of the adjacent polyvinyl alcohol, so as not to excessively add the aldehyde before or during the acetalization reaction with the aldehyde. Is preferred. When the aldehyde is added in excess of the amount required for acetalization, the degree of crosslinking increases.
- the polyvinyl acetal has a preferable lower limit of the hydroxyl group content (hydroxyl group amount) of 16 mol% and a preferable upper limit of 45 mol%.
- the amount of hydroxyl groups in the polyvinyl acetal is within this range, the adhesive strength to glass and the like is excellent, the compatibility with the plasticizer described later is excellent, high flexibility is exhibited, and the handleability is improved.
- the polyvinyl acetal resin composition of the present invention is used for an interlayer filling material for a touch panel, which will be described later, the adhesion of the interlayer filling material for the touch panel to the glass is improved, and the step following property of the interlayer filling material for the touch panel is also improved. To do.
- the more preferable lower limit of the hydroxyl group amount of the polyvinyl acetal is 18 mol%, the more preferable upper limit is 40 mol%, the still more preferable lower limit is 20 mol%, and the still more preferable upper limit is 38 mol%. Further, when the polyvinyl acetal resin composition of the present invention is used for an interlayer filling material for a touch panel described later, a more preferable lower limit of the hydroxyl group content is 18 mol%, a further preferable lower limit is 20 mol%, and a particularly preferable lower limit is 22 mol.
- the upper limit is 40 mol%, the more preferable upper limit is 38 mol%, the still more preferable upper limit is 36 mol%, and the particularly preferable upper limit is 35 mol%.
- the hydroxyl group amount of polyvinyl acetal is the value which expressed the mole fraction calculated
- the amount of ethylene group to which the hydroxyl group is bonded can be determined, for example, by a method based on JIS K6728 “Testing method for polyvinyl butyral”.
- the polyvinyl acetal has a preferable lower limit of 0.1 mol% and a preferable upper limit of 30 mol% of the degree of acetylation (acetyl group amount).
- acetyl group amount the degree of acetylation
- the amount of acetyl groups in the polyvinyl acetal is within this range, the moisture resistance is excellent, the compatibility with the plasticizer is excellent, high flexibility is exhibited, and the handleability is improved.
- the reaction efficiency at the time of manufacturing the said polyvinyl acetal can also be made high.
- the adhesion of the interlayer filling material for the touch panel to the glass is improved, and the step following property of the interlayer filling material for the touch panel is also improved.
- the more preferred lower limit of the amount of acetyl groups of the polyvinyl acetal is 0.2 mol%, the more preferred upper limit is 24 mol%, the still more preferred lower limit is 0.3 mol%, and the still more preferred upper limit is 20 mol%, particularly preferred.
- the upper limit is 19.5 mol%, and the most preferred upper limit is 15 mol%.
- the amount of acetyl groups in polyvinyl acetal is the value obtained by subtracting the amount of ethylene groups to which acetal groups are bonded and the amount of ethylene groups to which hydroxyl groups are bonded from the total amount of ethylene groups in the main chain. This is a value expressed as a percentage (mol%) of the mole fraction obtained by dividing by the total amount of ethylene groups.
- the amount of ethylene group to which the acetal group is bonded can be measured, for example, according to JIS K6728 “Testing method for polyvinyl butyral”.
- Examples of the method for adjusting the degree of acetylation of the polyvinyl acetal within the above range include a method for adjusting the degree of saponification of the polyvinyl alcohol. That is, the amount of acetyl groups in the polyvinyl acetal depends on the degree of saponification of the polyvinyl alcohol. If polyvinyl alcohol having a low saponification degree is used, the amount of acetyl groups in the polyvinyl acetal increases and the degree of saponification is high. The amount of acetyl groups in the polyvinyl acetal is reduced.
- the polyvinyl acetal has a preferable lower limit of the degree of acetalization of 50 mol% and a preferable upper limit of 85 mol%.
- the degree of acetalization of the polyvinyl acetal is within this range, the reaction time required for producing the polyvinyl acetal can be shortened, it is excellent in compatibility with the plasticizer, exhibits high flexibility and is easy to handle. improves.
- the more preferable lower limit of the degree of acetalization is 54 mol%, the more preferable upper limit is 82 mol%, the further preferable lower limit is 58 mol%, the still more preferable upper limit is 79 mol%, and the particularly preferable upper limit is 77 mol%. .
- the degree of acetalization of polyvinyl acetal is a value obtained by dividing the amount of ethylene groups to which the acetal group is bonded by the total amount of ethylene groups in the main chain, as a percentage (mol%). .
- the degree of acetalization is determined by measuring the amount of acetyl groups and the amount of vinyl alcohol (hydroxyl content) by a method based on JIS K6728 “Testing methods for polyvinyl butyral”, and calculating the molar fraction from the obtained measurement results. Subsequently, it can be calculated by subtracting the amount of acetyl groups and the amount of vinyl alcohol from 100 mol%.
- a method for adjusting the degree of acetalization of the polyvinyl acetal within the above range for example, a method for adjusting the amount of the aldehyde added. If the addition amount of the aldehyde is decreased, the degree of acetalization of the polyvinyl acetal is lowered, and if the addition amount of the aldehyde is increased, the degree of acetalization of the polyvinyl acetal is increased.
- the photo radical polymerization initiator is activated by irradiation with light to generate an active radical, and examples thereof include an intramolecular cleavage type, a hydrogen abstraction type, and an electron transfer type.
- hydrogen extraction is possible because it is highly stable at high temperatures, is not activated at the normal extrusion temperature of polyvinyl acetal (about 130-220 ° C), and the polyvinyl acetal resin composition can be easily molded by the extrusion method.
- Type radical polymerization initiators are preferred.
- the hydrogen abstraction type photo radical polymerization initiator include benzophenone, thioxanthone, Michler's ketone, and the like. These radical photopolymerization initiators may be used alone or in combination of two or more. Among them, benzophenone is preferable because it is excellent in activity during light irradiation, particularly excellent in stability at high temperatures, and hardly activated at the extrusion temperature of polyvinyl acetal.
- content of the said radical photopolymerization initiator is not specifically limited,
- the preferable minimum with respect to 100 weight part of said polyvinyl acetals is 0.1 weight part, and a preferable upper limit is 5.0 weight part. If the content of the radical photopolymerization initiator is less than 0.1 parts by weight, it may not be sufficiently crosslinked even when irradiated with light, and a high storage elastic modulus may not be exhibited at a high temperature. If it exceeds the parts by weight, the weather resistance may deteriorate and yellowing may occur.
- the more preferred lower limit of the content of the photo radical polymerization initiator is 0.3 parts by weight, the more preferred upper limit is 3.0 parts by weight, the still more preferred lower limit is 0.4 parts by weight, and the still more preferred upper limit is 1.5 parts by weight.
- the particularly preferred lower limit is 0.5 parts by weight, and the particularly preferred upper limit is 1.0 part by weight.
- the monomer or oligomer having a radical polymerizable double bond serves as a bridge for crosslinking between polyvinyl acetals when irradiated with ultraviolet rays. Especially, since a high crosslinking density is obtained, the polyfunctional monomer or oligomer which has two or more radically polymerizable double bonds in a molecule
- numerator is suitable.
- polyfunctional monomer or oligomer examples include acrylates and methacrylates. Specifically, for example, trimethylolpropane triacrylate, tetramethylolmethane tetraacrylate, pentaerythritol triacrylate, pentaerythritol tetraacrylate, dipentaerythritol monohydroxypentaacrylate, dipentaerythritol hexaacrylate or the same methacrylates as described above can be used. Can be mentioned.
- Examples include 1,4-butylene glycol diacrylate, 1,6-hexanediol diacrylate, polypropylene glycol # 700 diacrylate, polyethylene glycol diacrylate, commercially available oligoester acrylate, and methacrylates similar to those described above. These polyfunctional monomers or oligomers may be used alone or in combination of two or more.
- the monomer or oligomer having a radical polymerizable double bond preferably has a molecular weight of 10,000 or less. If a monomer or oligomer having a radical polymerizable double bond having a molecular weight of 10,000 or less is used, three-dimensional networking is efficiently performed by light irradiation.
