Classifications

• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
  • C09K3/00—Materials not provided for elsewhere
  • C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
• • 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 
  • G02F1/15—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 an electrochromic effect
  • G02F1/153—Constructional details
  • G02F1/161—Gaskets; Spacers; Sealing of cells; Filling or closing of cells

Definitions

• the present invention relates to a sealant for light control elements.
• liquid crystal light control elements using a liquid crystal material and electrochromic elements using an electrochromic compound are widely used.
• the liquid crystal light control element is a light control element that controls the amount of light transmission by changing the orientation of liquid crystal molecules by changing the potential difference between transparent electrode layers, and has excellent responsiveness.
• the electrochromic element is a light control element that reversibly changes color due to the electrochemical oxidation-reduction reaction of electrochromic compounds, and can maintain the colored state until it is decolorized, so it can be driven with low power consumption.
• Patent Document 1 discloses the use of a sealant containing an epoxy compound to surround the liquid crystal layer of the light control unit
• Patent Document 2 discloses the use of a sealant containing a (meth)acrylic compound or an epoxy compound as a sealing material for the electrochromic element.
• An object of the present invention is to provide a sealant for a light control device which has excellent adhesion and low contamination properties.
• Disclosure 1 is a sealant for a light control element, comprising a curable resin, a photoradical polymerization initiator, and an amine-based heat curing agent, wherein the curable resin comprises a (meth)acrylic compound having no epoxy group, the (meth)acrylic compound comprises a compound having two or more (meth)acryloyl groups in one molecule, and the curable resin does not comprise an epoxy compound or comprises 5 parts by mass or less of an epoxy compound per 100 parts by mass of the curable resin.
• the present disclosure 2 is the sealant for a light control element according to the present disclosure 1, wherein the curable resin does not contain an epoxy compound.
• the present disclosure 3 is the sealant for a light control element according to the present disclosure 1 or 2, in which the content of the amine-based heat curing agent relative to 100 parts by mass of the curable resin is 0.5 parts by mass or more and 3.0 parts by mass or less.
• the present disclosure 4 is a sealant for light control elements according to the present disclosure 1, 2, or 3, in which the content of the amine-based heat curing agent relative to 100 parts by mass of the compound having two or more (meth)acryloyl groups in one molecule is 0.5 parts by mass or more and 3.0 parts by mass or less.
• the present disclosure 5 is the sealing agent for a light control device according to the present disclosure 1, 2, 3, or 4, wherein the amine-based heat curing agent contains a hydrazide compound.
• the present disclosure 6 is a sealant for a light control element according to the present disclosure 1, 2, 3, 4, or 5, which is used for sealing an electrochromic element. The present invention will be described in detail below.
• the present inventors investigated further compounding an amine-based heat curing agent into a light control element sealant containing a (meth)acrylic compound including a compound having two or more (meth)acryloyl groups in one molecule and a photoradical polymerization initiator, and improving the adhesion of the sealant by a Michael addition reaction between the amine-based heat curing agent and the (meth)acrylic compound.
• a light control element sealant that has excellent adhesion and also has excellent low contamination properties by not using an epoxy compound or by reducing the amount of epoxy compound contained, and thus completed the present invention.
• the sealing agent for a light control element of the present invention contains a curable resin.
• the curable resin contains a (meth)acrylic compound having no epoxy group.
• the sealing agent for light control elements of the present invention has excellent low contamination properties.
• (meth)acrylic means acrylic or methacrylic
• (meth)acrylic compound means a compound having a (meth)acryloyl group
• (meth)acryloyl means acryloyl or methacryloyl.
• the (meth)acrylic compound includes a compound having two or more (meth)acryloyl groups in one molecule (hereinafter also referred to as a "difunctional or higher (meth)acrylic compound").
• difunctional or higher (meth)acrylic compound By including the difunctional or higher (meth)acrylic compound as the (meth)acrylic compound in combination with a photoradical polymerization initiator described below and an amine-based heat curing agent described below, the sealing agent for light control elements of the present invention has excellent curability and adhesion.
• examples of the difunctional (meth)acrylic compound having two (meth)acryloyl groups in one molecule include difunctional epoxy (meth)acrylates, difunctional (meth)acrylic acid ester compounds, difunctional urethane (meth)acrylates, etc.
• difunctional epoxy (meth)acrylates are preferred.
