WO2010140454A1 - 粘着剤層、粘着部材、その製造方法および画像表示装置 - Google Patents
粘着剤層、粘着部材、その製造方法および画像表示装置 Download PDFInfo
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- WO2010140454A1 WO2010140454A1 PCT/JP2010/058170 JP2010058170W WO2010140454A1 WO 2010140454 A1 WO2010140454 A1 WO 2010140454A1 JP 2010058170 W JP2010058170 W JP 2010058170W WO 2010140454 A1 WO2010140454 A1 WO 2010140454A1
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- pressure
- sensitive adhesive
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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
- C09J133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
-
- 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
- C09J133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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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
- C09J133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
- G02B5/3041—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks
- G02B5/305—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks including organic materials, e.g. polymeric layers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
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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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
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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
- C09J2433/00—Presence of (meth)acrylic polymer
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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
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249982—With component specified as adhesive or bonding agent
- Y10T428/249984—Adhesive or bonding component contains voids
Definitions
- the present invention relates to an adhesive layer obtained from a water-dispersed adhesive. Moreover, this invention relates to the adhesive member which has the said adhesive layer on a support base material, and its manufacturing method.
- the pressure-sensitive adhesive layer can be applied in various applications.
- the pressure-sensitive adhesive layer can be used as a pressure-sensitive adhesive member provided on one side or both sides of a supporting base material. It can be used as a double-sided pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer on both sides of the support substrate.
- a support base material in an adhesive member an optical film, a surface protection film base material, a separator, etc. can be used, for example.
- the optical film examples include a polarizing plate, a retardation plate, an optical compensation film, a brightness enhancement film, a prism sheet, a transparent conductive film used for a touch panel, and a laminate of these films.
- the pressure-sensitive adhesive member in which the pressure-sensitive adhesive layer is formed using an optical film as a supporting substrate is useful as a pressure-sensitive adhesive optical film, and is used in image display devices such as liquid crystal display devices, organic EL display devices, and PDPs.
- the surface protective film include various plastic films applied to the optical film and the like.
- an image display device such as a liquid crystal display device
- various optical films such as a polarizing plate and a retardation plate forming the device are bonded to an adherend such as a liquid crystal cell via an adhesive layer.
- the adhesive is preliminarily applied to one side of the optical film. Often provided as a layer.
- the adhesive layer is provided also in the surface protection film used in order to protect an optical film etc.
- the water-dispersed pressure-sensitive adhesive contains a surfactant for dispersing the pressure-sensitive adhesive component in water in addition to the pressure-sensitive adhesive component, the water-dispersed pressure-sensitive adhesive has the property of easily foaming and is obtained by the water-dispersed pressure-sensitive adhesive. In the adhesive layer, fine bubbles are mixed.
- Patent Documents 8 to 11 water-dispersed pressure-sensitive adhesives have been applied to applications that require coating appearance such as transparent tapes, industrial surface protection tapes, and semiconductor wafer processing tapes.
- a water-dispersed pressure-sensitive adhesive that can realize the applied appearance used has not been obtained.
- a pressure-sensitive adhesive layer having a good coating appearance is formed with a high yield from the viewpoint of production efficiency and the like even in a pressure-sensitive adhesive layer applied to a large-sized optical film. That is required. Therefore, it has been difficult to apply the water-dispersed pressure-sensitive adhesive for optical use.
- An object of the present invention is to provide a pressure-sensitive adhesive layer formed from a water-dispersed pressure-sensitive adhesive having a low environmental load, and exhibiting a high-quality coating appearance with no problem in fine bubble defects. .
- Another object of the present invention is to provide a pressure-sensitive adhesive member having the pressure-sensitive adhesive layer and a method for producing the pressure-sensitive adhesive layer, and to provide an image display device using a pressure-sensitive adhesive optical film as the pressure-sensitive adhesive member.
- the present invention is a pressure-sensitive adhesive layer formed by applying a water-dispersed pressure-sensitive adhesive composed of a dispersion in which at least a base polymer is dispersed and contained in water, and then drying.
- the pressure-sensitive adhesive layer does not contain bubbles having a maximum length exceeding 350 ⁇ m, and
- the present invention relates to a pressure-sensitive adhesive layer, wherein the number of bubbles having a maximum length of 50 to 350 ⁇ m on the surface of the pressure-sensitive adhesive layer is 1 / m 2 or less.
- the pressure-sensitive adhesive layer of the present invention is formed of a water-dispersed pressure-sensitive adhesive, it does not contain bubbles with a maximum length exceeding 350 ⁇ m, which is regarded as an appearance defect in optical applications. Appearance can be satisfied.
- the lower limit of the maximum length of bubbles not included in the pressure-sensitive adhesive layer is smaller, it is not recognized as an appearance defect. Therefore, the lower limit of the maximum length of bubbles preferably does not exceed 150 ⁇ m, and more preferably does not exceed 100 ⁇ m.
- the lower limit of the maximum length of bubbles not included in the adhesive layer is set to a small value depending on the application to which the adhesive layer is applied. For example, when an adhesive layer is applied to an optical film, it can be determined according to the size of the optical film. It is preferable to set the lower limit of the maximum length of the bubbles as the size of the optical film is reduced. For example, in the case of an optical film of a large size (20-42 inch size), it is preferable not to include bubbles having a maximum length exceeding 350 ⁇ m.
- the maximum length does not include bubbles exceeding 150 ⁇ m, and in the case of a small size (mobile) optical film, it is preferable that the maximum length does not include bubbles exceeding 100 ⁇ m.
- the number of bubbles having a maximum length of 50 to 350 ⁇ m on the surface of the pressure-sensitive adhesive layer is 1 / m 2 or less.
- the number of bubbles having a maximum length of 50 to 350 ⁇ m is preferably 1 / m 2 or less, more preferably 0.5 / m 2 or less on the surface of the pressure-sensitive adhesive layer. Further, it is preferably 0.1 piece / m 2 or less.
- the maximum length of the bubbles contained in the pressure-sensitive adhesive layer according to the number of bubbles can be set small according to the application to which the pressure-sensitive adhesive layer is applied, and the maximum length of the bubbles. Is preferably in the range of 50 to 150 ⁇ m, more preferably 50 to 100 ⁇ m, to satisfy the number of the bubbles.
- a (meth) acrylic polymer is suitable as the base polymer in the water-dispersed pressure-sensitive adhesive.
- the (meth) acrylic polymer that is the base polymer is preferably obtained by emulsion polymerization.
- a (meth) acrylic polymer obtained by emulsion polymerization is preferably used as the base polymer used for the water-dispersed pressure-sensitive adhesive.
- the present invention also relates to a pressure-sensitive adhesive layer formed of the water-dispersed pressure-sensitive adhesive.
- the adhesive member an adhesive optical film using an optical film as a supporting substrate is suitable.
- the present invention is a method for producing the adhesive member, A step (1) of performing a defoaming treatment of a water-dispersed adhesive comprising at least a dispersion in which a base polymer is dispersed and contained in water; A step (2) of applying a water-dispersed pressure-sensitive adhesive that has been subjected to the defoaming treatment step (1) to one or both sides of the support substrate; and A step (3) of drying the applied water-dispersed pressure-sensitive adhesive to form a pressure-sensitive adhesive layer; And the tank of the defoaming apparatus which performs the said defoaming process (1), and the pump set tank for supplying a water dispersion type adhesive to the said application
- the water-dispersed pressure-sensitive adhesive that has been subjected to the defoaming treatment step (1) has each pressure such that the pressure in the pump set tank and the connecting pipe is 1 kPa to 50 kPa lower than the pressure in the tank of the defoaming device. It is related with the manufacturing method of the adhesion member characterized by being set and conveying from the tank of a defoaming apparatus to a pump set tank.
- the present invention is a method for producing the adhesive member, Step (1) for defoaming a water-dispersed pressure-sensitive adhesive comprising a dispersion in which at least a base polymer is dispersed and contained in water
- Step (2) of applying a water-dispersed pressure-sensitive adhesive that has been subjected to the defoaming treatment step (1) to one or both sides of the support substrate and
- a tank of a defoaming apparatus that performs the defoaming treatment step (1) and a pump set tank for supplying a water-dispersed adhesive to the coating step (2) are connected via a buffer tank.
- the water-dispersed pressure-sensitive adhesive that has been subjected to the defoaming treatment step (1) has each pressure adjusted so that the pressure in the buffer tank and the connecting pipe is 1 kPa to 50 kPa lower than the pressure in the tank of the defoamer.
- the water dispersion type adhesive in the buffer tank sets each pressure so that the pressure in the pump set tank and the connecting pipe is 1 kPa to 50 kPa less than the pressure in the buffer tank, and from the buffer tank to the pump set tank. It is related with the manufacturing method of the adhesion member characterized by being conveyed.
- the coating step (2) and then the pressure-sensitive adhesive layer forming step (3) are performed.
- the water-dispersed pressure-sensitive adhesive has air bubbles removed in advance, and the defoamed water-dispersed pressure-sensitive adhesive is removed from the defoaming device to the pump set tank under reduced pressure. Then, the sheet is conveyed using the pressure difference through the decompression means.
- the defoaming device, the connecting pipe and the pump set tank are in a decompressed state, and air remains in the system when the water-dispersed adhesive is transported from the defoaming device to the pump set tank through the connecting pipe. Even in this case, it is possible to reliably prevent air from being mixed or dissolved as bubbles in the water-dispersed adhesive. Further, even when bubbles are remixed in the water-dispersed pressure-sensitive adhesive, it can be easily guided to the gas-liquid interface to be broken. In addition, since the water-dispersed pressure-sensitive adhesive is transported using the pressure difference, the transport amount of the water-dispersed pressure-sensitive adhesive can be easily adjusted.