- the molecular weight of the monomer or oligomer having a radical polymerizable double bond is more preferably 5000 or less.
- the content of the monomer or oligomer having a radical polymerizable double bond is not particularly limited, but a preferable lower limit with respect to 100 parts by weight of the polyvinyl acetal is 0.1 parts by weight, and a preferable upper limit is 40 parts by weight.
- a preferable lower limit with respect to 100 parts by weight of the polyvinyl acetal is 0.1 parts by weight, and a preferable upper limit is 40 parts by weight.
- the content of the monomer or oligomer having a radical polymerizable double bond is within this range, it can be sufficiently cross-linked by irradiating with light to exhibit a high storage elastic modulus at high temperature, Further, visual distortion does not occur due to the granular local cross-linking.
- the more preferred lower limit of the content of the monomer or oligomer having a radical polymerizable double bond is 0.5 parts by weight
- the more preferred upper limit is 25 parts by weight
- the still more preferred lower limit is 1 part by weight
- the still more preferred upper limit is 15 parts by weight.
- Parts, and a particularly preferred upper limit is 8 parts by weight.
- the polyvinyl acetal resin composition of the present invention preferably contains a plasticizer.
- a plasticizer By containing a plasticizer, it can be plasticized to improve the flexibility of the polyvinyl acetal resin composition.
- particularly high step followability can be exhibited by blending a plasticizer.
- the said plasticizer is not specifically limited, A conventionally well-known plasticizer can be used. Specific examples include organic acid ester plasticizers such as monobasic organic acid esters and polybasic organic acid esters, and phosphoric acid plasticizers such as organic phosphoric acid plasticizers and organic phosphorous acid plasticizers. These plasticizers may be used alone or in combination of two or more. Of these, organic acid ester plasticizers are preferred.
- the plasticizer is preferably a liquid plasticizer.
- the monobasic organic acid ester is not particularly limited.
- butyric acid, isobutyric acid, caproic acid, 2-ethylbutyric acid, heptylic acid, n-octylic acid, 2-ethylhexylic acid, pelargonic acid (n-nonylic acid) examples thereof include glycol esters obtained by reacting monobasic organic acids such as decyl acid with glycols such as triethylene glycol, tetraethylene glycol and tripropylene glycol.
- the polybasic organic acid ester is not particularly limited. For example, by reacting a polybasic organic acid such as adipic acid, sebacic acid or azelaic acid with an alcohol having a linear or branched structure having 4 to 8 carbon atoms. The obtained ester compound etc. are mentioned.
- the organic acid ester plasticizer is preferably a diester plasticizer represented by the following formula (1).
- R 1 —CO — (— R 3 —O—) p —CO—R 2 (1)
- R 1 and R 2 each represents an organic group having 5 to 10 carbon atoms (preferably 6 to 10 carbon atoms)
- R 3 represents an ethylene group, an isopropylene group or an n-propylene group
- p represents an integer of 3 to 10.
- organic acid ester plasticizer examples include triethylene glycol-di-2-ethylbutyrate, triethylene glycol-di-2-ethylhexanoate, triethylene glycol dicaprylate, and triethylene glycol diester.
- the organophosphate plasticizer is not particularly limited, and examples thereof include tributoxyethyl phosphate, isodecylphenyl phosphate, triisopropyl phosphate, and the like.
- dihexyl adipate DHA
- triethylene glycol-di-2-ethylhexanoate 3GO
- tetraethylene glycol-di-2-ethylhexanoate 4GO
- triethylene glycol-di -2-Ethylbutyrate 3GH
- Tetraethyleneglycol-di-2-ethylbutyrate 4GH
- Triethyleneglycol-di-n-heptanoate (3G7) At least one selected from the group consisting of triethylene glycol-di-2-ethylbutyrate, triethylene glycol-di-n-heptanoate (3G7), triethylene glycol-di-2-ethylhexanoate (3GO) is more preferred.
- Glycol - di-2-ethylhexanoate is more preferred.
- the content of the plasticizer is not particularly limited, but a preferable lower limit with respect to 100 parts by weight of the polyvinyl acetal is 1 part by weight, and a preferable upper limit is 75 parts by weight. When the content is within this range, high toughness and adhesion to inorganic materials can be exhibited. In addition, the plasticizer can be prevented from bleeding out.
- the more preferred lower limit of the plasticizer content is 2 parts by weight, the more preferred upper limit is 60 parts by weight, the still more preferred lower limit is 3 parts by weight, the still more preferred upper limit is 50 parts by weight, and the particularly preferred lower limit is 4 parts by weight.
- the particularly preferred upper limit is 40 parts by weight, the most preferred lower limit is 5 parts by weight, and the most preferred upper limit is 30 parts by weight.
- the content of the plasticizer is not particularly limited, but a preferable lower limit with respect to 100 parts by weight of the polyvinyl acetal is 5 parts by weight, A preferred upper limit is 75 parts by weight. If the content is within the above range, it is possible to sufficiently suppress the scattering of fragments when the portable information terminal is damaged, and to prevent bubbles from remaining in the steps during filling between layers (during bonding). It becomes easy to achieve both. If the content is less than 5 parts by weight, the moldability of the interlayer filling material for a touch panel may be lowered.
- the transparency of the interlayer filling material for a touch panel may decrease, or the plasticizer may bleed out.
- the more preferred lower limit of the plasticizer is 10 parts by weight, the still more preferred lower limit is 15 parts by weight, the particularly preferred lower limit is 20 parts by weight, the more preferred upper limit is 65 parts by weight, the still more preferred upper limit is 55 parts by weight, and the particularly preferred upper limit is 45 parts by weight.
- the cohesive force is generated by the polyvinyl acetal, so that the content of the plasticizer is preferably small. That is, it is preferable to increase the compatibility between the polyvinyl acetal and the plasticizer to reduce the content of the plasticizer. Thereby, scattering prevention property can be improved.
- a method for increasing the compatibility between the polyvinyl acetal and the plasticizer for example, a method for increasing the degree of acetalization of the polyvinyl acetal and a method for increasing the amount of acetyl groups are preferable.
- a method of removing the blocking property of the hydroxyl group of the polyvinyl acetal As a method of suppressing the blocking of the hydroxyl group, a method of lowering the aging temperature is preferable.
- the total content of the polyvinyl acetal and the plasticizer in the interlayer filling material for a touch panel is preferably 50% by weight or more.
- the content is less than 50% by weight, when the portable information terminal is damaged, scattering of fragments cannot be sufficiently suppressed, or air bubbles may remain in a step when filling (bonding) between layers.
- the more preferable lower limit of the content is 60% by weight, the still more preferable lower limit is 70% by weight, the still more preferable lower limit is 80% by weight, and the particularly preferable lower limit is 90% by weight.
- the polyvinyl acetal resin composition of the present invention is further provided with an adhesive strength modifier, a tackifier resin, a plasticizer, an emulsifier, a softener, fine particles, a filler, a pigment, a dye, a silane coupling agent, and an antioxidant, as necessary. Further, known additives such as surfactants and waxes may be contained.
- the polyvinyl acetal resin composition of the present invention can be used in the form of a sheet in addition to liquid (dispersed liquid, emulsion). In particular, it can be used as an adhesive sheet by forming it into a sheet.
- An adhesive sheet comprising the polyvinyl acetal resin composition of the present invention is also one aspect of the present invention.
- the polyvinyl acetal resin composition or the adhesive sheet of the present invention can be formed by a conventionally known method such as an extrusion method, a method of finishing, a casting method, a calendar method, or a pressing method. Of these, the extrusion method is preferable because of its excellent production efficiency.
- the polyvinyl acetal resin composition of the present invention does not react and generate gel even at a high temperature during extrusion.
- the polyvinyl acetal resin composition or adhesive sheet of the present invention can be cross-linked by irradiating light to exhibit a high storage elastic modulus even at high temperatures.
- the storage elastic modulus G ′ at 200 ° C. can be 5 ⁇ 10 3 Pa or more, preferably 1 ⁇ 10 4 Pa or more.