• the above-mentioned "epoxy (meth)acrylate” means a compound in which all epoxy groups in an epoxy compound have been reacted with (meth)acrylic acid.
• the above-mentioned bifunctional epoxy (meth)acrylate can be, for example, one obtained by reacting a bifunctional epoxy compound having two epoxy groups in one molecule with (meth)acrylic acid in the presence of a basic catalyst according to a conventional method.
• the bifunctional epoxy compound that is the raw material for the bifunctional epoxy (meth)acrylate may, for example, be a bisphenol A type epoxy compound, a bisphenol F type epoxy compound, a bisphenol S type epoxy compound, a 2,2'-diallyl bisphenol A type epoxy compound, a hydrogenated bisphenol type epoxy compound, a propylene oxide-added bisphenol A type epoxy compound, a resorcinol type epoxy compound, a biphenyl type epoxy compound, a sulfide type epoxy compound, a diphenyl ether type epoxy compound, a dicyclopentadiene type epoxy compound, a naphthalene type epoxy compound, a glycidylamine type epoxy compound, an alkyl polyol type epoxy compound, a rubber-modified epoxy compound, a glycidyl ester compound, or the like.
• a resorcinol type epoxy compound is preferred. That is, the bifunctional or higher (meth)acrylic compound
• the bifunctional or higher (meth)acrylic compound contains the resorcinol type epoxy (meth)acrylate
• the preferred lower limit of the content of the resorcinol type epoxy (meth)acrylate in 100 parts by mass of the curable resin is 10 parts by mass, and the preferred upper limit is 90 parts by mass.
• the content of the resorcinol type epoxy (meth)acrylate is within this range, the obtained sealing agent for light control elements has better reliability.
• the more preferred lower limit of the content of the resorcinol type epoxy (meth)acrylate is 30 parts by mass, and the more preferred upper limit is 80 parts by mass.
• bifunctional (meth)acrylic acid ester compounds include 1,3-butanediol di(meth)acrylate, 1,4-butanediol di(meth)acrylate, 1,6-hexanediol di(meth)acrylate, 1,9-nonanediol di(meth)acrylate, 1,10-decanediol di(meth)acrylate, ethylene glycol di(meth)acrylate, diethylene glycol di(meth)acrylate, tetraethylene glycol di(meth)acrylate, polyethylene glycol di(meth)acrylate, 2-n-butyl-2-ethyl-1,3-propanediol di(meth)acrylate, dipropylene glycol di(meth)acrylate, tripropylene glycol di(meth)acrylate, polypropylene glycol di(meth)acrylate, t) acrylate, neopentyl glycol di(meth)acrylate,
• bifunctional urethane (meth)acrylate can be obtained, for example, by reacting a bifunctional isocyanate compound with a (meth)acrylic acid derivative having a hydroxyl group in the presence of a catalytic amount of a tin-based compound.
• bifunctional isocyanate compounds include isophorone diisocyanate, 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, hexamethylene diisocyanate, trimethylhexamethylene diisocyanate, diphenylmethane-4,4'-diisocyanate (MDI), hydrogenated MDI, polymeric MDI, 1,5-naphthalene diisocyanate, norbornane diisocyanate, tolidine diisocyanate, xylylene diisocyanate (XDI), hydrogenated XDI, lysine diisocyanate, and tetramethylxylylene diisocyanate.
• MDI diphenylmethane-4,4'-diisocyanate
• XDI xylylene diisocyanate
• XDI xylylene diisocyanate
• XDI hydrogenated XDI
• lysine diisocyanate
• difunctional isocyanate compound a chain-extended difunctional isocyanate compound obtained by reacting a polyol with an excess of a difunctional isocyanate compound can also be used.
• the polyol include ethylene glycol, propylene glycol, glycerin, sorbitol, trimethylolpropane, carbonate diol, polyether diol, polyester diol, and polycaprolactone diol.
• Examples of the (meth)acrylic acid derivative having a hydroxyl group include hydroxyalkyl mono(meth)acrylates, mono(meth)acrylates of dihydric alcohols, and mono(meth)acrylates of trihydric alcohols.
• Examples of the hydroxyalkyl mono(meth)acrylate include 2-hydroxyethyl(meth)acrylate, 2-hydroxypropyl(meth)acrylate, 2-hydroxybutyl(meth)acrylate, and 4-hydroxybutyl(meth)acrylate.
• Examples of the dihydric alcohol include ethylene glycol, propylene glycol, 1,3-propanediol, 1,3-butanediol, 1,4-butanediol, and polyethylene glycol.