- the pressure difference between the tanks is preferably in the range of 1 kPa to 50 kPa, and more preferably in the range of 5 kPa to 20 kPa. In the initial state (the state in which no water-dispersed adhesive is conveyed), the pressure difference in the tank may exceed the above range.
- the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive after the defoaming treatment step (1) is the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive before the defoaming treatment step (1). It is preferable that it is 10% or less.
- the defoaming treatment step (1) by controlling the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive to 15% or less before the treatment, bubbles generated in the pressure-sensitive adhesive layer can be greatly reduced.
- the dissolved oxygen concentration is preferably 10% or less, more preferably 8% or less, and even more preferably 5% or less before the treatment.
- the dissolved oxygen concentration of the water-dispersed adhesive applied in the application step (2) is preferably 3 mg / L or less.
- the dissolved oxygen concentration of the applied water-dispersed pressure-sensitive adhesive is preferably 2 mg / L or less, more preferably 1.5 mg / L or less.
- the present invention also relates to an image display device characterized by using at least one of the pressure-sensitive adhesive layer or the pressure-sensitive adhesive member.
- the pressure-sensitive adhesive layer of the present invention is formed from a high-viscosity water-dispersed pressure-sensitive adhesive, the pressure-sensitive adhesive layer exhibits a high-quality coating appearance without any problem with fine bubble defects.
- the pressure-sensitive adhesive layer is formed by applying the defoaming treatment step (1) to the water-dispersed pressure-sensitive adhesive, and then removing the defoamed water-dispersed pressure-sensitive adhesive from the defoaming device. It is obtained by carrying out a coating step (2) and then a pressure-sensitive adhesive layer forming step (3) after transporting to a tank using a pressure difference through a pressure reducing means under reduced pressure.
- Japanese Patent Application Laid-Open No. 2004-249215 discloses the dissolved oxygen concentration of at least one of the coating solution before degassing sent to the degassing device or the coating solution drained from the degassing device.
- a deaeration system configured to detect the detection unit and to control the deaeration control unit by the control unit based on the detection result of the dissolved oxygen concentration detection unit to adjust the deaeration degree of the deaeration device.
- 2000-26295 discloses that when starting the feeding of the coating liquid to the coating head, the inside of the liquid feeding system for supplying the coating liquid to the coating head is depressurized and then filled with the liquid sealing liquid.
- a liquid feeding method configured to extrude and replace the liquid seal liquid with a coating liquid is described.
- the coating liquid is continuously deaerated in-line via the deaerator.
- a method is limited to the case where the viscosity of the coating solution is generally low, which is less than 100 mPa ⁇ s, and the viscosity of the coating solution having a viscosity of 100 mPa ⁇ s or more, particularly 1000 mPa ⁇ s or more.
- the coating liquid deaerated and defoamed as described above is temporarily stored in a storage tank such as a buffer tank, and the stored coating liquid is pumped through a pump immediately before the coating is performed. After being conveyed to a set tank or the like, it is configured to be supplied to the coating head.
- the pressure-sensitive adhesive layer can be formed.
- the pressure-sensitive adhesive layer of the present invention is formed by applying a water-dispersed pressure-sensitive adhesive and then drying it.
- the water-dispersed pressure-sensitive adhesive is a dispersion in which a base polymer is dispersed and contained in water.
- the water-dispersed pressure-sensitive adhesive is an aqueous dispersion as described above, and can be suitably applied even when the viscosity is a high viscosity in the range of 100 mPa ⁇ s to 10000 mPa ⁇ s.
- the solid content concentration of the water-dispersed pressure-sensitive adhesive is usually about 1 to 70% by weight.
- a water-dispersed pressure-sensitive adhesive having such a high viscosity is suitable for forming a pressure-sensitive adhesive layer.
- the viscosity of the water-dispersed pressure-sensitive adhesive is preferably in the range of 1000 mPa ⁇ s to 5000 mPa ⁇ s.
- the viscosity value of the water-dispersed pressure-sensitive adhesive is a value measured using a HAAKE viscometer (Rheo Stress 1) at a temperature of 30 ° C. and a shear rate of 1 (1 / s).
- the water-dispersed adhesive is a dispersion in which at least a base polymer is dispersed and contained in water.
- a dispersion in which a base polymer is dispersed in the presence of a surfactant is usually used. If the base polymer is dispersed and contained in water, a self-dispersing base polymer is used. What is used as the dispersion liquid by self-dispersion can be used.
- examples of the base polymer in the dispersion include those obtained by polymerizing a monomer by emulsion polymerization or dispersion polymerization in the presence of a surfactant.
- the dispersion can be produced by emulsifying and dispersing a separately produced base polymer in water in the presence of an emulsifier.
- the polymer and the emulsifier are heated and melted in advance or without being heated and melted, and they and water are subjected to high shear using a mixer such as a pressure kneader, a colloid mill, and a high-speed stirring shaft.
- Various adhesives can be used as the water-dispersed adhesive, for example, rubber adhesives, acrylic adhesives, silicone adhesives, urethane adhesives, vinyl alkyl ether adhesives, polyvinyl alcohol adhesives. Examples thereof include a pressure-sensitive adhesive, a polyvinylpyrrolidone pressure-sensitive adhesive, a polyacrylamide-based pressure-sensitive adhesive, and a cellulose-based pressure-sensitive adhesive.
- An adhesive base polymer and a dispersing means are selected according to the type of the adhesive.
- the present invention is excellent in optical transparency, exhibits appropriate wettability, cohesiveness, and adhesive pressure-sensitive adhesive properties, and is excellent in weather resistance, heat resistance, and the like.
- a system adhesive is preferably used.
- the (meth) acrylic polymer that is the base polymer of the water-dispersed acrylic pressure-sensitive adhesive is obtained, for example, by emulsion polymerization of a monomer component mainly composed of (meth) acrylic acid alkyl ester in the presence of an emulsifier. Obtained as a copolymer emulsion.
- the (meth) acrylic acid alkyl ester refers to an acrylic acid alkyl ester and / or a methacrylic acid alkyl ester, and (meth) in the present invention has the same meaning.
- Examples of the (meth) acrylic acid alkyl ester constituting the main skeleton of the (meth) acrylic polymer include linear or branched alkyl groups having 1 to 18 carbon atoms.
- the alkyl group includes methyl group, ethyl group, propyl group, isopropyl group, butyl group, isobutyl group, amyl group, hexyl group, cyclohexyl group, heptyl group, 2-ethylhexyl group, isooctyl group, nonyl group, decyl group.
- alkyl groups preferably have an average carbon number of 3 to 9.
- (meth) acrylic acid alkyl ester containing an aromatic ring such as phenoxyethyl (meth) acrylate can be used.
- the (meth) acrylic acid alkyl ester containing an aromatic ring can be used by mixing a polymer obtained by polymerizing it with the above-mentioned (meth) acrylic polymer.
- the (meth) acrylic acid alkyl ester to be contained is preferably copolymerized with the (meth) acrylic acid alkyl ester.
- (meth) acrylic polymer one or more having a polymerizable functional group having an unsaturated double bond such as a (meth) acryloyl group or a vinyl group for the purpose of improving adhesiveness and heat resistance
- a polymerizable functional group having an unsaturated double bond such as a (meth) acryloyl group or a vinyl group for the purpose of improving adhesiveness and heat resistance
- copolymerized monomers include, for example, 2-hydroxyethyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate, (meth) acrylic acid 6 Hydroxyl-containing monomers such as hydroxyhexyl, 8-hydroxyoctyl (meth) acrylate, 10-hydroxydecyl (meth) acrylate, 12-hydroxylauryl (meth) acrylate and (4-hydroxymethylcyclohexyl) -methyl acrylate Carboxyl group-containing monomers such as (meth) acrylic acid, carboxyethyl (meth) acrylate, carboxypentyl (meth) acrylate, itaconic acid, maleic acid, fumaric acid and crotonic acid; acid anhydrides such as maleic anhydride and itaconic anhydride Monomer-containing monomer; Caprolac of acrylic acid Adducts such as styrene sulfonic acid
- (meth) acrylamide, N, N-dimethyl (meth) acrylamide, N-butyl (meth) acrylamide, N-methylol (meth) acrylamide, N-methylolpropane (meth) acrylamide, N-hydroxyethyl (meth) acrylamide (N-substituted) amide monomers such as: (meth) acrylic acid aminoethyl, (meth) acrylic acid N, N-dimethylaminoethyl, (meth) acrylic acid t-butylaminoethyl alkyl (meth) acrylate Aminoalkyl monomers; (meth) acrylic acid alkoxyalkyl monomers such as methoxyethyl (meth) acrylate and ethoxyethyl (meth) acrylate; N- (meth) acryloyloxymethylenesuccinimide and N- (meth) acryloyl-6 -Oxyhexamethyl
- Further modifying monomers include vinyl acetate, vinyl propionate, N-vinyl pyrrolidone, methyl vinyl pyrrolidone, vinyl pyridine, vinyl piperidone, vinyl pyrimidine, vinyl piperazine, vinyl pyrazine, vinyl pyrrole, vinyl imidazole, vinyl oxazole, vinyl morpholine, N- Vinyl monomers such as vinylcarboxylic amides, styrene, ⁇ -methylstyrene, N-vinylcaprolactam; cyanoacrylate monomers such as acrylonitrile and methacrylonitrile; epoxy group-containing acrylic monomers such as glycidyl (meth) acrylate; (Meth) acrylic acid polyethylene glycol, (meth) acrylic acid polypropylene glycol, (meth) acrylic acid methoxyethylene glycol, (meth) acrylic acid meso Glycol acrylic ester monomers such as xypolypropylene glycol; acrylic ester monomers such as
- copolymerization monomer examples include ethylene glycol di (meth) acrylate, diethylene glycol di (meth) acrylate, tripropylene glycol di (meth) acrylate, tetraethylene glycol di (meth) acrylate, and 1,6-hexanediol di (meta).