- the storage elastic modulus G ′ at 200 ° C. is determined by using a dynamic viscoelasticity measuring device such as ARES-G2 (TAINSTRUMMENTS), DVA-200 (ITT Measurement Control), etc. , And frequency 1 Hz, distortion 1% can be measured.
- the method of light irradiation is not particularly limited, and examples thereof include a method of irradiating the adhesive sheet of the present invention and the polyvinyl acetal resin composition of the present invention after molding using an ultraviolet irradiation device such as an ultrahigh pressure mercury lamp. .
- an ultraviolet irradiation device such as an ultrahigh pressure mercury lamp.
- What is necessary is just to set suitably the wavelength and illumination intensity of the light at the time of the said light irradiation by the kind etc. of the said radical photopolymerization initiator.
- benzophenone which is a hydrogen abstraction type photo radical polymerization initiator is used as the photo radical polymerization initiator
- light having a wavelength of 250 to 400 nm is irradiated at an illuminance of 10 mW / cm 2 for 10 seconds to 30 minutes. Is preferred.
- the use of the polyvinyl acetal resin composition of the present invention is not particularly limited, it can be used for applications such as paints, wash primers, binders for ceramics, interlayer films for laminated glass, and interlayer filling materials for touch panels. Especially, it is very useful as an interlayer filling material for touch panels.
- Touch panels are used in various fields.
- a touch panel is disposed under a surface protection panel made of glass or the like, followed by a polarizing film or a display.
- the interlayer between the surface protection panel and the touch panel and the interlayer between the touch panel and the polarizing film are filled with a filling material that has a smaller refractive index difference with these members than air.
- the display screen is improved in transparency, brightness, contrast, and the like.
- an acrylic pressure-sensitive adhesive or pressure-sensitive adhesive tape is frequently used from the viewpoints of transparency, adhesiveness, coating property and the like.
- an acrylic pressure-sensitive adhesive or adhesive tape is pasted as a filling material, entrainment of bubbles may occur at the time of pasting, and bubbles may remain between the surface protection panel and the filling material.
- a printing part is formed on the back side of the surface protection panel for the purpose of masking or the like, and a step formed by such a printing part or a boundary part of a wiring step formed on the touch panel In other words, bubbles remain in the surface, and the visibility or durability is deteriorated.
- plasticized polyvinyl acetal As an interlayer filling material for a touch panel, a sheet-like interlayer filling material for a touch panel using plasticized polyvinyl acetal has been studied as an alternative to the acrylic pressure-sensitive adhesive that has been widely used. Since plasticized polyvinyl acetal has low tack at room temperature, there is little glue residue on the punching blade during punching at room temperature. On the other hand, by pressing while heating, it is possible to sufficiently follow the decorative printed portion step and the wiring step. Furthermore, in the unlikely event that the portable information terminal is damaged due to an impact such as dropping, an effect of suppressing scattering of fragments such as glass can be expected.
- the present inventors examined the cause of foaming when a touch panel using an interlayer filling material for a touch panel containing plasticized polyvinyl acetal is exposed to high temperature and high humidity. As a result, it has been found that fine foreign matter having a size of several to several tens of ⁇ m adhered to the surface of the adherend is the cause. If the interlayer filling material for a touch panel is pasted with such fine foreign matter attached, even if it is heated and pressure-bonded, it cannot follow completely, and very small bubbles are formed around the fine foreign matter. Remains. Such minute bubbles are usually hardly recognized with the naked eye, but when exposed to high temperature and high humidity, it was considered that they grow into bubbles that can be recognized with the naked eye.
- Bubbles are generated from an adherend such as a polycarbonate plate, an acrylic plate, or a polarizing film under high temperature and high humidity, and when the outgas is concentrated on a minute bubble portion, the stress of the interlayer filling material for the touch panel is caused by the stress. It seemed to grow by partly deforming.
- the present inventors use the polyvinyl acetal resin composition of the present invention as an interlayer filling material for a touch panel so that foaming does not occur even when exposed to high temperature and high humidity. I found out that I can do it.
- the interlayer filling material for a touch panel comprising the polyvinyl acetal resin composition of the present invention has high thermal stability and can be easily molded by, for example, an extrusion method.
- the radical photopolymerization initiator is activated to generate radicals, which pull the C—H hydrogen in the polyvinyl acetal, via a monomer or oligomer having a radical polymerizable double bond. Polyvinyl acetal is crosslinked.
- an interlayer filling material for a touch panel is used and an uncrosslinked interlayer filling material for a touch panel is heated (around 85 ° C.) at the time of filling (bonding) between layers, the storage elastic modulus and loss elastic modulus are greatly reduced. And even if it is a thin filling material, the bubble remaining in the boundary part of a level
- the interlayer filling material for touch panels can be crosslinked.
- the cross-linked interlayer filling material for a touch panel can exhibit a high storage elastic modulus even when exposed to high temperature and high humidity.
- An interlayer filling material for a touch panel used for filling an interlayer between a touch panel and another member or between a plurality of transparent conductive films constituting the touch panel, and the polyvinyl acetal resin composition or the adhesive sheet of the present invention
- An interlayer filling material for a touch panel is also one aspect of the present invention.
- the thickness when the interlayer filling material for a touch panel of the present invention is in a sheet form is not particularly limited and is set depending on the application, but a preferable lower limit is 5 ⁇ m and a preferable upper limit is 800 ⁇ m. When the thickness is less than 5 ⁇ m, bubbles may easily remain in the step during filling between layers (during bonding).
- the more preferable lower limit of the thickness is 10 ⁇ m, the more preferable upper limit is 400 ⁇ m, the still more preferable lower limit is 50 ⁇ m, the still more preferable upper limit is 300 ⁇ m, the still more preferable lower limit is 100 ⁇ m, and the still more preferable upper limit is 200 ⁇ m.
- the method for producing the interlayer filling material for a touch panel of the present invention is not particularly limited.
- the polyvinyl acetal, the photo radical polymerization initiator, and a monomer or oligomer having a radical polymerizable double bond Then, a composition containing an additive such as a plasticizer blended as necessary is formed into a sheet by a normal film forming method such as an extrusion method, a coating method, a casting method, a calendar method, or a pressing method. A method is mentioned. Of these, the extrusion method is preferable because of its excellent production efficiency.
- the interlayer filling material for a touch panel of the present invention can be easily molded without being crosslinked even at a high temperature during extrusion.
- a more specific application of the interlayer filling material for a touch panel of the present invention is not particularly limited.
- a flat type or a flexible type using an image display panel such as a portable information terminal (for example, a smartphone or a tablet), an LCD, an EL, or a PDP.
- an image display device for example, electronic paper, PDA, TV, game machine
- an interlayer between a surface protection panel and a touch panel an interlayer between a touch panel and a polarizing film, and an interlayer between a plurality of transparent conductive films constituting the touch panel
- FIG. 1 is a cross-sectional view schematically showing an example of a method of using the interlayer filling material for a touch panel of the present invention.
- the interlayer between the surface protection panel 3 and the touch panel 2 and the interlayer between the touch panel 2 and the polarizing film 4 are filled with the interlayer filling material 1 for a touch panel of the present invention.
- a decorative printing portion 5 is formed on the peripheral portion of the back side of the surface protection panel 3 for the purpose of masking or the like, but the interlayer filling material 1 for a touch panel of the present invention is such a decorative printing. Air bubbles remaining at the boundary of the step at the time of filling (bonding) between the layers sufficiently following the step formed by the part 5 and the step (not shown) of the wiring formed on the touch panel 2. Can be removed.
- At least one kind of interlayer selected from the group consisting of an interlayer between a surface protection panel and a touch panel, an interlayer between a touch panel and a polarizing film, and an interlayer between a plurality of transparent conductive films constituting the touch panel is an interlayer for a touch panel of the present invention.
- a laminate that is filled with a filling material is also one aspect of the present invention.
- the said surface protection panel is not specifically limited, For example, what is normally used for a portable information terminal, a flat type, or a flexible image display apparatus, such as a glass plate, a polycarbonate plate, an acrylic plate, can be used.
- the said touch panel is not specifically limited, For example, what is normally used for a portable information terminal, a flat type, or a flexible image display apparatus, such as a touch panel having a plurality of layers such as an ITO film, can be used.