• Examples of the trihydric alcohol include trimethylolethane, trimethylolpropane, and glycerin.
• examples of trifunctional or higher (meth)acrylic compounds having three or more (meth)acryloyl groups in one molecule include, for example, ethylene oxide-added isocyanuric acid tri(meth)acrylate, trimethylolpropane tri(meth)acrylate, ethylene oxide-added trimethylolpropane tri(meth)acrylate, propylene oxide-added trimethylolpropane tri(meth)acrylate, caprolactone-modified trimethylolpropane tri(meth)acrylate, glycerin tri(meth)acrylate, propylene oxide-added glycerin tri(meth)acrylate, pentaerythritol tri(meth)acrylate, tris(meth)acryloyloxyethyl phosphate, ditrimethylolpropane tetra(meth)acrylate, pentaerythritol tetra(meth)acrylate
• the preferred lower limit of the content of the difunctional or higher (meth)acrylic compound in 100 parts by mass of the curable resin is 90 parts by mass.
• the content of the difunctional or higher (meth)acrylic compound is 90 parts by mass or more, the resulting sealant for light control elements has excellent low contamination properties.
• a more preferred lower limit of the content of the difunctional or higher (meth)acrylic compound is 95 parts by mass, and an even more preferred lower limit is 97 parts by mass. It is particularly preferred that the content of the difunctional or higher (meth)acrylic compound is 100 parts by mass, that is, the curable resin is composed only of the difunctional or higher (meth)acrylic compound.
• the (meth)acrylic compound may contain a monofunctional (meth)acrylic compound having one (meth)acryloyl group in one molecule.
• the curable resin does not contain an epoxy compound, or contains 5 parts by mass or less of an epoxy compound per 100 parts by mass of the curable resin.
• the sealant for light control elements of the present invention has excellent low contamination properties.
• epoxy compound means a compound having an epoxy group.
• the above epoxy compounds include, for example, bisphenol A type epoxy compounds, bisphenol F type epoxy compounds, bisphenol S type epoxy compounds, 2,2'-diallyl bisphenol A type epoxy compounds, hydrogenated bisphenol type epoxy compounds, propylene oxide-added bisphenol A type epoxy compounds, resorcinol type epoxy compounds, biphenyl type epoxy compounds, sulfide type epoxy compounds, diphenyl ether type epoxy compounds, dicyclopentadiene type epoxy compounds, naphthalene type epoxy compounds, phenol novolac type epoxy compounds, orthocresol novolac type epoxy compounds, dicyclopentadiene novolac type epoxy compounds, biphenyl novolac type epoxy compounds, naphthalene phenol novolac type epoxy compounds, glycidyl amine type epoxy compounds, alkyl polyol type epoxy compounds, rubber modified type epoxy compounds, glycidyl ester compounds, etc.
• the epoxy compound also includes a partially (meth)acrylic modified epoxy compound.
• the partially (meth)acrylic modified epoxy compound means a compound having one or more epoxy groups and one or more (meth)acryloyl groups in one molecule, which is obtained by reacting a part of an epoxy group of an epoxy compound having two or more epoxy groups with (meth)acrylic acid.
• the partially (meth)acrylic modified epoxy compound has a (meth)acryloyl group, it is treated as the epoxy compound, not the (meth)acrylic compound.
• the curable resin preferably does not contain an epoxy compound.
• the upper limit of the content of the epoxy compound in 100 parts by mass of the curable resin is 5 parts by mass.
• the preferred upper limit of the content of the epoxy compound is 3 parts by mass, and the more preferred upper limit is 1 part by mass.
• the preferred lower limit of the total content of the curable resin in 100 parts by mass of the sealant for light control devices of the present invention is 65 parts by mass, and the preferred upper limit is 96 parts by mass. When the total content of the curable resin is within this range, the resulting sealant for light control devices has better curability and adhesion.
• the more preferred lower limit of the total content of the curable resin is 70 parts by mass, and the more preferred upper limit is 88 parts by mass.
• the sealing agent for light control elements of the present invention contains a photoradical polymerization initiator.
• the photoradical polymerization initiator include benzophenone compounds, acetophenone compounds, acylphosphine oxide compounds, titanocene compounds, oxime ester compounds, benzoin ether compounds, and thioxanthone compounds.