- the (meth) acrylic polymer is mainly composed of (meth) acrylic acid alkyl ester in the weight ratio of all constituent monomers, and the proportion of the copolymerization monomer in the (meth) acrylic polymer is not particularly limited,
- the ratio of the copolymerization monomer is preferably about 0 to 20%, about 0.1 to 15%, and more preferably about 0.1 to 10% in the weight ratio of all the constituent monomers.
- hydroxyl group-containing monomers and carboxyl group-containing monomers are preferably used from the viewpoint of adhesion and durability.
- These copolymerization monomers serve as reaction points with the crosslinking agent when the water-dispersed adhesive contains a crosslinking agent. Since a hydroxyl group-containing monomer, a carboxyl group-containing monomer, and the like are rich in reactivity with an intermolecular crosslinking agent, they are preferably used for improving the cohesiveness and heat resistance of the resulting pressure-sensitive adhesive layer.
- a hydroxyl group-containing monomer and a carboxyl group-containing monomer are contained as the copolymerization monomer, these copolymerization monomers are used in the proportion of the copolymerization monomer, but the carboxyl group-containing monomer is 0.1 to 10% by weight and the hydroxyl group
- the content of the monomer is preferably 0.01 to 2% by weight.
- the carboxyl group-containing monomer is more preferably 0.2 to 8% by weight, and further preferably 0.6 to 6% by weight.
- the hydroxyl group-containing monomer is more preferably 0.03 to 1.5% by weight, and even more preferably 0.05 to 1% by weight.
- anionic emulsifiers and nonionic emulsifiers used in emulsion polymerization can be used without particular limitation.
- anionic emulsifiers such as sodium lauryl sulfate, ammonium lauryl sulfate, sodium dodecylbenzene sulfonate, sodium polyoxyethylene alkyl ether sulfate, sodium polyoxyethylene alkyl phenyl ether sulfate, polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, etc.
- Nonionic emulsifiers and the like are examples of the like.
- a radical polymerizable emulsifier in which a reactive functional group such as a propenyl group, an allyl group or a (meth) acryloyl group is introduced into the emulsifier.
- Radical polymerizable emulsifiers are described, for example, in JP-A-4-50204 and JP-A-4-53802.
- the amount of the emulsifier used is not particularly limited, but is preferably about 0.3 to 5 parts by weight with respect to 100 parts by weight of the monomer component mainly composed of the (meth) acrylic acid alkyl ester.
- the amount of emulsifier used is more preferably 0.7 to 4 parts by weight.
- Emulsion polymerization of the monomer component is carried out by a conventional method using an appropriate polymerization initiator in the presence of the emulsifier to prepare an aqueous dispersion of an acrylic polymer.
- Emulsion polymerization is performed by general batch polymerization, continuous dropping polymerization, divided dropping polymerization, or the like.
- the polymerization temperature can be about 30 to 90 ° C.
- polymerization initiator examples include 2,2′-azobisisobutyronitrile, 2,2′-azobis (2-amidinopropane) dihydrochloride, 2,2′-azobis (N, N′-dimethyleneisobutyl). Azo compounds such as amidine), 2,2′-azobis (2-methylpropionamidine) dihydrochloride, 2,2′-azobis [N- (2-carboxyethyl) -2-methylpropionamidine] hydrate, potassium persulfate And persulfates such as ammonium persulfate, peroxides such as benzoyl peroxide and t-butyl hydroperoxide, and redox initiators such as persulfate and sodium bisulfite.
- an appropriate chain transfer agent typified by mercaptans, mercaptopropionic acid esters and the like may be used as necessary to adjust the molecular weight of the resulting polymer.
- the (meth) acrylic polymer of the present invention usually has a weight average molecular weight in the range of 1 million to 3 million. In view of durability, particularly heat resistance, it is preferable to use those having a weight average molecular weight of 1,000,000 to 2,500,000. Further, it is more preferably 1.7 million to 2.5 million, and further preferably 1.8 million to 2.5 million. When the weight average molecular weight is less than 1,000,000, it is not preferable from the viewpoint of heat resistance. Moreover, when a weight average molecular weight becomes larger than 3 million, it is unpreferable also at the point which bonding property and adhesive force fall.
- the weight average molecular weight is a value measured by GPC (gel permeation chromatography) and calculated in terms of polystyrene.
- the water-dispersed pressure-sensitive adhesive can be used as a radiation curable pressure-sensitive adhesive.
- a radiation curable base polymer having a radiation curable functional group such as a (meth) acryloyl group or a vinyl group is used as the base polymer of the pressure-sensitive adhesive.
- a reactive diluent may be further blended with the base polymer.
- a radiation curable type for example, it contains a monomer that forms a base polymer or a partial polymer thereof, and forms a pressure-sensitive adhesive layer that contains the base polymer by irradiation with radiation such as an electron beam or ultraviolet rays. (In this case, a monomer that forms the base polymer or a partial polymer thereof is used as the base polymer).
- the radiation curable pressure-sensitive adhesive can contain a polymerization initiator.
- the radiation curable base polymer has a base polymer having a functional group a, a functional group b reactive with the functional group a, and a polymerizable carbon-carbon double bond such as a (meth) acryloyl group or a vinyl group. Obtained by reacting a compound.
- the functional group a and the functional group b include a carboxyl group, an acid anhydride group, a hydroxy group, an amino group, an epoxy group, an isocyanate group, an aziridine group, and the like. You can select and use. Even in the case of the radiation curable type, an acrylic polymer is preferable as the base polymer of the pressure-sensitive adhesive.
- a radically polymerizable monomer and / or oligomer component having at least one radiation-curable functional group is used.
- the water-dispersed pressure-sensitive adhesive of the present invention includes a crosslinking agent in addition to the above base polymer (in the case of radiation curable type, in addition to the base polymer, a monomer forming the base polymer or a partial polymer thereof, a reactive diluent). Can be contained.
- the crosslinking agent used when the water-dispersed pressure-sensitive adhesive is a water-dispersed acrylic pressure-sensitive adhesive include isocyanate-based crosslinking agents, epoxy-based crosslinking agents, oxazoline-based crosslinking agents, aziridine-based crosslinking agents, carbodiimide-based crosslinking agents, and metal chelates. Commonly used materials such as a system cross-linking agent can be used. These crosslinking agents have the effect of reacting with a functional group introduced into the polymer and crosslinking by using a functional group-containing monomer.
- the blending ratio of the base polymer and the crosslinking agent is not particularly limited, but is usually blended at a ratio of about 10 parts by weight or less of the crosslinking agent (solid content) with respect to 100 parts by weight of the base polymer (solid content).
- the blending ratio of the crosslinking agent is preferably 0.001 to 10 parts by weight, more preferably about 0.01 to 5 parts by weight.
- the water-dispersed pressure-sensitive adhesive of the present invention includes a tackifier, a plasticizer, a glass fiber, a glass bead, a metal powder, a filler composed of other inorganic powders, a pigment, a colorant, if necessary.
- Fillers, antioxidants, ultraviolet absorbers, silane coupling agents, and the like, and various additives can be appropriately used without departing from the object of the present invention.
- These additives can also be blended as an emulsion.
- the pressure-sensitive adhesive layer of the present invention is formed from the above-mentioned water-dispersed pressure-sensitive adhesive.
- the applied water-dispersed pressure-sensitive adhesive is first subjected to a defoaming step (1).
- the step (2) of applying the water-dispersed pressure-sensitive adhesive in which the defoaming treatment step (1) has been applied to one side or both sides of the supporting substrate, and the applied water-dispersed pressure-sensitive adhesive are dried and adhered.
- Step (3) for forming the agent layer is sequentially performed.
- the tank of the defoaming apparatus which performs the said defoaming process process (1), and a water dispersion type
- the pump set tank for supplying the pressure-sensitive adhesive is connected via a connecting pipe, and the water-dispersed pressure-sensitive adhesive subjected to the defoaming treatment step (1) uses the pressure difference in each tank. Then, it is conveyed from the defoaming device to the pump set tank.
- the tank of the defoaming device and the pump set tank can be connected via the buffer tank and the connecting pipe. In this case, the water-dispersed adhesive is transferred from the defoaming device to the pump set tank. It is conveyed from the defoaming device to the pump set tank using the pressure difference inside.
- FIG. 1 is a schematic explanatory view showing an adhesive application system for a water-dispersed adhesive according to this embodiment.
- a tank and a pump set tank of a defoaming device are connected via a buffer tank and a connecting pipe. This is the case.
- FIG. 1 shows a case where one buffer tank is provided, a plurality of buffer tanks can be provided.
- the buffer tanks are connected via a connecting pipe, and the buffer tank and the connecting pipe in the connecting pipe are transported more than the pressure of the buffer tank that transports the water-dispersed adhesive.
- Each pressure is set so that the pressure becomes 1 kPa to 50 kPa, and the water-dispersed pressure-sensitive adhesive is conveyed using the pressure difference in each buffer tank as described above.
- an adhesive application system S basically includes a defoaming apparatus 1 for performing defoaming processing of a water-dispersed adhesive 2 containing an adhesive charged in a sealed tank 11 in a batch mode, and a sealed tank.
- the buffer tank 3 having a sealed tank 31 for temporarily storing the water-dispersed adhesive 2 defoamed in the tank 11, and the water-dispersed adhesive 2 conveyed from the sealed tank 31 of the buffer tank 3 are stored for application.