- the configuration of the touch panel is not particularly limited, and examples thereof include an out-cell type, an in-cell type, an on-cell type, a cover glass integrated type, and a cover sheet integrated type.
- the touch panel system is not particularly limited, and examples thereof include a resistance film type, a capacitance type, an optical type, and an ultrasonic type. It does not specifically limit as said polarizing film, The thing normally used for a portable information terminal, a flat type, or a flexible image display apparatus etc. can be used.
- the interlayer filling material for a touch panel of the present invention at least selected from the group consisting of an interlayer between a surface protection panel and a touch panel, an interlayer between a touch panel and a polarizing film, and an interlayer of a plurality of transparent conductive films constituting the touch panel.
- the method for producing a laminate by filling one kind of interlayer is not particularly limited.
- the interlayer between the surface protection panel and the touch panel, the interlayer between the touch panel and the polarizing film, and a plurality of transparent conductive films constituting the touch panel There is a method in which the interlayer filling material for touch panel of the present invention is sandwiched between the layers and pre-heat-pressed at around 70 ° C.
- pre-heat-pressure bonding on the conditions of 1 atmosphere, 70 degreeC, and 30 minutes, for example using a vacuum laminator.
- main-bonding by autoclave treatment for example, 85 ° C, 0.5 MPa or more for 30 minutes
- the polyvinyl acetal is crosslinked by irradiating light to obtain the laminate of the present invention. It is done.
- the light irradiation method is not particularly limited, and examples thereof include a method of irradiating light to the laminate after the main pressure bonding using an ultraviolet irradiation device such as an ultrahigh pressure mercury lamp. What is necessary is just to set suitably the wavelength and illuminance of the light at the time of the said light irradiation by the kind etc. of the said hydrogen abstraction type photoinitiator.
- an ultraviolet irradiation device such as an ultrahigh pressure mercury lamp.
- a polyvinyl acetal resin composition that is excellent in thermal stability and can be molded by an extrusion method and that can exhibit a high storage elastic modulus even at high temperatures, an adhesive sheet comprising the polyvinyl acetal resin composition, An interlayer filling material for a touch panel made of a polyvinyl acetal resin composition and a laminate produced using the interlayer filling material for a touch panel can be provided.
- Example 1 (1) Preparation of polyvinyl butyral In a reactor equipped with a stirrer, 2700 mL of ion-exchanged water, 300 g of polyvinyl alcohol having an average polymerization degree of 1800 and a saponification degree of 99.3 mol% were added, dissolved with heating to dissolve the solution. Obtained. Next, 35 wt% hydrochloric acid as a catalyst was added to this solution so that the hydrochloric acid concentration would be 0.2 wt%, the temperature was adjusted to 15 ° C., and n-butyraldehyde (n-BA) was stirred. 21 g was added.
- n-BA n-butyraldehyde
- n-butyraldehyde n-BA
- white particulate polyvinyl butyral resin was precipitated.
- 35 wt% hydrochloric acid was added so that the hydrochloric acid concentration was 1.8 wt%, heated to 50 ° C., and aged at 50 ° C. for 2 hours.
- the solution was cooled, neutralized, washed with water, and dried to obtain polyvinyl butyral (PVB).
- the obtained polyvinyl butyral had a hydroxyl group content of 31.0 mol%, an acetyl group content of 0.7 mol%, and a butyralization degree (Bu-conversion degree) of 68.3 mol%.
- interlayer filling material for touch panel 30 parts by weight of triethylene glycol-di-2-ethylhexanoate (3GO) as a plasticizer with respect to 100 parts by weight of the obtained polyvinyl butyral, photo radical polymerization initiator 1 part by weight of benzophenone and 4 parts by weight of trimethylolpropane triacrylate as a monomer having a radical polymerizable double bond were added and kneaded sufficiently to obtain a kneaded product.
- the obtained kneaded material was press-molded with a press molding machine to form a sheet, and an interlayer filling material for a touch panel having a thickness of 150 ⁇ m was obtained.
- the interlayer filling material for a touch panel was irradiated with light having a wavelength of 365 nm for 1200 seconds at an illuminance of 10 mW / cm 2 using an ultrahigh pressure mercury lamp.
- a temperature drop rate of 3 ° C./min and a frequency of 1 Hz using a dynamic viscoelasticity measuring device ARES-G2 (TAINSTRUMENTS), ADVA-200 (IT Measurement & Control).
- ARES-G2 TAINSTRUMENTS
- ADVA-200 IT Measurement & Control
- Example 2 A polyvinyl butyral resin composition was obtained in the same manner as in Example 1 except that 1 part by weight of thioxanthone was used as a radical photopolymerization initiator. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- Example 3 A polyvinyl butyral resin composition was obtained in the same manner as in Example 1 except that 0.5 part by weight of benzophenone was used as a radical photopolymerization initiator. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- Example 4 A polyvinyl butyral resin composition was obtained in the same manner as in Example 1 except that 10 parts by weight of ethoxytrimethylolpropane triacrylate was used as a monomer having a radical polymerizable double bond. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- Example 5 A polyvinyl butyral resin composition as in Example 1, except that 4 parts by weight of ditrimethylolpropane tetraacrylate was used as an oligomer having a radical polymerizable double bond instead of a monomer having a radical polymerizable double bond. Got. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- Example 6 A polyvinyl butyral resin composition as in Example 1 except that 4 parts by weight of dipentaerythritol hexaacrylate was used as an oligomer having a radical polymerizable double bond instead of a monomer having a radical polymerizable double bond. Got. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- Example 7 A polyvinyl butyral resin composition was obtained in the same manner as in Example 1 except that 10 parts by weight of trimethylolpropane triacrylate was used as a monomer having a radical polymerizable double bond. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- Example 8 A polyvinyl butyral resin composition was obtained in the same manner as in Example 1 except that 30 parts by weight of trimethylolpropane triacrylate was used as a monomer having a radical polymerizable double bond without blending a plasticizer. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- Example 9 A polyvinyl butyral resin composition was obtained in the same manner as in Example 1 except that 0.5 part by weight of trimethylolpropane triacrylate was used as a monomer having a radical polymerizable double bond. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- Example 1 A polyvinyl butyral resin composition was obtained in the same manner as in Example 1 except that the radical photopolymerization initiator and the monomer having a radical polymerizable double bond were not blended. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- Example 2 A polyvinyl butyral resin composition was obtained in the same manner as in Example 1 except that no monomer having a radical polymerizable double bond was added. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- Example 3 A polyvinyl butyral resin composition was obtained in the same manner as in Example 1 except that the radical photopolymerization initiator was not blended. Further, an interlayer filling material for a touch panel was obtained in the same manner as in Example 1.
- a diluted sample obtained by diluting the obtained acrylic copolymer 50 times with tetrahydrofuran (THF) was filtered through a filter (material: polytetrafluoroethylene, pore diameter: 0.2 ⁇ m) to prepare a measurement sample.
- This measurement sample is supplied to a gel permeation chromatograph (manufactured by Waters, 2690 Separations Model), GPC measurement is performed under the conditions of a sample flow rate of 1 ml / min and a column temperature of 40 ° C., and the polystyrene equivalent molecular weight of the acrylic copolymer is measured. Was measured to determine the weight average molecular weight (Mw).
- the weight average molecular weight of the obtained acrylic copolymer was 650,000.
- GPC LF-804 manufactured by Showa Denko
- a differential refractometer was used as the detector.
- interlayer filling material for touch panel One side of interlayer filling material for touch panel is affixed to glass of 15.0 cm x 7.5 cm and thickness 0.7 mm, and the other side of interlayer filling material for touch panel was affixed to an ITO-coated polyethylene terephthalate film (ITO-PET) to prepare a glass / interlayer filling material for touch panel / ITO-PET film structure.
- ITO-PET ITO-coated polyethylene terephthalate film
- a steel ball having a weight of 130 g is dropped from a height of 1 m in an environment of 23 ° C. with respect to the obtained laminate, and 1 when the laminate is not broken, and the glass piece of the laminate is broken is scattered.
- the case was set to 5.