• photoradical polymerization initiator examples include 1-hydroxycyclohexyl phenyl ketone, 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)-1-butanone, 2-(dimethylamino)-2-((4-methylphenyl)methyl)-1-(4-(4-morpholinyl)phenyl)-1-butanone, 2,2-dimethoxy-1,2-diphenylethan-1-one, bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide, and 2-methyl-1-(4-methylthiophenyl).
• 2-morpholinopropan-1-one 1-(4-(2-hydroxyethoxy)-phenyl)-2-hydroxy-2-methyl-1-propan-1-one, 1-(4-(phenylthio)phenyl)-1,2-octanedione 2-(O-benzoyloxime), 2-(acetoxyimino)-1-(4-(4-(2-hydroxyethoxy)phenylthio)phenyl)propan-1-one, 2,4,6-trimethylbenzoyldiphenylphosphine oxide, 2,4-dimethylthioxanthen-9-one, and the like.
• the content of the photoradical polymerization initiator is preferably 0.01 parts by mass at the lower limit and 10 parts by mass at the upper limit relative to 100 parts by mass of the curable resin. When the content of the photoradical polymerization initiator is within this range, the resulting sealing agent for light control elements has better storage stability and photocurability.
• a more preferred lower limit of the content of the photoradical polymerization initiator is 0.1 parts by mass, and a more preferred upper limit is 5 parts by mass.
• the sealing agent for light control elements of the present invention may contain a thermal radical polymerization initiator.
• the thermal radical polymerization initiator include those composed of an azo compound, an organic peroxide, etc. Among them, from the viewpoint of suppressing contamination of liquid crystal, electrochromic compound solution, etc., an initiator composed of an azo compound (hereinafter also referred to as "azo initiator”) is preferable.
• the thermal radical polymerization initiators may be used alone or in combination of two or more kinds.
• the azo compound may, for example, have a structure in which a plurality of units such as polyalkylene oxide or polydimethylsiloxane are bonded via an azo group.
• a polymeric azo compound having a structure in which a plurality of units such as polyalkylene oxide are bonded via the azo group those having a polyethylene oxide structure are preferred.
• the azo compound examples include 2,2'-azobis(2,4-dimethylvaleronitrile), 4,4'-azobis(4-cyanovaleric acid), a polycondensate of 4,4'-azobis(4-cyanopentanoic acid) and polyalkylene glycol, and a polycondensate of 4,4'-azobis(4-cyanopentanoic acid) and polydimethylsiloxane having a terminal amino group.
• the azo initiator examples include VPE-0201, VPE-0401, VPE-0601, VPS-0501, VPS-1001, V-65, and V-501 (all manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.).
• organic peroxides examples include ketone peroxides, peroxyketals, hydroperoxides, dialkyl peroxides, peroxy esters, diacyl peroxides, and peroxydicarbonates.
• the content of the thermal radical polymerization initiator is preferably 0.01 parts by mass at the lower limit and 10 parts by mass at the upper limit relative to 100 parts by mass of the curable resin. When the content of the thermal radical polymerization initiator is within this range, the resulting sealing agent for light control elements has better storage stability and thermosetting properties.
• a more preferred lower limit of the content of the thermal radical polymerization initiator is 0.1 parts by mass, and a more preferred upper limit is 5 parts by mass.
• the sealing agent for light control elements of the present invention contains an amine-based heat curing agent.
• the amine-based heat curing agent plays a role as a nucleophile in the Michael addition reaction with the (meth)acrylic compound. Even if the light control element sealant of the present invention does not contain the epoxy compound or contains only a small amount of the epoxy compound, the light control element sealant of the present invention has excellent adhesiveness due to the progression of the Michael addition reaction between the (meth)acrylic compound and the amine-based heat curing agent.
• the amine-based heat curing agent also acts as a curing agent for the epoxy compound.
• amine-based heat curing agent examples include hydrazide compounds, imidazole derivatives, amine adduct compounds, etc. Among these, primary amine compounds and secondary amine compounds are preferred, and hydrazide compounds are more preferred.
• hydrazide compound refers to a compound having a hydrazide group.
• hydrazide compounds examples include sebacic acid dihydrazide, isophthalic acid dihydrazide, adipic acid dihydrazide, and malonic acid dihydrazide.
• the preferred lower limit of the content of the amine-based heat curing agent relative to 100 parts by mass of the curable resin is 0.5 parts by mass, and the preferred upper limit is 3.0 parts by mass.