- a pump set tank 5 having a closed tank 51 to be fed, a liquid feed pump 92 for feeding the water-dispersed adhesive 2 from the sealed tank 51 of the pump set tank 5 to the coating device 94 through the filter 93, and the defoaming device 1
- the sealed tank 11 of the defoaming device 1 and the sealed tank 31 of the buffer tank 3 are connected via a connecting pipe 4, and the drain valve 14 is provided on the side of the sealed tank 11 via the connecting pipe 4.
- An open / close valve 41 is interposed on the side of the sealed tank 31 of the buffer tank 3.
- the sealed tank 31 of the buffer tank 3 and the sealed tank 51 of the pump set tank 5 are connected via a connecting pipe 6, and the drain pipe is connected to the sealed tank 31 side of the buffer tank 3 through the connecting pipe 6.
- an open / close valve 61 is interposed on the closed tank 51 side of the valve 33 and the pump set tank 5.
- a drain valve 53 is interposed on the downstream side of the pump set tank 5 and connected to the pump 92.
- the sealed tank 11 of the defoaming device 1 is connected to the vacuum pump 7 by a suction pipe 8 via a vacuum valve 16, and the sealed tank 31 of the buffer tank 3 is connected to a suction pipe via a vacuum valve 35. 8 is connected to the vacuum pump 7. Further, the sealed tank 51 of the pump set tank 5 is connected to the vacuum pump 7 by a suction pipe 8 through a vacuum valve 55.
- the defoaming apparatus 1 has a sealed tank 11, and a stirring blade 12 for stirring the water-dispersed adhesive 2 is disposed in the sealed tank 11.
- a pressure gauge 13 At the upper part of the closed tank 11, a pressure gauge 13, a leak valve 15, and a vacuum valve 16 interposed in the suction pipe 8 are provided.
- the pressure in the closed tank 11 in the defoaming device 1 is adjusted by operating and adjusting the opening degree of the leak valve 15 and the vacuum valve 16.
- a charge tank 91 for supplying the water-dispersed adhesive 2 to the sealed tank 11 is connected to the sealed tank 11 of the defoaming device 1 via a connecting pipe 96, and is supplied from the charge tank 91 to the sealed tank 11.
- the amount of the water-dispersed pressure-sensitive adhesive 2 is adjusted by controlling the opening / closing of the opening / closing valve 95.
- the buffer tank 3 has a sealed tank 31, and a pressure gauge 32, a leak valve 34, and a vacuum valve 35 interposed in the suction pipe 8 are provided above the sealed tank 31.
- the pressure in the sealed tank 31 is adjusted by manipulating and adjusting the opening degree of the leak valve 34 and the vacuum valve 35.
- the pump set tank 5 has a sealed tank 51, and a pressure gauge 52, a leak valve 54, and a vacuum valve 55 interposed in the suction pipe 8 are provided above the sealed tank 51.
- the pressure in the sealed tank 51 is adjusted by operating and adjusting the opening degree of the leak valve 54 and the vacuum valve 55.
- FIG. 2 is a flowchart showing processing operations performed in the adhesive application system.
- the defoaming process (1) of the water dispersion-type adhesive 2 is performed in the defoaming apparatus 1 (S2).
- the vacuum valve 16 is opened, and the other leak valve 15, open / close valve 95, and drain valve 14 are closed.
- the inside of the closed tank 11 is depressurized by the vacuum pump 7 and the stirring blade 12 is rotated. Thereby, the defoaming process of the water dispersion-type adhesive 2 is performed.
- the defoaming treatment step (1) is performed by depressurizing the inside of the sealed tank 11 of the defoaming operation 1 to about 10 kPa or less, preferably 5 kPa or less, more preferably 2 kPa or less.
- the rotation of the stirring blade 12 is stopped, the opening degree of the leak valve 15 is adjusted, and the pressure in the sealed tank 11 is adjusted to a predetermined set pressure (S3). Thereafter, all the valves are closed and the inside of the defoaming apparatus 1 is held in a closed system.
- the vacuum valve 35 and the opening / closing valve 41 provided in the sealed tank 31 constituting the buffer tank 3 are opened, and the sealed tank 31 and the connecting pipe 4 are decompressed via the vacuum pump 7.
- the absolute pressure is 50 kPa or less, preferably 20 kPa or less, more preferably 7 kPa or less.
- the saturated vapor pressure differs depending on the properties of the water-dispersed adhesive 2, it is necessary to set the pressure in the liquid-feeding system so that the water-dispersed adhesive 2 does not boil depending on the temperature at the time of liquid feeding. There is.
- the inside of the sealed tank 31 and the connecting pipe 4 is adjusted to a predetermined set pressure (S4).
- the drain valve 14 interposed in the connecting pipe 4 is opened on the downstream side of the sealed tank 11.
- a pressure difference is generated between the sealed tank 11 of the defoaming device 1 and the sealed tank 31 and the connecting pipe 4 of the buffer tank 3, and water is dispersed from the sealed tank 11 to the sealed tank 31 based on the pressure difference.
- the conveyance of the mold pressure-sensitive adhesive 2 is started (S5).
- the pressure difference between the upstream portion and the downstream portion of the liquid feeding becomes an important factor for controlling the liquid feeding flow rate.
- it is preferably in the range of 1 kPa to 50 kPa, and more preferably in the range of 5 kPa to 20 kPa.
- the opening degree of the leak valve 15 on the defoaming device 1 side and the leak valve 34 on the buffer tank 3 side are adjusted to thereby adjust the sealed tank 11 and the buffer tank 3 of the defoaming device 1.
- the closed tank 31 is adjusted to a predetermined set pressure (S6).
- S6 a predetermined set pressure
- the drain valve 14 and the opening / closing valve 41 are closed before the water-dispersed pressure-sensitive adhesive 2 is completely removed from the sealed tank 11. Thereby, it is possible to prevent bubbles from being mixed due to the air flow generated when the water-dispersed pressure-sensitive adhesive 2 is completely removed.
- the closed tank 31 may be open or closed. Even in the case of a closed system, the inside of the closed tank 31 of the buffer tank 3 may be at normal pressure or at reduced pressure. In addition, if the inside of the airtight tank 31 is a pressure-reduced state, stationary defoaming can be promoted.
- the vacuum valve 55 and the opening / closing valve 61 of the sealed tank 51 constituting the pump set tank 5 are opened, and the sealed tank 51 and the connecting pipe 6 are decompressed via the vacuum pump 7. Further, by operating / adjusting the opening degree of the leak valve 54, the inside of the sealed tank 51 and the connecting pipe 6 is adjusted to a predetermined set pressure (S7). In this adjusted state, the drain valve 33 interposed in the connecting pipe 6 is opened on the downstream side of the sealed tank 31. At this time, a pressure difference is generated between the sealed tank 31, the sealed tank 51, and the connecting pipe 6, and the conveyance of the water-dispersed adhesive 2 from the sealed tank 31 to the sealed tank 51 is started based on the pressure difference. (S8).
- the pressure difference between the upstream portion and the downstream portion of the liquid feeding is preferably in the range of 1 kPa to 50 kPa, and more preferably in the range of 5 kPa to 20 kPa.
- the opening degree of the leak valve 34 on the buffer tank 3 side and the leak valve 54 on the pump set tank 5 side are adjusted, so that the sealed tank 31 and the pump set tank 5 of the buffer tank 3 are adjusted.
- the inside of the closed tank 51 is adjusted to a predetermined set pressure.
- the drain valve 33 and the open / close valve 61 are closed before the water-dispersed pressure-sensitive adhesive 2 is completely removed from the sealed tank 31. Thereby, it is possible to prevent bubbles from being mixed due to the air flow generated when the water-dispersed pressure-sensitive adhesive 2 is completely removed.
- the drain valve 53 is opened and the liquid feed pump 92 is driven.
- the water-dispersed pressure-sensitive adhesive 2 is conveyed from the liquid feed pump 92 to the coating device 94 through the filter 93.
- a step (2) of applying a water-dispersed pressure-sensitive adhesive to one side or both sides of a supporting substrate, and then a step of drying the applied water-dispersed pressure-sensitive adhesive to form a pressure-sensitive adhesive layer (3). ) Is applied (S9).
- the water-dispersed pressure-sensitive adhesive 2 is transported to the coating device 94 by first flowing water through the filter 93 to remove bubbles in the filter 93, and then sealing the water-dispersed pressure-sensitive adhesive 2 for about 1 to 3 hours. It is preferable to carry out after circulating in the tank 51 and replacing the water in the filter 93 with the water-dispersed adhesive 2.
- the circulation of the water-dispersed pressure-sensitive adhesive 2 is provided with a valve in a liquid feeding pipe connecting the filter 93 and the coating device 94, and separated from the liquid feeding pipe into the sealed tank 51.
- a circulation pipe to be connected can be provided, and circulation can be performed by opening and closing the valve, or a removable liquid feeding pipe can be directly connected to the sealed tank 51.
- the operation of the vacuum pump 7 and various valves in the system may be performed manually after checking the pointers of the pressure gauges 13, 32, 52, or the pointers of the pressure gauges 13, 32, 52. It may be automatically performed by a remote instruction by the control based on. Further, the number of vacuum pumps 7 may be one or plural.
- the reason for paying attention to the dissolved oxygen concentration in the water-dispersed pressure-sensitive adhesive 2 is that when air is dissolved in the water-dispersed pressure-sensitive adhesive 2, air is generated as bubbles when the water-dispersed pressure-sensitive adhesive 2 is dried. This is because various problems occur due to the bubbles, and it is necessary to strictly control the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive 2 during the period from defoaming to coating. Note that, when the amount of air dissolved in the water-dispersed pressure-sensitive adhesive 2 is quantified, the amount of air dissolved in the water-dispersed pressure-sensitive adhesive 2 is generally expressed using the dissolved oxygen concentration.