- this structure was pressure-bonded at 70 ° C. for 30 minutes using a vacuum laminator at 1 atm, then treated with an autoclave at 85 ° C. and 0.5 MPa for 30 minutes, and then decompressed and taken out at 30 ° C. or less. It was.
- a layered product in which light of 365 nm is irradiated at an illuminance of 10 mW / cm 2 for 1200 seconds, and the interlayer between the glass and the ITO-PET film is filled with an interlayer filling material for a touch panel.
- the obtained laminate was observed with a digital microscope (manufactured by Keyence Corporation), and the case where no bubbles remained was evaluated as “ ⁇ ”, and the case where bubbles remained was evaluated as “x”.
- the obtained laminate was allowed to stand for 250 hours under a high temperature and high humidity condition of a temperature of 85 ° C. and a humidity of 85% to perform a high temperature and high humidity treatment.
- the structure after the high-temperature and high-humidity treatment was observed with a digital microscope (manufactured by Keyence Corporation). The case where foaming was not observed was evaluated as “ ⁇ ”, and the case where foaming was observed was evaluated as “x”.
- a polyvinyl acetal resin composition that is excellent in thermal stability and can be molded by an extrusion method and that can exhibit a high storage elastic modulus even at high temperatures, an adhesive sheet comprising the polyvinyl acetal resin composition, An interlayer filling material for a touch panel made of a polyvinyl acetal resin composition and a laminate produced using the interlayer filling material for a touch panel can be provided.
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Abstract
Description
しかしながら、ポリビニルアセタールは、20℃程度の常温下での貯蔵弾性率は高いものの、高温下では貯蔵弾性率が大きく低下してしまうという問題があった。
光ラジカル重合開始剤(とりわけ水素引抜型光ラジカル重合開始剤)は、高温下でも安定性が高く、ポリビニルアセタールの通常の押し出し成形温度(100~220℃程度)では活性化しない。しかしながら、光ラジカル重合開始剤に光を照射すると活性化してラジカルを生じ、該ラジカルがポリビニルアセタール中のC-Hの水素を引き、ラジカル重合性二重結合を有するモノマー又はオリゴマーを介して架橋するため、高温下でも高い貯蔵安定性を発揮できるものと考えられた。
上記ポリビニルアセタールは、例えば、ポリ酢酸ビニルを鹸化することにより得られたポリビニルアルコールを、触媒存在下でアルデヒドによりアセタール化することにより調製することができる。
上記ポリビニルアルコールの平均重合度は特に限定されないが、より優れた性能を発揮する観点からは分子量の大きなポリビニルアセタールが好適であるため、平均重合度の高いポリビニルアルコールを用いることが好ましい。上記ポリビニルアルコールの平均重合度の好ましい下限は200、好ましい上限は4000である。上記ポリビニルアルコールの平均重合度がこの範囲内であると、ポリビニルアルコールをアセタール化する際の反応が容易であり、かつ、得られるポリビニルアセタールは高い機械的強度を発揮することができる。また、本発明のポリビニルアセタール樹脂組成物を後述するタッチパネル用層間充填材料に用いる場合に、携帯情報端末が破損したときに破片の飛散を抑制することができる。上記ポリビニルアルコールの平均重合度のより好ましい下限は600、より好ましい上限は3800であり、更に好ましい下限は800、更に好ましい上限は3600である。
なお、本明細書においてポリビニルアルコールの平均重合度は、JIS K6726:1994年に基づき求められる粘度平均重合度をいう。ポリビニルアルコール樹脂として2種以上のポリビニルアルコール樹脂を混合して用いる場合は、混合後のポリビニルアルコール樹脂全体の見掛け上の粘度平均重合度をいう。
上記炭素数が1~10のアルデヒドは特に限定されず、直鎖状のアルデヒドであってもよいし、分枝状のアルデヒドであってもよく、例えば、n-ブチルアルデヒド、イソブチルアルデヒド、n-バレルアルデヒド、2-エチルブチルアルデヒド、n-ヘキシルアルデヒド、n-オクチルアルデヒド、n-ノニルアルデヒド、n-デシルアルデヒド、ホルムアルデヒド、アセトアルデヒド、ベンズアルデヒド等が挙げられる。これらのアルデヒドは単独で用いられてもよく、2種以上を併用してもよい。なかでも、n-ブチルアルデヒド、n-ヘキシルアルデヒド、n-バレルアルデヒドが好ましく、n-ブチルアルデヒドがより好ましい。
即ち、上記ポリビニルアセタールは、ポリビニルブチラール(上記アルデヒドがn-ブチルアルデヒドである場合、上記ポリビニルアセタールをポリビニルブチラールという)であることが好ましい。上記ポリビニルブチラールは、ガラス等に対する接着力が適切に発現し、耐光性、耐候性等にも優れる。また、必要に応じて2種以上のポリビニルアセタールを併用してもよい。
このような分子間架橋の少ないポリビニルアセタールを得る方法として、例えば、隣接するポリビニルアルコールの主鎖を架橋させないように、上記アルデヒドによるアセタール化反応の前又は途中で上記アルデヒドを過剰に投入しないようにする方法が好ましい。アセタール化に必要な量を超えて上記アルデヒドを投入すると、架橋の度合いが高くなる。
上記ポリビニルアセタールの水酸基量のより好ましい下限は18モル%、より好ましい上限は40モル%であり、更に好ましい下限は20モル%、更に好ましい上限は38モル%である。また、本発明のポリビニルアセタール樹脂組成物を後述するタッチパネル用層間充填材料に用いる場合には、上記水酸基量のより好ましい下限は18モル%、更に好ましい下限は20モル%、特に好ましい下限は22モル%であり、より好ましい上限は40モル%、更に好ましい上限は38モル%、更により好ましい上限は36モル%、特に好ましい上限は35モル%である。
なお、ポリビニルアセタールの水酸基量は、水酸基が結合しているエチレン基量を、主鎖の全エチレン基量で除算して求めたモル分率を百分率(モル%)で表した値である。水酸基が結合しているエチレン基量は、例えば、JIS K6728「ポリビニルブチラール試験方法」に準拠した方法により求めることができる。
上記ポリビニルアセタールのアセチル基量のより好ましい下限は0.2モル%、より好ましい上限は24モル%であり、更に好ましい下限は0.3モル%、更に好ましい上限は20モル%であり、特に好ましい上限は19.5モル%、最も好ましい上限は15モル%である。
なお、ポリビニルアセタールのアセチル基量は、主鎖の全エチレン基量から、アセタール基が結合しているエチレン基量と、水酸基が結合しているエチレン基量とを差し引いた値を、主鎖の全エチレン基量で除算して求めたモル分率を百分率(モル%)で表した値である。アセタール基が結合しているエチレン基量は、例えば、JIS K6728「ポリビニルブチラール試験方法」に準拠して測定できる。