• the content of the amine-based heat curing agent relative to 100 parts by mass of the curable resin is 0.5 parts by mass or more, the resulting light control element sealant has better adhesion.
• the content of the amine-based heat curing agent relative to 100 parts by mass of the curable resin is 3.0 parts by mass or less, the resulting light control element sealant has better low contamination.
• the more preferred lower limit of the content of the amine-based heat curing agent relative to 100 parts by mass of the curable resin is 1.0 parts by mass, and the more preferred upper limit is 1.5 parts by mass.
• the preferred lower limit of the content of the amine-based heat curing agent relative to 100 parts by mass of the difunctional or more (meth)acrylic compound is 0.5 parts by mass, and the preferred upper limit is 3.0 parts by mass.
• the content of the amine-based heat curing agent relative to 100 parts by mass of the difunctional or more (meth)acrylic compound is 0.5 parts by mass or more, the obtained light control element sealant has better adhesion.
• the content of the amine-based heat curing agent relative to 100 parts by mass of the difunctional or more (meth)acrylic compound is 3.0 parts by mass or less, the obtained light control element sealant has better low contamination.
• the more preferred lower limit of the content of the amine-based heat curing agent relative to 100 parts by mass of the difunctional or more (meth)acrylic compound is 1.0 parts by mass, and the more preferred upper limit is 1.5 parts by mass.
• the sealing agent for light control elements of the present invention may further contain a filler for the purposes of improving viscosity, further improving adhesion by a stress dispersion effect, improving the linear expansion coefficient, and further improving moisture permeability prevention properties.
• an inorganic filler or an organic filler can be used as the filler.
• the inorganic filler include silica, talc, glass beads, asbestos, gypsum, diatomaceous earth, smectite, bentonite, montmorillonite, sericite, activated clay, alumina, zinc oxide, iron oxide, magnesium oxide, tin oxide, titanium oxide, calcium carbonate, magnesium carbonate, magnesium hydroxide, aluminum hydroxide, aluminum nitride, silicon nitride, barium sulfate, and calcium silicate.
• the organic filler include polyester fine particles, polyurethane fine particles, vinyl polymer fine particles, (meth)acrylic polymer fine particles, etc.
• the organic filler may have a core-shell structure. The above fillers may be used alone or in combination of two or more kinds.
• the preferred lower limit of the content of the filler relative to 100 parts by mass of the curable resin is 10 parts by mass, and the preferred upper limit is 50 parts by mass.
• the content of the filler is within this range, the effect of improving adhesion is excellent without deteriorating the coatability, etc.
• a more preferred upper limit of the content of the filler is 40 parts by mass.
• the light control element sealant of the present invention preferably further contains a silane coupling agent.
• the silane coupling agent mainly serves as an adhesion aid for favorably adhering the light control element sealant to a substrate or the like.
• the silane coupling agent for example, 3-aminopropyltrimethoxysilane, 3-mercaptopropyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, etc. are suitably used.
• the preferred lower limit of the content of the silane coupling agent relative to 100 parts by mass of the curable resin is 0.8 parts by mass, and the preferred upper limit is 3.4 parts by mass.
• the more preferred lower limit of the content of the silane coupling agent is 1.0 part by mass, and the more preferred upper limit is 3.0 parts by mass.
• the sealing agent for light control elements of the present invention may further contain additives such as light shielding agents, stress relaxation agents, reactive diluents, thixotropic agents, spacers, curing accelerators, defoamers, leveling agents, and polymerization inhibitors, as necessary.
• additives such as light shielding agents, stress relaxation agents, reactive diluents, thixotropic agents, spacers, curing accelerators, defoamers, leveling agents, and polymerization inhibitors, as necessary.
• Examples of a method for producing the sealing agent for light-adjusting elements of the present invention include a method of mixing a curable resin, a photoradical polymerization initiator, an amine-based heat curing agent, and other components such as an inorganic filler and a silane coupling agent using a mixer.
• Examples of the mixer include a homodisper, a homomixer, a universal mixer, a planetary mixer, a kneader, and a three-roll mixer.
• the sealing agent for light control elements of the present invention is suitably used for sealing electrochromic elements.
• the sealing portion formed by the sealing agent for light control elements of the present invention is preferably provided around a solution containing an electrochromic compound and an electrolyte.
• the present invention provides a sealant for light control elements that has excellent adhesion and low contamination.