- the dissolved oxygen concentration in the water-dispersed pressure-sensitive adhesive 2 is measured before the defoaming process step (1) is performed in the defoaming apparatus 1 (before defoaming), after the defoaming process is performed (after defoaming), and the buffer. It is measured after being transferred to the closed tank 31 of the tank 3 (after transfer). Moreover, the dissolved oxygen concentration of the water dispersion-type adhesive 2 apply
- the measurement of the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive 2 in the present invention is specifically according to the description of the examples.
- a dissolved oxygen measuring device 100 is disposed at the bottom of the sealed tank 11 of the defoaming device 1, and the water dispersion type adhesive is placed in the sealed tank 11 through the dissolved oxygen measuring device 100.
- the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive 2 can be measured before defoaming in which the agent 2 is charged and after the water-dispersed pressure-sensitive adhesive 2 is defoamed.
- the measurement of the dissolved oxygen concentration of the water dispersion-type adhesive 2 may take out the water dispersion-type adhesive 2 as a sample out of the system before defoaming and after defoaming, and may measure it with a measuring device.
- a dissolved oxygen measuring device 101 is disposed at the bottom of the sealed tank 31 of the buffer tank 3, and the water-dispersed adhesive 2 is buffered through the dissolved oxygen measuring device 101.
- the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive 2 after being transferred to the tank 3 can be measured.
- the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive 2 may be measured with a measuring instrument after taking the water-dispersed pressure-sensitive adhesive 2 out of the system as a sample.
- a dissolved oxygen measuring device 102 is disposed at the bottom of the sealed tank 51 of the pump set tank 5, and the dissolved oxygen measuring device 102 is passed through the dissolved oxygen measuring device 102 before the application step (2).
- the dissolved oxygen concentration before and after circulation of the filter of the water-dispersed pressure-sensitive adhesive 2 can be measured.
- a plurality of water-dispersed pressure-sensitive adhesive samples are extracted before the coating step (2), and the dissolved oxygen concentration of each water-dispersed pressure-sensitive adhesive sample and the final dissolved oxygen concentration are measured after the coating step (2). can do.
- an adhesive layer is formed on the support substrate.
- Various materials can be used for the support substrate, and examples thereof include an optical film, a surface protective film substrate, and a separator.
- the water-dispersed adhesive is applied to the separator and dried to form an adhesive layer, whereby an adhesive member is obtained.
- the adhesive layer formed on the separator is transferred to an optical film or the like, or the water-dispersed adhesive is applied to an optical film or the like and dried to form an adhesive layer. It is produced by a method of directly forming on an optical film or the like.
- Various methods are used for the coating step (2). Specifically, for example, roll coat, kiss roll coat, gravure coat, reverse coat, roll brush, spray coat, dip roll coat, bar coat, knife coat, air knife coat, curtain coat, lip coat, die coater, etc. Examples thereof include an extrusion coating method.
- the drying temperature eg 40 to 150 ° C.
- the drying time 20 seconds to 30 minutes
- the thickness of the pressure-sensitive adhesive layer is not particularly limited, and is, for example, about 1 to 100 ⁇ m.
- the thickness is preferably 5 to 50 ⁇ m, more preferably 10 to 30 ⁇ m.
- the pressure-sensitive adhesive layer preferably has a total light transmittance in a usable wavelength region of 10% or more and a haze of 75% or less as measured by the following method.
- the total light transmittance of the pressure-sensitive adhesive layer measured by the following method is 10% or more and the haze is 75% or less, it is easy to recognize the appearance defect due to bubbles. In optical applications, it is desirable that the total light transmittance is high and the haze is small.
- the total light transmittance is preferably 14% or more, more preferably 18% or more.
- the haze is preferably 65% or less.
- ⁇ Total light transmittance and haze in usable light wavelength range> Laminated structure (polarizing plate / adhesive layer) in which a 100 ⁇ m thick polarizing plate (manufactured by Nitto Denko Corporation, TEG-DU) is bonded to one surface of the pressure sensitive adhesive layer (thickness: 23 ⁇ m) to be measured ), A total light transmittance (%): JISK-7361 and haze (%): JIS K-7136 were measured using a haze meter HM-150 type (manufactured by Murakami Color Research Laboratory Co., Ltd.).
- constituent material of the separator examples include, for example, plastic films such as polyethylene, polypropylene, polyethylene terephthalate, and polyester films, porous materials such as paper, cloth, and nonwoven fabric, nets, foam sheets, metal foils, and laminates thereof.
- plastic films such as polyethylene, polypropylene, polyethylene terephthalate, and polyester films
- porous materials such as paper, cloth, and nonwoven fabric, nets, foam sheets, metal foils, and laminates thereof.
- a thin film can be used, but a plastic film is preferably used because of its excellent surface smoothness.
- the plastic film is not particularly limited as long as it can protect the pressure-sensitive adhesive layer.
- a polyethylene film, a polypropylene film, a polybutene film, a polybutadiene film, a polymethylpentene film, a polyvinyl chloride film, and a vinyl chloride co-polymer are used.
- examples thereof include a polymer film, a polyethylene terephthalate film, a polybutylene terephthalate film, a polyurethane film, and an ethylene-vinyl acetate copolymer film.
- the thickness of the separator is usually about 5 to 200 ⁇ m, preferably about 5 to 100 ⁇ m.
- mold release and antifouling treatment with a silicone type, fluorine type, long chain alkyl type or fatty acid amide type release agent, silica powder, etc., coating type, kneading type, vapor deposition type It is also possible to carry out antistatic treatment such as.
- the release property from the pressure-sensitive adhesive layer can be further improved by appropriately performing a release treatment such as silicone treatment, long-chain alkyl treatment, or fluorine treatment on the surface of the separator.
- the pressure-sensitive adhesive layer When the pressure-sensitive adhesive layer is exposed, the pressure-sensitive adhesive layer may be protected with a separator until practical use.
- seat which carried out the peeling process used in preparation of said adhesive member can be used as a separator of an adhesive optical film as it is, and can simplify in the surface of a process.
- the support substrate is a surface protective film substrate or an optical film
- an anchor layer is formed on the surface of the optical film in order to improve adhesion between the pressure-sensitive adhesive layer, corona treatment
- the pressure-sensitive adhesive layer can be formed after various easy adhesion treatments such as plasma treatment. Moreover, you may perform an easily bonding process on the surface of an adhesive layer.
- an anchor agent selected from polyurethane, polyester, and polymers containing an amino group in the molecule is preferably used, and polymers containing an amino group in the molecule are particularly preferred.
- Polymers containing an amino group in the molecule ensure good adhesion because the amino group in the molecule exhibits an interaction such as a reaction or ionic interaction with the carboxyl group in the pressure-sensitive adhesive.
- polymers containing an amino group in the molecule include polymers of amino-containing group-containing monomers such as polyethyleneimine, polyallylamine, polyvinylamine, polyvinylpyridine, polyvinylpyrrolidine, and dimethylaminoethyl acrylate.
- the same material as the separator can be exemplified.
- the surface of the plastic film can be appropriately roughened or provided with a release treatment layer.
- the optical film one used for forming an image display device such as a liquid crystal display device is used, and the type thereof is not particularly limited.
- the optical film includes a polarizing plate.
- a polarizing plate having a transparent protective film on one or both sides of a polarizer is generally used.
- the polarizer is not particularly limited, and various types can be used.
- polarizers include dichroic iodine and dichroic dyes on hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, and ethylene / vinyl acetate copolymer partially saponified films.
- hydrophilic polymer films such as polyvinyl alcohol films, partially formalized polyvinyl alcohol films, and ethylene / vinyl acetate copolymer partially saponified films.
- examples thereof include polyene-based oriented films such as those obtained by adsorbing substances and uniaxially stretched, polyvinyl alcohol dehydrated products and polyvinyl chloride dehydrochlorinated products.
- a polarizer composed of a polyvinyl alcohol film and a dichroic material such as iodine is preferable.
- the thickness of these polarizers is not particularly limited, but is generally about 5 to 80 ⁇ m.
- a polarizer in which a polyvinyl alcohol film is dyed with iodine and uniaxially stretched can be prepared, for example, by dyeing polyvinyl alcohol in an aqueous solution of iodine and stretching it 3 to 7 times the original length. If necessary, it can be immersed in an aqueous solution such as potassium iodide which may contain boric acid, zinc sulfate, zinc chloride or the like. Further, if necessary, the polyvinyl alcohol film may be immersed in water and washed before dyeing.
- Stretching may be performed after dyeing with iodine, may be performed while dyeing, or may be dyed with iodine after stretching.
- the film can be stretched even in an aqueous solution such as boric acid or potassium iodide or in a water bath.
- thermoplastic resin excellent in transparency, mechanical strength, thermal stability, moisture barrier property, isotropy and the like is used.
- thermoplastic resins include cellulose resins such as triacetyl cellulose, polyester resins, polyethersulfone resins, polysulfone resins, polycarbonate resins, polyamide resins, polyimide resins, polyolefin resins, (meth) acrylic resins, cyclic Examples thereof include polyolefin resins (norbornene resins), polyarylate resins, polystyrene resins, polyvinyl alcohol resins, and mixtures thereof.
- a transparent protective film is bonded to one side of the polarizer by an adhesive layer.
- thermosetting resin such as a system or an ultraviolet curable resin
- a thermosetting resin such as a system or an ultraviolet curable resin
- the additive include an ultraviolet absorber, an antioxidant, a lubricant, a plasticizer, a mold release agent, an anti-coloring agent, a flame retardant, a nucleating agent, an antistatic agent, a pigment, and a coloring agent.