なお、ポリビニルアセタールのアセタール化度は、アセタール基が結合しているエチレン基量を、主鎖の全エチレン基量で除算して求めたモル分率を百分率(モル%)で表した値である。アセタール化度は、JIS K6728「ポリビニルブチラール試験方法」に準拠した方法により、アセチル基量とビニルアルコール量(水酸基の含有率)とを測定し、得られた測定結果からモル分率を算出し、次いで、100モル%からアセチル基量とビニルアルコール量とを差し引くことにより算出されうる。
上記水素引抜型光ラジカル重合開始剤としては、例えば、ベンゾフェノン、チオキサントン、ミヒラーズケトン等が挙げられる。これらの光ラジカル重合開始剤は単独で用いてもよく、2種以上を併用してもよい。なかでも、光照射時の活性に優れるとともに、高温下での安定性に特に優れ、ポリビニルアセタールの押し出し温度ではほとんど活性化しないことから、ベンゾフェノンが好適である。
上記多塩基性有機酸エステルは特に限定されず、例えば、アジピン酸、セバシン酸、アゼライン酸等の多塩基性有機酸と、炭素数4~8の直鎖又は分岐構造を有するアルコールとの反応によって得られたエステル化合物等が挙げられる。
R1-CO-(-R3-O-)p-CO-R2 (1)
式(1)中、R1及びR2はそれぞれ炭素数5~10(好ましくは炭素数6~10)の有機基を表し、R3はエチレン基、イソプロピレン基又はn-プロピレン基を表し、pは3~10の整数を表す。
また、本発明のポリビニルアセタール樹脂組成物を後述するタッチパネル用層間充填材料に用いる場合には、上記可塑剤の含有量は特に限定されないが、上記ポリビニルアセタール100重量部に対する好ましい下限は5重量部、好ましい上限は75重量部である。上記含有量が上記範囲であれば、携帯情報端末が破損した場合に破片の飛散を充分に抑制することと、層間の充填時(貼合時)に段差に気泡が残存することを抑制することとを両立しやすくなる。上記含有量が5重量部未満であると、タッチパネル用層間充填材料の成形性が低下することがある。上記含有量が75重量部を超えると、タッチパネル用層間充填材料の透明性が低下したり、上記可塑剤がブリードアウトしたりすることがある。上記可塑剤のより好ましい下限は10重量部、更に好ましい下限は15重量部、特に好ましい下限は20重量部であり、より好ましい上限は65重量部、更に好ましい上限は55重量部、特に好ましい上限は45重量部である。
上記ポリビニルアセタールと上記可塑剤との相溶性を高める方法として、例えば、上記ポリビニルアセタールのアセタール化度を大きくする方法、アセチル基量を高くする方法が好ましい。また、上記ポリビニルアセタールの水酸基のブロック性を落とす方法も好ましい。水酸基のブロック化を抑制する方法として、熟成温度を下げる方法が好ましい。
本発明のポリビニルアセタール樹脂組成物からなる接着シートもまた、本発明の1つである。
上記光照射時の光の波長や照度は、上記光ラジカル重合開始剤の種類等により適宜設定すればよい。例えば、上記光ラジカル重合開始剤として水素引抜型光ラジカル重合開始剤であるベンゾフェノンを用いる場合には、250~400nmの波長の光を、10mW/cm2の照度で10秒間~30分間照射することが好ましい。
このような携帯情報端末においては、表面保護パネルとタッチパネルとの層間、及び、タッチパネルと偏光フィルムとの層間を、空気と比較してこれらの部材との屈折率差が小さい充填材料で埋めることにより、表示画面の透明性、輝度、コントラスト等を改善し、視認性を向上させることが行われている。
また、万一落下等の衝撃により携帯情報端末が破損した場合、従来のアクリル系粘着剤又は粘着テープでは、凝集破壊が起こり、ガラス等の破片の飛散を充分に抑制することは難しかった。飛散防止フィルムを別途設けることも検討されているが、コスト及び携帯情報端末の薄型化の観点からは、飛散防止フィルムを使用せずに飛散を抑制することが望まれていた。
しかしながら、可塑化ポリビニルアセタールを用いたタッチパネル用層間充填材料を用いたタッチパネルを高温高湿下(例えば、温度85℃、湿度85%)に晒すと、発泡が生じてしまうことがあるという問題があった。このような問題はアクリル系粘着剤を用いた場合にも生じるが、可塑化ポリビニルアセタールを用いた場合により顕著となった。
本発明のポリビニルアセタール樹脂組成物からなるタッチパネル用層間充填材料は、高い熱安定性を有し、例えば押し出し法によっても容易に成形できる。しかしながら、いったん光を照射すると、光ラジカル重合開始剤が活性化してラジカルを生じ、該ラジカルがポリビニルアセタール中のC-Hの水素を引き、ラジカル重合性二重結合を有するモノマー又はオリゴマーを介してポリビニルアセタールが架橋される。
このようなタッチパネル用層間充填材料を用い、層間の充填時(貼合時)に、未架橋のタッチパネル用層間充填材料を加熱(85℃付近)すれば、貯蔵弾性率及び損失弾性率が大きく低下し、たとえ薄い充填材料であっても加飾印刷部段差又は配線段差に充分に追従して、段差の境界部に残存する気泡を除去できることができる。一方、充填後(貼合後)に光を照射すれば、タッチパネル用層間充填材料を架橋することができる。架橋されたタッチパネル用層間充填材料は、高温高湿下に晒されたときにでも高い貯蔵弾性率を発揮できる。従って、たとえ貼合後に微細な異物の周辺にごく微小な気泡が残存し、高温高湿下で該気泡が成長しようとしても、高い貯蔵弾性率を有するタッチパネル用層間充填材料がその応力によっては変形したりすることなく、気泡の成長を抑えることができる。
タッチパネルと他の部材との層間又は上記タッチパネルを構成する複数の透明導電フィルムの層間を充填するために用いられるタッチパネル用層間充填材料であって、本発明のポリビニルアセタール樹脂組成物、又は、接着シートからなるタッチパネル用層間充填材料もまた、本発明の1つである。
本発明のタッチパネル用層間充填材料は、たとえ薄い充填材料であっても加飾印刷部段差や配線段差に充分に追従して、段差の境界部に残存する気泡を除去することができる。
図1においては、表面保護パネル3の裏側にはマスキング等を目的として周縁部に加飾印刷部5が形成されているが、本発明のタッチパネル用層間充填材料1は、このような加飾印刷部5により形成された段差にも、タッチパネル2に形成されている配線の段差(図示しない)にも充分に追従して、層間の充填時(貼合時)に段差の境界部に残存する気泡を除去することができる。
上記表面保護パネルは特に限定されず、例えば、ガラス板、ポリカーボネート板、アクリル板等の、携帯情報端末、平面型又はフレキシブル画像表示装置等に通常使用されるものを用いることができる。
上記タッチパネルは特に限定されず、例えば、ITO膜等の複数の層を有するタッチパネル等の、携帯情報端末、平面型又はフレキシブル画像表示装置等に通常使用されるものを用いることができる。上記タッチパネルの構成は特に限定されず、例えば、アウトセル型、インセル型、オンセル型、カバーガラス一体型、カバーシート一体型等が挙げられる。上記タッチパネルの方式も特に限定されず、例えば、抵抗膜式、静電容量式、光学式、超音波式等が挙げられる。
上記偏光フィルムとしても特に限定されず、携帯情報端末、平面型又はフレキシブル画像表示装置等に通常使用されるものを用いることができる。
上記光照射時の光の波長や照度は、上記水素引抜型光開始剤の種類等により適宜設定すればよい。例えば、上記水素引抜型光開始剤としてベンゾフェノンを用いる場合には、250~400nmの波長の光を、10mW/cm2の照度で10秒間~30分間照射することが好ましい。
(1)ポリビニルブチラールの調製
攪拌装置を備えた反応機に、イオン交換水2700mL、平均重合度1800、鹸化度99.3モル%のポリビニルアルコールを300g投入し、攪拌しながら加熱溶解し、溶液を得た。次に、この溶液に触媒として35重量%塩酸を、塩酸濃度が0.2重量%となるように添加し、温度を15℃に調整した後、攪拌しながらn-ブチルアルデヒド(n-BA)21gを添加した。その後、n-ブチルアルデヒド(n-BA)145gを添加したところ、白色粒子状のポリビニルブチラール樹脂が析出した。析出してから15分後に、35重量%塩酸を、塩酸濃度が1.8重量%になるように添加し、50℃に加熱し、50℃で2時間熟成させた。次いで、溶液を冷却し、中和した後水洗し、乾燥させることにより、ポリビニルブチラール(PVB)を得た。
得られたポリビニルブチラールの水酸基量は31.0モル%、アセチル基量は0.7モル%、ブチラール化度(Bu化度)は68.3モル%であった。
得られたポリビニルブチラール100重量部に対して、可塑剤としてトリエチレングリコール-ジ-2-エチルヘキサノエート(3GO)30重量部、光ラジカル重合開始剤としてベンゾフェノン1重量部、及び、ラジカル重合性二重結合を有するモノマーとしてトリメチロールプロパントリアクリレート4重量部を添加し、充分に混練してポリビニルブチラール樹脂組成物を得た。
