CN102031077A - Adhesive composition and adhesion layer - Google Patents
Adhesive composition and adhesion layer Download PDFInfo
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- CN102031077A CN102031077A CN 201010541899 CN201010541899A CN102031077A CN 102031077 A CN102031077 A CN 102031077A CN 201010541899 CN201010541899 CN 201010541899 CN 201010541899 A CN201010541899 A CN 201010541899A CN 102031077 A CN102031077 A CN 102031077A
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Abstract
The invention discloses an adhesive composition and an adhesion layer. The adhesive composition comprises acrylic copolymer, total solvent and cross linking agent, wherein the total solvent comprises a first solvent and a second solvent, and the boiling point of the second solvent is higher than 111 DEG C. After being polymerized, the adhesive composition forms a viscose, and the first solvent has favorable solubility to the viscose. The weight ratio of the first solvent to the second solvent is 80-90:1-20. The adhesive composition is prepared by regulating the types and the proportion of the solvents, and the adhesive composition has the characteristics of low volatility, good coating property, good processability, etc. In addition, the adhesion layer formed by the adhesive composition has favorable durability and appropriate flexibility relative to base materials.
Description
Technical field
The present invention is relevant for sticking agent constituent and adhering layer, and is particularly to pressure-sensitive sticking agent constituent and pressure-sensitive adhering layer.
Background technology
The thin slice that contains organic materials often is attached on the substrate as glass, pottery or metal via the pressure-sensitive sticking agent.For instance, the Polarizer that liquid-crystal display (LCD) uses is generally the film of three-decker, and wherein optical anisotropic film (for example cellulosetri-acetate (TAC) film) attaches to the both side surface of polyethenol series Polarizer simultaneously.For Polarizer being attached at other optical element, for example have the phase retardation film or the liquid crystal born of the same parents of multilayered structure, can on the surface of Polarizer, be coated with the pressure-sensitive adhering layer.
In the process of preparation sticking agent constituent, aqueous vapor is if react with the sticking agent constituent, white atomizing takes place in coating process easily, if use the not good problem of display effect that can cause in optical component, reduces using and the activity duration (pot life) of sticking agent.In addition,, can make dispense tip air-dry easily if the solvent that the pressure-sensitive sticking agent uses is volatile, and in coating, cause inhomogeneous, blob of viscose generates or the coating rear surface have bad order such as lines etc. problem, cause device usefulness low even can't use.And if the solvent that the pressure-sensitive sticking agent uses is not volatile, the pressure-sensitive adhering layer of formation is in heating or the hot and humid easy down problem of peeling off or foaming of environment.
Therefore, industry still is devoted to develop to possess suitable evaporation rate and have and enough can be used and the pressure-sensitive sticking agent of activity duration characteristic, and its formed adhering layer has good coating, weather resistance and processibility.
Summary of the invention
Purpose of the present invention is for providing a kind of sticking agent constituent and adhering layer.The sticking agent constituent comprises multiple solvent of different nature, and by the kind and the ratio of adjusting solvent, the sticking agent constituent has the characteristic of low volatility, good coating, processibility etc. simultaneously.In addition, the adhering layer that utilizes the sticking agent constituent to form also has favorable durability, and has suitable retractility with respect to base material.
On the one hand, a kind of sticking agent constituent is proposed according to the present invention.The sticking agent constituent comprises acrylic copolymer, total solvent and linking agent.Total solvent comprises first solvent and second solvent.The boiling point of second solvent is higher than 111 degree Celsius.The sticking agent constituent can form viscose after carrying out polymerization, first solvent has good solubleness for viscose.The weight of first solvent: the weight of second solvent is 80～99: 1～20.
Further, this acrylic copolymer is formed by the following material of copolymerization: (a) (methyl) Acrylic Acid Monomer 85 to 99.5 weight parts; And (b) tool crosslinkable functional group and contain the ethene functional group and/or vinylformic acid functional group's monomer 0.5 to 15 weight part, wherein (a) with (b) add up to totally 100 weight parts.
Further, this tool crosslinkable functional group and contain the ethene functional group and/or vinylformic acid functional group's monomer is to be selected from by vinylformic acid 2-hydroxyl ethyl ester, methacrylic acid 2-hydroxyl ethyl ester, methacrylic acid 2-hydroxypropyl acrylate, vinylformic acid 2-hydroxypropyl acrylate, methacrylic acid 2-hydroxyl ethylene glycol, vinylformic acid 2-hydroxyl ethylene glycol, methacrylic acid 2-hydroxyl propylene glycol, vinylformic acid 2-hydroxyl propylene glycol, methacrylic acid, vinylformic acid, acrylic acid dimer, methylene-succinic acid, maleic acid and group that MALEIC ANHYDRIDE constituted or above-mentioned combination.
Further, this sticking agent constituent is applied to optical component.