- the content of the thermoplastic resin in the transparent protective film is preferably 50 to 100% by weight, more preferably 50 to 99% by weight, still more preferably 60 to 98% by weight, and particularly preferably 70 to 97% by weight. .
- content of the said thermoplastic resin in a transparent protective film is 50 weight% or less, there exists a possibility that the high transparency etc. which a thermoplastic resin originally has cannot fully be expressed.
- an optical film for example, it is used for forming a liquid crystal display device such as a reflection plate, an anti-transmission plate, a retardation plate (including wavelength plates such as 1/2 and 1/4), a visual compensation film, and a brightness enhancement film. And an optical layer that may be formed. These can be used alone as an optical film, or can be laminated on the polarizing plate for practical use and used as one layer or two or more layers.
- An optical film in which the optical layer is laminated on a polarizing plate can be formed by a method of sequentially laminating separately in the manufacturing process of a liquid crystal display device or the like.
- an appropriate adhesive means such as an adhesive layer can be used for the lamination.
- their optical axes can be set at an appropriate arrangement angle in accordance with the target phase difference characteristic.
- the pressure-sensitive adhesive optical film of the present invention can be preferably used for forming various image display devices such as a liquid crystal display device.
- the liquid crystal display device can be formed according to the conventional method. That is, a liquid crystal display device is generally formed by appropriately assembling components such as a display panel such as a liquid crystal cell, an adhesive optical film, and an illumination system as required, and incorporating a drive circuit. There is no particular limitation except that the pressure-sensitive adhesive optical film according to the present invention is used.
- the liquid crystal cell any type such as a TN type, STN type, ⁇ type, VA type, IPS type, or the like can be used.
- Appropriate liquid crystal display devices such as a liquid crystal display device in which an adhesive optical film is disposed on one side or both sides of a display panel such as a liquid crystal cell, and a lighting system using a backlight or a reflecting plate can be formed.
- the optical film by this invention can be installed in the one side or both sides of display panels, such as a liquid crystal cell.
- optical films When optical films are provided on both sides, they may be the same or different.
- a single layer or a suitable part such as a diffusing plate, an antiglare layer, an antireflection film, a protective plate, a prism array, a lens array sheet, a light diffusing plate, a backlight, etc. Two or more layers can be arranged.
- Example 1 Pre-emulsion preparation
- a container 92 parts of butyl acrylate, 6 parts of methacrylic acid, 2 parts of mono [poly (propylene oxide) methacrylate] phosphate (average polymerization degree of propylene oxide of about 5.0), 3-methacryloyloxypropyl-trimethoxysilane 0.03 part (KBM-503, manufactured by Shin-Etsu Chemical Co., Ltd.) was added and mixed to prepare a mixture of reaction components.
- KBM-503 manufactured by Shin-Etsu Chemical Co., Ltd.
- Defoaming treatment was performed for 30 minutes for the water-dispersed pressure-sensitive adhesive 2 charged in the sealed tank 11.
- the vacuum valve 16 is opened, all other valves connected to the defoaming device 1 are closed, the internal pressure of the sealed tank 11 is set to 3 kPa, and the stirring blade 12 is rotated.
- Vacuum degassing was performed.
- the water-dispersed pressure-sensitive adhesive 2 was sampled, and the dissolved oxygen concentration after defoaming was measured via a dissolved oxygen concentration meter. As a result, it was 0.41 mg / L.
- the dissolved oxygen concentration (0.41 mg / L) after defoaming is 7.13% of the dissolved oxygen concentration (5.75 mg / L) before defoaming, and is reduced to 10% or less before defoaming.
- the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive 2 before defoaming is sampled and taken out from the connecting pipe 96 between the open / close valve 95 and the closed tank 11, and the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive 2 after defoaming
- the value is a value obtained by sampling and taking out the sample immediately after passing through the drain valve 14 after defoaming.
- the dissolved oxygen concentration was measured by putting a water-dispersed adhesive (about 150 ml) sampled and taken out into a 200 ml wide-mouth glass bottle, and a dissolved oxygen concentration meter (Dissolved Oxgen Meter / model, Thermo Electron Co., Ltd.). ), And the electrode was put in and measured while slowly stirring. The measurement temperature was 26 ° C. Other measurements of dissolved oxygen concentration were performed in the same manner.
- the drain valve 14 and the open / close valve 41 are opened, and the water dispersion type adhesive is applied from the sealed tank 11 of the defoaming device 1 to the sealed tank 31 of the buffer tank 3 based on the pressure difference between the sealed tank 11 and the sealed tank 31. Agent 2 was transported.
- the opening of the leak valve 15 is operated and adjusted from the value of the pressure gauge 13, and the internal pressure of the sealed tank 11 of the defoaming device 1 is set to 11 kPa until the water-dispersed adhesive 2 fills the connecting pipe 4.
- the internal pressure of the closed tank 11 of the defoaming device 1 was adjusted to 17 kPa. That is, by operating and adjusting the leak valve 15, the difference between the internal pressure of the closed tank 11 of the defoaming device 1 and the internal pressure of the closed tank 31 of the buffer tank 3 was adjusted to be within 13 kPa.
- the dissolved oxygen concentration (0.28 mg / L) after transporting the water-dispersed pressure-sensitive adhesive 2 to the sealed tank 31 is 4.87% of the dissolved oxygen concentration (5.75 mg / L) before defoaming. It can be seen that the dissolved oxygen concentration is further reduced than after defoaming and is reduced to 5% or less before defoaming.
- the dissolved oxygen concentration value of the water-dispersed pressure-sensitive adhesive 2 is a value measured by sampling and taking out the one immediately after passing through the drain valve 33.
- the opening of the leak valve 34 and the vacuum valve 35 of the buffer tank 3 and the leak valve 54 and the vacuum valve 55 of the pump set tank 5 are operated and adjusted, and the internal pressure of the sealed tank 31 of the buffer tank 3 is controlled by the vacuum pump 7.
- the vacuum pump 7. was reduced to 11 kPa
- the internal pressure of the sealed tank 51 of the pump set tank 5 was reduced to 4 kPa.
- the drain valve 33 and the opening / closing valve 61 are opened, and the pump set tank 5 is closed from the sealed tank 31 of the buffer tank 3 based on the pressure difference between the sealed tank 31 of the buffer tank 3 and the sealed tank 51 of the pump set tank 5.
- the water-dispersed pressure-sensitive adhesive 2 was conveyed to the closed tank 51.
- the opening of the leak valve 34 is manipulated and adjusted from the value of the pressure gauge 32, and the internal pressure of the sealed tank 31 of the buffer tank 3 is set to 11 kPa until the water-dispersed adhesive 2 fills the connecting pipe 6.
- the internal pressure of the closed tank 31 of the buffer tank 3 was adjusted to 23 kPa. That is, by operating and adjusting the leak valve 54, the difference between the internal pressure of the closed tank 31 of the buffer tank 3 and the internal pressure of the closed tank 51 of the pump set tank 5 was adjusted to be within 19 kPa.
- the dissolved oxygen concentration (0.28 mg / L) after transporting the water-dispersed pressure-sensitive adhesive 2 to the sealed tank 51 is 4.87% of the dissolved oxygen concentration (5.75 mg / L) before defoaming.
- the dissolved oxygen concentration value of the water-dispersed pressure-sensitive adhesive 2 is a value measured by sampling and taking out the one immediately after passing through the drain valve 53.
- the water-dispersed pressure-sensitive adhesive 2 in the sealed tank 51 of the pump set tank 5 was conveyed to the coating device 94 through the filter 93 by the liquid feed pump 92, and the following pressure-sensitive adhesive layer was formed.
- water was passed through the filter 93 to remove bubbles in the filter 93.
- the water-dispersed pressure-sensitive adhesive 2 is caused to flow, and the water of the filter 93 is pushed out by the water-dispersed pressure-sensitive adhesive 2 and discharged.
- Water in 93 was replaced with water-dispersed pressure-sensitive adhesive 2.
- the dissolved oxygen concentration before replacing water was 0.83 mg / L, and after replacement, 0.66 mg / L.
- the dissolved oxygen concentration value of the water-dispersed pressure-sensitive adhesive 2 is a value measured immediately after passing through the drain valve 53 by sampling and taking out the thing before the coating device 94.
- the transported water-dispersed pressure-sensitive adhesive 2 is applied to the surface of a separator made of a peeled polyethylene terephthalate film (thickness 38 ⁇ m) with a die coater so that the thickness after drying is 23 ⁇ m, and then 100 ° C. And dried for 135 seconds to form an adhesive layer.
- the dissolved oxygen concentration in the applied water-dispersed pressure-sensitive adhesive 2 was 0.55 mg / L.
- the dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive 2 immediately before the application was measured by sampling the water-dispersed pressure-sensitive adhesive 2 in front of the coating device 94 (a position just before the coater).
- the final dissolved oxygen concentration of the water-dispersed pressure-sensitive adhesive 2 remaining in front of the coating device 94 (a position just before the coater) at the end of coating was 1.04 mg / L.
- Example 2 Preparation of water-dispersed adhesive
- a reaction vessel equipped with a cooling tube, a nitrogen introducing tube, a thermometer and a stirring device was charged with 30 parts of water and 0.3 part of ammonium persulfate and purged with nitrogen for 1 hour under stirring.
- Emulsified with 70 parts of water was added dropwise at 80 ° C. over 3 hours, followed by aging at 80 ° C.
- copolymer emulsion As a water-soluble cross-linking agent containing an oxazoline group, 100 parts by weight of the solid content (water-dispersed copolymer) of this copolymer emulsion is trade name “Epocross WS-700” (oxazoline group) of Nippon Shokubai Co., Ltd. Equivalent: 220 g ⁇ solid / eq.) 0.1 part (in terms of solid content) was mixed to prepare a water-dispersed adhesive (base polymer solid content 39%, viscosity 6000 mPa ⁇ s).