得られたポリビニルブチラール100重量部に対して、可塑剤としてトリエチレングリコール-ジ-2-エチルヘキサノエート(3GO)を30重量部、光ラジカル重合開始剤としてベンゾフェノン1重量部、及び、ラジカル重合性二重結合を有するモノマーとしてトリメチロールプロパントリアクリレート4重量部を添加し、充分に混練して混練物を得た。得られた混練物をプレス成形機でプレス成形してシート状に製膜し、厚み150μmのタッチパネル用層間充填材料を得た。
光照射前後のシート状成形体について、動的粘弾性測定装置ARES-G2(TAINSTRUMENTS社製)、ADVA-200(アイティー計測制御社製)等を用いて、降温速度3℃/分、周波数1Hz、歪1%の条件にて200℃における貯蔵弾性率G’を測定したところ、光照射前には14700Paであったものが、光照射後には127000Paとなった。
光ラジカル重合開始剤としてチオキサントンを1重量部用いたこと以外は実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
光ラジカル重合開始剤としてベンゾフェノンを0.5重量部用いたこと以外は実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
ラジカル重合性二重結合を有するモノマーとしてエトキシトリメチロールプロパントリアクリレートを10重量部用いたこと以外は実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
ラジカル重合性二重結合を有するモノマーの代わりに、ラジカル重合性二重結合を有するオリゴマーとしてジトリメチロールプロパンテトラアクリレートを4重量部用いたこと以外は、実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
ラジカル重合性二重結合を有するモノマーの代わりに、ラジカル重合性二重結合を有するオリゴマーとしてジペンタエリスリトールヘキサアクリレートを4重量部用いたこと以外は、実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
ラジカル重合性二重結合を有するモノマーとしてトリメチロールプロパントリアクリレートを10重量部用いたこと以外は実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
可塑剤を配合せずに、ラジカル重合性二重結合を有するモノマーとしてトリメチロールプロパントリアクリレートを30重量部用いたこと以外は実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
ラジカル重合性二重結合を有するモノマーとしてトリメチロールプロパントリアクリレートを0.5重量部用いたこと以外は実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
光ラジカル重合開始剤及びラジカル重合性二重結合を有するモノマーを配合しなかった以外は実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
ラジカル重合性二重結合を有するモノマーを配合しなかったこと以外は実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
光ラジカル重合開始剤を配合しなかったこと以外は実施例1と同様にしてポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
実施例1と同様の方法により調製したポリビニルブチラール100重量部に対して、可塑剤としてトリエチレングリコール-ジ-2-エチルヘキサノエート(3GO)30重量部、ホウ酸0.05重量部を添加し、充分に混練してポリビニルブチラール樹脂組成物を得た。また、実施例1と同様にしてタッチパネル用層間充填材料を得た。
(1)アクリル共重合体の調製
攪拌機、還流冷却管、温度計、窒素ガス導入口を備えた反応容器に、n-ブチルアクリレート65.0重量部、メチルメタクリレート26.0重量部、エチルアクリレート4.0重量部、ヒドロキシエチルアクリレート1.0重量部、アクリル酸4.0重量部と重合開始剤として2,2’-アゾビスイソブチルニトリル0.2重量部とを酢酸エチル100重量部に溶解し、窒素置換後、80℃で8時間重合してアクリル共重合体を得た。
得られたアクリル共重合体をテトラヒドロフラン(THF)によって50倍希釈して得られた希釈液をフィルター(材質:ポリテトラフルオロエチレン、ポア径:0.2μm)で濾過し、測定サンプルを調製した。この測定サンプルをゲルパーミエーションクロマトグラフ(Waters社製、2690 Separations Model)に供給して、サンプル流量1ミリリットル/min、カラム温度40℃の条件でGPC測定を行い、アクリル共重合体のポリスチレン換算分子量を測定して、重量平均分子量(Mw)を求めた。
得られたアクリル共重合体の重量平均分子量は65万であった。
カラムとしてはGPC LF-804(昭和電工社製)を用い、検出器としては示差屈折計を用いた。
上記アクリル共重合体100重量部を酢酸エチルで希釈し樹脂固形分45%の粘着剤溶液を得た。上記粘着剤溶液100重量部に対し、イソシアネート系架橋剤(日本ポリウレタン社製コロネートL-45、固形分45%)を1重量部添加し15分攪拌後、厚み50μmの離型PETフィルムの離型処理面に乾燥後の厚さが150μmになるように塗工して、80℃で15分間乾燥した。更に得られた粘着剤層の上に、離型処理面が粘着剤層に接するようにして新たに用意した離型PETフィルムを重ね合わせて積層体を得た。その後シートを23℃で5日間養生し、離型PETフィルムが両面に貼り付けられた厚み150μmのタッチパネル用層間充填材料を得た。
実施例及び比較例で得られたポリビニルブチラール樹脂組成物及びタッチパネル用層間充填材料について、以下の方法により評価を行った。
結果を表1、2に示した。
得られたポリビニルブチラール樹脂組成物を180℃、1時間加熱処理した。加熱処理後のポリビニルブチラール樹脂組成物について目視にて観察して、ゲル化が全く認められなかった場合を「○」と、一部でもゲル化が認められた場合を「×」と評価した。
実施例及び比較例で得られたポリビニルブチラール樹脂組成物を、200℃の温度条件で押し出し成形して、厚み200μmのシート状成形体を得た。
得られたシート状成形体に、超高圧水銀灯を用いて、365nmの波長の光を10mW/cm2の照度で1200秒間照射した。
光照射前後のシート状成形体を酢酸エチル中に23℃にて24時間浸漬した後、酢酸エチルから取り出して、110℃の条件下で1時間乾燥させた。乾燥後の試験片の重量を測定し、下記式を用いてゲル分率を算出した。
ゲル分率(重量%)=100×W2/W1
(W1:浸漬前の試験片の重量、W2:浸漬、乾燥後の試験片の重量)
実施例及び比較例で得られたポリビニルブチラール樹脂組成物を、200℃の温度条件で押し出し成形して、厚み200μmのシート状成形体を得た。
得られたシート状成形体を4枚積層し、800μm厚みの積層体を作製し、UV照射前の貯蔵弾性率測定サンプルとした。
また、得られたシート状成形体に、超高圧水銀灯を用いて、365nmの波長の光を10mW/cm2の照度で500秒間照射した。UV照射後のシート状成形体を4枚積層し、800μm厚みの積層体を作製し、UV照射後の貯蔵弾性率測定サンプルとした。
UV照射前の貯蔵弾性率測定サンプル及びUV照射後の貯蔵弾性率測定サンプルについて、動的粘弾性測定装置ARES-G2(TAINSTRUMENTS社製)を用いて、降温速度3℃/分、周波数1Hz、歪1%の条件にて200℃における貯蔵弾性率G’を測定した。
タッチパネル用層間充填材料を用いて25mm×100mmにカットし、ガラスに貼合した。プラズマ処理を施したPETフィルム(25mm×100mm)を貼合し、25℃で真空ラミネートした後、オートクレーブ中で75℃、0.5MPa条件で30分間加熱圧着し、評価サンプルを得た。得られた評価サンプルを用いて、JIS K 6854:1994年に準拠して300mm/分で180°ピール試験を行い、剥離強度を測定した。剥離強度が5N/25mm以上であったものを「○」とし、5N/25mm未満であったものを「×」とした。
タッチパネル用層間充填材料を50mm×50mmのトムソン刃で50回打ち抜いたときに、トムソン刃へのタッチパネル用層間充填材料の付着(糊残り)発生の有無を目視により確認した。トムソン刃に糊残りが発生しなかったものを「○」とし、糊残りが発生したものを「×」とした。
15.0cm×7.5cm、厚み0.7mmのガラスにタッチパネル用層間充填材料の片面を貼付し、タッチパネル用層間充填材料のもう一方の面をITOがコーティングされたポリエチレンテレフタレートフィルム(ITO-PET)に貼付し、ガラス/タッチパネル用層間充填材料/ITO-PETフィルム構成体を作製した。この構成体を、70℃で30分、1気圧で真空ラミネータを用いた圧着してから、85℃、0.5MPaのオートクレーブで30分処理し、30℃以下にしてから解圧して取り出した。次いで、超高圧水銀灯を用いて、365nmの波長の光を10mW/cm2の照度で1200秒間照射して、ガラスとITO-PETフィルムとの層間がタッチパネル用層間充填材料で充填されている積層体を得た。