• Examples 1 to 20, Comparative Examples 1 to 8 According to the compounding ratios shown in Tables 1 to 3, each material was stirred with a planetary stirrer and then uniformly mixed with a ceramic triple roll to obtain sealing agents for light control elements of Examples 1 to 20 and Comparative Examples 1 to 8.
• Awatori Mixer manufactured by Thinky Corporation was used as the planetary stirrer.
• the obtained sealing agent for light control elements was dropped in small drops onto one of two glass substrates with ITO thin film (length 4.5 mm, width 2.5 mm).
• the other glass substrate with ITO thin film was attached to this in a cross shape, and after irradiating with ultraviolet light of 100 mW/ cm2 from a metal halide lamp for 30 seconds, it was heated at 120°C for 60 minutes to obtain a test piece.
• the edge of the substrate in the prepared test piece was pressed into the substrate with a metal cylinder of radius 5 mm at a speed of 5 mm/min, and the strength at which the panel peeled off was measured.
• the measured value (kgf) was divided by the diameter (cm) of the joint to obtain the adhesive strength, and the adhesiveness was evaluated according to the following criteria.
• ⁇ When the adhesive strength was 2.5 kgf/cm or more.
• ⁇ When the adhesive strength was 2.0 kgf/cm or more and less than 2.5 kgf/cm.
• ⁇ When the adhesive strength was 1.5 kgf/cm or more and less than 2.0 kgf/cm.
• ⁇ When the adhesive strength was less than 1.5 kgf/cm.
• the obtained light control element sealant was applied to a smooth release film using a coater to a thickness of 200 to 300 ⁇ m.
• the light control element sealant was irradiated with 100 mW/ cm2 ultraviolet light from a metal halide lamp for 30 seconds, and then heated at 120°C for 60 minutes to harden the light control element sealant, thereby obtaining a film for moisture permeability measurement.
• a moisture permeability test cup was prepared according to the moisture permeability test method for moisture-proof packaging materials (cup method) of JIS Z 0208, and the obtained moisture permeability test film was attached to the cup, which was then placed in a constant temperature and humidity oven at 80°C and 90% RH to measure the moisture permeability.
• the moisture permeability prevention was evaluated according to the following criteria.
• Moisture permeability is more than 80g/ m2 ⁇ 24hr.
• the obtained light control sealant was applied to one of two glass substrates with an ITO thin film using a dispenser to draw a square frame to form a seal pattern, and then the other substrate was placed on top of it in a vacuum. After releasing the vacuum, the seal pattern portion was irradiated with ultraviolet light of 100 mW/ cm2 from a metal halide lamp for 30 seconds, and then heated at 120°C for 60 minutes to obtain a test piece. The seal pattern portion in the obtained test piece was visually observed, and the coatability was evaluated according to the following criteria. ⁇ : When the seal pattern had no breaks or undulations and a clean line was drawn. ⁇ : When there were no breaks, but the seal pattern had undulations. ⁇ : When breaks were found.
• the obtained light control element sealant was applied to one of the two glass substrates with the ITO thin film using a dispenser so as to draw a circular frame, forming an outer frame seal pattern.
• the light control element sealant was dotted on the inside of the formed seal pattern.
• a ⁇ -butyrolactone solution containing 30% by mass of ethyl 2-cyano-3,3-diphenylacrylate as an electrochromic compound was applied dropwise to the entire inside of the frame of the sealant of the glass substrate with the ITO thin film, and the other substrate was placed on top of it in a vacuum.
• the outer frame seal pattern was irradiated with 100 mW/ cm2 ultraviolet light from a metal halide lamp for 30 seconds, and then heated at 120°C for 60 minutes to obtain a test piece.
• a mask was placed to prevent the dotted light control element sealant from being irradiated with ultraviolet light.
• a voltage of 1.0 V was applied to the obtained test piece for 5 minutes, and the display unevenness and the stained distance around the dotted areas of the light control element sealant were checked, and the low staining property was evaluated according to the following criteria.
• the present invention provides a sealant for light control elements that has excellent adhesion and low contamination.

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• 2024
  • 2024-11-14 WO PCT/JP2024/040451 patent/WO2025105426A1/ja active Pending
  • 2024-11-14 JP JP2025536315A patent/JP7755773B2/ja active Active
  • 2024-11-14 CN CN202480040632.2A patent/CN121399536A/zh active Pending
  • 2024-11-15 TW TW113143974A patent/TW202532571A/zh unknown

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