- Example 1 (Defoaming treatment of water-dispersed adhesive) In Example 1, operation similar to Example 1 was performed except having used the said water dispersion type adhesive.
- the dissolved oxygen concentration before defoaming of the water-dispersed pressure-sensitive adhesive was 4.88 mg / L.
- the dissolved oxygen concentration after defoaming was 0.32 mg / L, which was 6.56% of the dissolved oxygen concentration before defoaming (4.88 mg / L).
- Example 1 (Vacuum conveyance of water-dispersed adhesive) In Example 1, operation similar to Example 1 was performed except having used the said water dispersion type adhesive. It was 0.15 mg / L when the dissolved oxygen concentration after conveyance to a buffer tank was measured. The dissolved oxygen concentration (0.15 mg / L) after being transferred to the buffer tank was 3.07% of the dissolved oxygen concentration (4.88 mg / L) before defoaming. Moreover, it was 0.15 mg / L when the dissolved oxygen concentration after conveyance to a pump set tank was measured. The dissolved oxygen concentration (0.15 mg / L) after being transferred to the pump set tank was 3.07% of the dissolved oxygen concentration (4.88 mg / L) before defoaming.
- Example 1 a pressure-sensitive adhesive layer was prepared in the same manner as in Example 1 except that the defoaming treatment was not performed on the water-dispersed pressure-sensitive adhesive.
- Example 2 a pressure-sensitive adhesive layer was prepared in the same manner as in Example 1 except that the water-dispersed pressure-sensitive adhesive was defoamed and then not conveyed under reduced pressure.
- Air bubbles in the adhesive layer The number and size of air bubbles contained in the pressure-sensitive adhesive layer (area 10 m 2 ) were confirmed visually and with an optical microscope. The maximum bubble length ( ⁇ m) and the ratio of the number of bubbles having a maximum length of 50 ⁇ m or more (number / m 2 ) are shown.
- ⁇ Defect observation> A sample obtained by sandwiching both sides of the pressure-sensitive adhesive layer (thickness: 23 ⁇ m) obtained in Examples and Comparative Examples with a polyethylene terephthalate film (MRF38, manufactured by Mitsubishi Chemical Polyester Co., Ltd.) having a thickness of 38 ⁇ m was used as a sample.
- a polarizing plate manufactured by Nitto Denko Corp., TEG-DU was placed on the sample, whether or not bubble defects were visible from the side of the polarizing plate was visually confirmed, and evaluated according to the following criteria. ⁇ : Bubbles cannot be seen visually.
- X Bubbles can be visually observed.
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Abstract
Description
当該粘着剤層は、最大長さが350μmを超える気泡を含んでおらず、かつ、
粘着剤層の面において、最大長さが50~350μm気泡の個数が、1個/m2以下であることを特徴とする粘着剤層、に関する。
少なくともベースポリマーが水中に分散含有されている分散液からなる、水分散型粘着剤の脱泡処理を行なう工程(1)、
支持基材の片面または両面に、脱泡処理工程(1)が行なわれた水分散型粘着剤を塗布する工程(2)、および、
塗布された水分散型粘着剤を乾燥して粘着剤層を形成する工程(3)を有し、
かつ、前記脱泡処理工程(1)を行なう脱泡装置のタンクと、前記塗布工程(2)に水分散型粘着剤を供給するためのポンプセットタンクが、連結管を介して連結されており、
前記脱泡処理工程(1)が行なわれた水分散型粘着剤は、脱泡装置のタンク内の圧力よりも、ポンプセットタンク及び連結管内の圧力が、1kPa~50kPa小さくなるように、各圧力を設定して、脱泡装置のタンクからポンプセットタンクへ搬送されること特徴とする粘着部材の製造方法、に関する。
少なくともベースポリマーが水中に分散含有されている分散液からなる、水分散型粘着剤の脱泡処理を行なう工程(1)
支持基材の片面または両面に、脱泡処理工程(1)が行なわれた水分散型粘着剤を塗布する工程(2)、および、
塗布された水分散型粘着剤を乾燥して粘着剤層を形成する工程(3)を有し、
かつ、前記脱泡処理工程(1)を行なう脱泡装置のタンクと、前記塗布工程(2)に水分散型粘着剤を供給するためのポンプセットタンクが、バッファタンクを介して、かつ連結管を介して連結されており、
前記脱泡処理工程(1)が行なわれた水分散型粘着剤は、脱泡装置のタンク内の圧力よりも、バッファタンク及び連結管内の圧力が、1kPa~50kPa小さくなるように、各圧力を設定して、脱泡装置のタンクからバッファタンクへ搬送され、
バッファタンク内の水分散型粘着剤は、バッファタンクの圧力よりも、ポンプセットタンク及び連結管内の圧力が、1kPa~50kPa小さくなるように、各圧力を設定して、バッファタンクからポンプセットタンクへ搬送されること特徴とする粘着部材の製造方法、に関する。
測定対象となる粘着剤層(厚み23μm)の一方の面に、厚さ100μmの偏光板(日東電工社製,TEG-DU)を貼り合せた積層物(偏光板/粘着剤層、の積層構造)について、ヘイズメーターHM-150型((株)村上色彩技術研究所製)を用いて、全光線透過率(%):JISK-7361およびヘイズ(%):JIS K-7136を測定した。
(プレエマルションの調製)
容器に、アクリル酸ブチル92部、メタクリル酸6部、モノ[ポリ(プロピレンオキシド)メタクリレート]リン酸エステル(プロピレンオキシドの平均重合度約5.0)2部、3-メタクリロイルオキシプロピル-トリメトキシシラン(KBM-503、信越化学(株)製)0.03部を加えて混合し、反応成分の混合物を調製した。次いで、調製した反応成分の混合物388gに、反応性乳化剤アクアロンHS-10(第一工業製薬(株))46.6g、イオン交換水346gを加え、ホモジナイザー(特殊機化(株)製)を用いて、5分間、5000(1/min)で、攪拌し強制乳化して、モノマープレエマルションを調製した。
冷却管、窒素導入管、温度計および攪拌機を備えた反応容器に、上記で調製したモノマープレエマルションのうちの156g、イオン交換水219gを仕込み、次いで、反応容器を窒素置換し、過硫酸アンモニウム0.023g(仕込まれたモノマープレエマルションの固形分100部に対して、0.03部)を添加して、65℃で、2.5時間重合した。次いで、残りのモノマープレエマルションの625gに過硫酸アンモニウム0.217g(残りのモノマープレエマルションの固形分100部に対して、0.07部)を添加し、これを、反応容器に3時間かけて滴下して、その後、窒素置換しながら、70℃で3時間重合し、固形分40%の水分散型共重合体のエマルション溶液を得た。
得られた水分散型共重合体のエマルション溶液を室温まで冷却し、10%アンモニア水を添加して、pHを8に調整し、さらに、カルボジイミド系架橋剤(カルボジライトV-04,水溶性タイプ,日清紡(株)製)を、水分散型共重合体の固形分100部に対して、0.1部添加して、水分散型粘着剤組成物(粘度6000mPa・s)を調製した。
図1に従って、下記操作を行なった。先ず、上記水分散型粘着剤(80kg)2を脱泡装置1の密閉タンク11内に投入した。この状態で水分散型粘着剤2をサンプリングして溶存酸素濃度計を介して脱泡前の溶存酸素濃度を測定したところ、5.75mg/Lであった。
次に、脱泡装置1のリークバルブ15、真空バルブ16及びバッファタンク3のリークバルブ34、真空バルブ35の開度を操作・調整し、真空ポンプ7によって脱泡装置1の密閉タンク11の内部圧力を11kPaに、バッファタンク3の密閉タンク31の内部圧力を4kPaに減圧・調整した。
上記の搬送された水分散型粘着剤2を、剥離処理したポリエチレンテレフタレートフィルム(厚さ38μm)からなるセパレータの表面に、乾燥後の厚みが23μmになるようにダイコーターにより塗布した後、100℃で135秒間乾燥して、粘着剤層を形成した。なお、塗布される水分散型粘着剤2に溶存酸素濃度は、0.55mg/Lであった。当該塗布直前の水分散型粘着剤2の溶存酸素濃度は、塗布装置94の手前(コーターの寸前の箇所)で、水分散型粘着剤2をサンプリングして測定した。また、塗布終了時に、塗布装置94の手前に(コーターの寸前の箇所)残存していた、水分散型粘着剤2の最終溶存酸素濃度は1.04mg/Lであった。
(水分散型粘着剤の調製)