ただし、落球箇所のガラス自体から生じたガラス粉又はガラス自体の破壊による破片はガラス片には含めず、ガラスとタッチパネル用層間充填材料との界面における、ガラスのタッチパネル用層間充填材料からの剥離によるガラス片、又は、タッチパネル用層間充填材料の凝集破壊による充填材料付きガラス片を評価対象とした。
76mm×52mm、厚み1.0~1.2mmの白板ガラス(松浪硝子製S9112)に白板ガラスと同サイズにカットしたタッチパネル用層間充填材料の片面を貼付し、タッチパネル用層間充填材料のもう一方の面を白板ガラスと同サイズにカットしたITO-PETフィルム(ITOをコーティングしたポリエチレンテレフタレート(PET)フィルム)に貼付し、ガラス/タッチパネル用層間充填材料/ITO-PETフィルム構成体を作製した。このとき、ガラスとタッチパネル用層間充填材料との界面に気泡を封入した。次いで、この構成体を、70℃で30分、1気圧で真空ラミネータを用いて圧着してから、85℃、0.5MPaのオートクレーブで30分処理し、30℃以下にしてから解圧して取り出した。次いで、超高圧水銀灯を用いて、365nmの波長の光を10mW/cm2の照度で1200秒間照射して、ガラスとITO-PETフィルムとの層間がタッチパネル用層間充填材料で充填されている積層体を得た。
得られた積層体をデジタルマイクロスコープ(キーエンス社製)にて観察し、気泡が残存していなかった場合を「○」と、残存していた場合を「×」と評価した。
76mm×52mm、厚み1.0~1.2mmの白板ガラス(松浪硝子製S9112)に、外枠76mm×52mm、内枠56mm×32mmのロの字型の額縁状の厚み75μmの片面粘着剤を貼付し段差を作製した。
タッチパネル用層間充填材料を76mm×52mmにカットし、白板ガラスのロの字型の額縁状段差を貼付している面に添付し、更に、ITOがコーティングされたポリエチレンテレフタレートフィルム(ITO-PET、積水ナノコートテクノロジー社製)を76mm×52mmにカットし、タッチパネル用層間充填材料に添付した。それぞれ貼合する際にはできる限り気泡が入らない様にした。次いで、この構成体を、70℃で30分、1気圧で真空ラミネータを用いて圧着してから、85℃、0.5MPaのオートクレーブで30分処理し、30℃以下にしてから解圧して取り出した。次いで、超高圧水銀灯を用いて、365nmの波長の光を10mW/cm2の照度で1200秒間照射して、ガラスとITO-PETフィルムとの層間がタッチパネル用層間充填材料で充填されている積層体を得た。
得られた積層体をデジタルマイクロスコープ(キーエンス社製)にて観察し、段差の界面での気泡残存を確認できた場合を「×」と、気泡残存が確認できなかった場合を「○」と評価した。
76mm×52mm、厚み1.0~1.2mmの白板ガラス(松浪硝子製S9112)の表面に、モデル異物としてジビニルベンゼン系化合物からなる粒子径が40μmの微粒子(積水化学工業社製、ミクロパール)を30個/cm2の密度で均一に散布した。
タッチパネル用層間充填材料を76mm×52mmにカットし、白板ガラスのモデル異物を散布した面に添付し、更に、ITOがコーティングされたポリエチレンテレフタレートフィルム(ITO-PET、積水ナノコートテクノロジー社製)を76mm×52mmにカットし、タッチパネル用層間充填材料に添付した。それぞれ貼合する際にはできる限り気泡が入らない様にした。次いで、この構成体を、70℃で30分、1気圧で真空ラミネータを用いて圧着してから、85℃、0.5MPaのオートクレーブで30分処理し、30℃以下にしてから解圧して取り出した。次いで、超高圧水銀灯を用いて、365nmの波長の光を10mW/cm2の照度で1200秒間照射して、ガラスとITO-PETフィルムとの層間がタッチパネル用層間充填材料で充填されている積層体を得た。
次いで、得られた積層体を温度85℃、湿度85%の高温高湿条件下で250時間放置して、高温高湿処理を施した。
高温高湿処理後の構成体をデジタルマイクロスコープ(キーエンス社製)にて観察し、発泡が認められなかった場合を「○」と、発泡が認められた場合を「×」と評価した。
2 タッチパネル
3 表面保護パネル
4 偏光フィルム
5 加飾印刷部
Claims (11)
- ポリビニルアセタール、光ラジカル重合開始剤、及び、ラジカル重合性二重結合を有するモノマー又はオリゴマーを含有することを特徴とするポリビニルアセタール樹脂組成物。
- ポリビニルアセタールは、ポリビニルブチラールであることを特徴とする請求項1記載のポリビニルアセタール樹脂組成物。
- 光ラジカル重合開始剤は、ベンゾフェノンであることを特徴とする請求項1又は2記載のポリビニルアセタール樹脂組成物。
- 光ラジカル重合開始剤の含有量がポリビニルアセタール100重量部に対して0.1~5重量部であることを特徴とする請求項1、2又は3記載のポリビニルアセタール樹脂組成物。
- ラジカル重合性二重結合を有するモノマー又はオリゴマーは、分子内にラジカル重合性二重結合を2以上有する多官能モノマー又はオリゴマーであることを特徴とする請求項1、2、3又は4記載のポリビニルアセタール樹脂組成物。
- ラジカル重合性二重結合を有するモノマー又はオリゴマーの含有量がポリビニルアセタール100重量部に対して0.1~40重量部であることを特徴とする請求項1、2、3、4又は5記載のポリビニルアセタール樹脂組成物。
- 更に、可塑剤を含有することを特徴とする請求項1、2、3、4、5又は6記載のポリビニルアセタール樹脂組成物。
- 請求項1、2、3、4、5、6又は7に記載のポリビニルアセタール樹脂組成物からなることを特徴とする接着シート。
- タッチパネルと他の部材との層間又は前記タッチパネルを構成する複数の透明導電フィルムの層間を充填するために用いられるタッチパネル用層間充填材料であって、請求項1、2、3、4、5、6又は7記載のポリビニルアセタール樹脂組成物、又は、請求項8記載の接着シートからなることを特徴とするタッチパネル用層間充填材料。
- ポリビニルアセタールと可塑剤との合計の含有量が50重量%以上であることを特徴とする請求項9記載のタッチパネル用層間充填材料。
- 表面保護パネルとタッチパネルとの層間、タッチパネルと偏光フィルムとの層間、及び、タッチパネルを構成する複数の透明導電フィルムの層間からなる群から選択される少なくとも1種の層間が、請求項9又は10記載のタッチパネル用層間充填材料で充填されていることを特徴とする積層体。
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- 2016-10-06 US US15/765,629 patent/US20200270385A1/en not_active Abandoned
- 2016-10-06 EP EP16853697.7A patent/EP3360903B1/en active Active
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WO2022265073A1 (ja) * | 2021-06-18 | 2022-12-22 | 積水化学工業株式会社 | 粘着フィルム、及び積層体 |
WO2022265075A1 (ja) * | 2021-06-18 | 2022-12-22 | 積水化学工業株式会社 | 粘着フィルム、積層体、液晶ディスプレイ及び合わせガラス |
WO2022265077A1 (ja) * | 2021-06-18 | 2022-12-22 | 積水化学工業株式会社 | 粘着フィルム、積層体、液晶ディスプレイ及び合わせガラス |
Also Published As
Publication number | Publication date |
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US20200270385A1 (en) | 2020-08-27 |
EP3360903A4 (en) | 2019-05-08 |
JP6815868B2 (ja) | 2021-01-20 |
TWI767889B (zh) | 2022-06-21 |
US20230159689A1 (en) | 2023-05-25 |
TW201726795A (zh) | 2017-08-01 |
JPWO2017061545A1 (ja) | 2018-07-26 |
EP3360903A1 (en) | 2018-08-15 |
CN107614543A (zh) | 2018-01-19 |
KR20180068899A (ko) | 2018-06-22 |
EP3360903B1 (en) | 2022-11-02 |
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