冷却管、窒素導入管、温度計および撹拌装置を備えた反応容器に、水30部および過硫酸アンモニウム0.3部を仕込み、撹拌下に1時間窒素置換した。ここにアクリル酸2-エチルへキシル95部、アクリル酸5部および乳化剤としてポリオキシエチレンラウリルエーテル硫酸アンモニウム(第一工業製薬(株)の商品名「ハイテノールLA-16」)1.0部(固形分換算)を水70部で乳化したものを80℃で3時間かけて滴下し、さらに80℃で2時間熟成を行った。その後、室温まで冷却し、10重量%アンモニア水によりpH8に調整して、共重合体エマルションを得た。この共重合体エマルションに、その固形分(水分散系共重合体)100部に対し、オキサゾリン基を含有する水溶性架橋剤として(株)日本触媒の商品名「エポクロスWS-700」(オキサゾリン基当量:220g・solid/eq.)0.1部(固形分換算)を混合して、水分散型粘着剤(ベースポリマーの固形分39%,粘度6000mPa・s)を調製した。
実施例1において、上記水分散型粘着剤を用いたこと以外は実施例1と同様の操作を居行なった。水分散型粘着剤の脱泡前の溶存酸素濃度は、4.88mg/Lであった。脱泡後の溶存酸素濃度は、0.32mg/Lであり、脱泡前の溶存酸素濃度(4.88mg/L)の6.56%であった。
実施例1において、上記水分散型粘着剤を用いたこと以外は実施例1と同様の操作を居行なった。バッファタンクに搬送後の溶存酸素濃度を測定したところ、0.15mg/Lであった。バッファタンクに搬送後の溶存酸素濃度(0.15mg/L)、脱泡前の溶存酸素濃度(4.88mg/L)の3.07%であった。
またポンプセットタンクに搬送後の溶存酸素濃度を測定したところ、0.15mg/Lであった。ポンプセットタンクに搬送後の溶存酸素濃度(0.15mg/L)、脱泡前の溶存酸素濃度(4.88mg/L)の3.07%であった。
次いで、実施例1と同様にして、搬送された水分散型粘着剤を、剥離処理したポリエチレンテレフタレートフィルム(厚さ38μm)からなるセパレータの表面に、乾燥後の厚みが23μmになるようにダイコーターにより塗布した後、100℃で135秒間乾燥して、粘着剤層を形成した。なお、塗布される水分散型粘着剤に溶存酸素濃度は、0.80mg/Lであった。また、塗布終了時における、水分散型粘着剤の最終溶存酸素濃度は0.86mg/Lであった。
実施例1において、水分散型粘着剤に対して、脱泡処理を行なわなかったこと以外は、実施例1と同様にして粘着剤層を作成した。
実施例1において、水分散型粘着剤に対して、脱泡処理した後に、減圧搬送を行なわなかったこと以外は、実施例1と同様にして粘着剤層を作成した。
粘着剤層(面積10m2)に含まれる気泡を目視および光学顕微鏡にて、その個数と大きさを確認した。気泡の最大長さ(μm)と、最大長さが50μm以上の気泡の個数の割合(個/m2)を示す。
実施例および比較例において得られた粘着剤層(厚み23μm)の両面を、厚み38μmのポリエチレンテレフタレートフィルム(三菱化学ポリエステル(株)製,MRF38)で挟み込んだものをサンプルとした。当該サンプルの上に、偏光板(日東電工社製,TEG-DU)を載せ、当該偏光板の側から、気泡欠陥が見えるか否かを目視で確認し、下記基準で評価した。
○:目視で気泡が見えない。
×:目視で気泡が見える。
2 水分散型粘着剤
3 バッファタンク
4 連結管
5 ポンプセットタンク
7 真空ポンプ
6 連結管
11 密閉タンク
13 真空バルブ
31 密閉タンク
51 密閉タンク
Claims (11)
- 少なくともベースポリマーが水中に分散含有されている分散液からなる水分散型粘着剤を塗布した後、乾燥することにより形成された粘着剤層であって、
当該粘着剤層は、最大長さが350μmを超える気泡を含んでおらず、かつ、
粘着剤層の面において、最大長さが50~350μmの気泡の個数が、1個/m2以下であることを特徴とする粘着剤層。 - 水分散型粘着剤におけるベースポリマーが、(メタ)アクリル系ポリマーであることを特徴とする請求項1記載の粘着剤層。
- ベースポリマーである、(メタ)アクリル系ポリマーが、乳化重合により得られたものであることを特徴とする請求項2記載の粘着剤層。
- 支持基材の片面または両面に、請求項1記載の粘着剤層を有することを特徴とする粘着部材。
- 支持基材が光学フィルムであることを特徴とする請求項4記載の粘着部材。
- 請求項4記載の粘着部材の製造方法であって、
少なくともベースポリマーが水中に分散含有されている分散液からなる、水分散型粘着剤の脱泡処理を行なう工程(1)
支持基材の片面または両面に、脱泡処理工程(1)が行なわれた水分散型粘着剤を塗布する工程(2)、および、
塗布された水分散型粘着剤を乾燥して粘着剤層を形成する工程(3)を有し、
かつ、前記脱泡処理工程(1)を行なう脱泡装置のタンクと、前記塗布工程(2)に水分散型粘着剤を供給するためのポンプセットタンクが、連結管を介して連結されており、
前記脱泡処理工程(1)が行なわれた水分散型粘着剤は、脱泡装置のタンク内の圧力よりも、ポンプセットタンク及び連結管内の圧力が、1kPa~50kPa小さくなるように、各圧力を設定して、脱泡装置のタンクからポンプセットタンクへ搬送されること特徴とする粘着部材の製造方法。 - 請求項4記載の粘着部材の製造方法であって、
少なくともベースポリマーが水中に分散含有されている分散液からなる、水分散型粘着剤の脱泡処理を行なう工程(1)
支持基材の片面または両面に、脱泡処理工程(1)が行なわれた水分散型粘着剤を塗布する工程(2)、および、
塗布された水分散型粘着剤を乾燥して粘着剤層を形成する工程(3)を有し、
かつ、前記脱泡処理工程(1)を行なう脱泡装置のタンクと、前記塗布工程(2)に水分散型粘着剤を供給するためのポンプセットタンクが、バッファタンクを介して、かつ連結管を介して連結されており、
前記脱泡処理工程(1)が行なわれた水分散型粘着剤は、脱泡装置のタンク内の圧力よりも、バッファタンク及び連結管内の圧力が、1kPa~50kPa小さくなるように、各圧力を設定して、脱泡装置のタンクからバッファタンクへ搬送され、
バッファタンク内の水分散型粘着剤は、バッファタンクの圧力よりも、ポンプセットタンク及び連結管内の圧力が、1kPa~50kPa小さくなるように、各圧力を設定して、バッファタンクからポンプセットタンクへ搬送されること特徴とする粘着部材の製造方法。 - 前記脱泡処理工程(1)の後における水分散型粘着剤の溶存酸素濃度は、脱泡処理工程(1)の前における水分散型粘着剤の溶存酸素濃度の15%以下であることを特徴とする請求項6または7記載の粘着部材の製造方法。
- 塗布工程(2)において塗布される水分散型粘着剤の溶存酸素濃度が、3mg/L以下であることを特徴とする請求項6または7記載の粘着部材の製造方法。
- 支持基材が光学フィルムであることを特徴とする請求項6または7の粘着部材の製造方法。
- 請求項1~3のいずれかに記載の粘着剤層または請求項4もしくは5記載の粘着部材を少なくとも1つ用いていることを特徴とする画像表示装置。
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KR1020117029092A KR101379536B1 (ko) | 2009-06-05 | 2010-05-14 | 점착제층, 점착 부재, 그 제조 방법 및 화상 표시 장치 |
US13/376,308 US20120077018A1 (en) | 2009-06-05 | 2010-05-14 | Adhesive layer, adhesive member, method for producing same, and image display |
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JP5847429B2 (ja) * | 2011-04-25 | 2016-01-20 | 日東電工株式会社 | 光学フィルム用粘着剤層およびその製造方法、粘着型光学フィルムおよびその製造方法、画像表示装置ならびに塗布液供給装置 |
JP6114126B2 (ja) * | 2013-07-04 | 2017-04-12 | 日東電工株式会社 | 積層体の製造方法 |
JP5815645B2 (ja) * | 2013-11-14 | 2015-11-17 | 日東電工株式会社 | 光学フィルムの製造方法、光学フィルムおよび画像表示装置 |
JP5979123B2 (ja) * | 2013-12-05 | 2016-08-24 | 住友化学株式会社 | 気泡欠陥の少ない偏光子 |
CN107894741B (zh) * | 2017-11-06 | 2020-03-17 | 西安交通大学 | 一种溶液环境可控的高性能薄膜制备装备 |
KR102154997B1 (ko) * | 2018-11-30 | 2020-09-14 | 주식회사 영우 | 저밀도 아크릴 폼 점착테이프 및 이의 제조방법 |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001209982A (ja) * | 2000-01-28 | 2001-08-03 | Matsushita Electric Ind Co Ltd | 接着剤のリサイクル装置 |
JP2002188063A (ja) * | 2000-12-21 | 2002-07-05 | Nitto Denko Corp | 粘着シートの製造方法およびその装置 |
JP2002309212A (ja) * | 2001-04-18 | 2002-10-23 | Nitto Denko Corp | ガラス板用水分散型粘着シートおよび粘着型光学フィルム、液晶表示装置 |
JP2008214500A (ja) * | 2007-03-05 | 2008-09-18 | Nitto Denko Cs System Kk | セパレーター剥離用粘着テープおよびそれを用いたセパレーター剥離方法 |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2001209982A (ja) * | 2000-01-28 | 2001-08-03 | Matsushita Electric Ind Co Ltd | 接着剤のリサイクル装置 |
JP2002188063A (ja) * | 2000-12-21 | 2002-07-05 | Nitto Denko Corp | 粘着シートの製造方法およびその装置 |
JP2002309212A (ja) * | 2001-04-18 | 2002-10-23 | Nitto Denko Corp | ガラス板用水分散型粘着シートおよび粘着型光学フィルム、液晶表示装置 |
JP2008214500A (ja) * | 2007-03-05 | 2008-09-18 | Nitto Denko Cs System Kk | セパレーター剥離用粘着テープおよびそれを用いたセパレーター剥離方法 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2021100423A1 (ja) * | 2019-11-19 | 2021-05-27 | 日東電工株式会社 | 光学積層体の製造方法、接着剤塗工装置及び光学積層体の製造装置 |
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US20120077018A1 (en) | 2012-03-29 |
KR101379536B1 (ko) | 2014-03-28 |
KR20120025506A (ko) | 2012-03-15 |
JP2010280856A (ja) | 2010-12-16 |
CN102439104A (zh) | 2012-05-02 |
TWI494395B (zh) | 2015-08-01 |
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