Further, this second solvent is selected from by acetate, dimethyl formamide, dimethyl sulfoxide (DMSO), group that propyl carbinol, butylacetate, isobutyl acetate, dimethylbenzene, chlorobenzene, butanols, ethylene glycol, aniline, mibk and pentyl acetate constituted or above-mentioned combination.
Further, the boiling point of this second solvent is higher than the boiling point of this first solvent.
Further, the weight average molecular weight of this acrylic copolymer is 500,000 to 2,000,000.
Further, this total solvent also comprises the 3rd solvent, and the 3rd solvent comprises hexane or normal heptane.
Further, in the gross weight of this first solvent, this second solvent and the 3rd solvent, the weight of the 3rd solvent accounts for 0.01～10%.
Further, the weight of this first solvent: the weight of this second solvent is 85～95: 5～15.
Further, this linking agent comprises isocyanate-based linking agent or metal-chelating system linking agent, this sticking agent constituent also comprises silane coupling agent, wherein with respect to this acrylic copolymers of 100 weight parts, this isocyanate-based linking agent is 0.1～10 weight part, or this metal-chelating system linking agent is 0.1～10 weight part, or this silane coupling agent is 0.001～2 weight part.
Further, with respect to this acrylic copolymer of 100 weight parts, this silane coupling agent is 0.1～1 weight part.
Further, with respect to this acrylic copolymer of 100 weight parts, this isocyanate-based linking agent is 0.5～2 weight part, and this metal-chelating system linking agent is 0.5～2 weight part.
Further, this isocyanate-based linking agent and this metal-chelating system linking agent use simultaneously.
Further, this first solvent is to be selected from by methyl acetate, acetone, toluene, ethyl acetate, group that ethanol, benzene, tetrahydrofuran (THF), chloroform, Virahol and methylene dichloride constituted or above-mentioned combination.
Further, the weight of this acrylic copolymer: the weight of this total solvent is 18: 82.
One side again according to the present invention proposes a kind of adhering layer.Adhering layer forms with following method.Above-mentioned sticking agent constituent is provided; The sticking agent constituent is carried out polymerization and total solvent is vapored away, to obtain adhering layer.
Compared with prior art, sticking agent constituent of the present invention comprises multiple solvent of different nature, and by the kind and the ratio of adjusting solvent, the sticking agent constituent has the characteristic of low volatility, good coating, processibility etc. simultaneously.In addition, the adhering layer that utilizes the sticking agent constituent to form also has favorable durability, and has suitable retractility with respect to base material.
Description of drawings
Embodiment
Embodiments of the invention provide a kind of sticking agent constituent.The sticking agent constituent can form viscose after carrying out polymerization.Viscose can form adhering layer after total solvent vapors away.Therefore, in other words, the sticking agent constituent can form adhering layer after carrying out polymerization and total solvent vapored away.
In an embodiment of the present invention, the sticking agent constituent comprises acrylic copolymer, total solvent and linking agent.Because the sticking agent constituent comprises acrylic copolymer, therefore the viscose that forms can be considered the vinylformic acid viscose.In an embodiment, viscose is a vinylformic acid pressure-sensitive viscose.Total solvent comprises first solvent and second solvent.First solvent has good solubleness for the sticking agent constituent, also to having good solubleness by the formed viscose of sticking agent constituent.Second solvent has the low-volatile characteristic of high boiling point, and for example boiling point is higher than 111 degree Celsius.The boiling point of second solvent is higher than first solvent.In an embodiment, the weight of acrylic copolymer: the weight of total solvent is 18: 82.The weight of first solvent: the weight of second solvent is 80～99: 1～20, and preferably, the weight of first solvent: the weight of second solvent is 85～95: 5～15.
Acrylic copolymer is by copolymerization tool crosslinkable functional group and contains the ethene functional group and/or vinylformic acid functional group's monomer and (methyl) Acrylic Acid Monomer form.The main body of (methyl) Acrylic Acid Monomer is (methyl) Acrylic Acid Monomer, and wherein methyl is not essential.(methyl) Acrylic Acid Monomer such as tool alkyl, alkyl carbon number are generally 1-12 also can be more.The method of copolymerization comprises for example solution polymerization process, emulsion polymerization method, suspension polymerization or overall polymerization etc., is preferably the solution polymerization process of organic solvent.
Tool crosslinkable functional group and contain the ethene functional group and/or vinylformic acid functional group's monomer and (methyl) Acrylic Acid Monomer add up under the situation of 100 weight parts totally, (methyl) Acrylic Acid Monomer accounts for 85 to 99.5 weight parts, preferable 90 to 99.5 weight parts, tool crosslinkable functional group and contain the ethene functional group and/or vinylformic acid functional group's monomer accounts for 0.5 to 15 weight part, preferable 0.5 to 10 weight part.Use the tool crosslinkable functional group of above-mentioned part by weight and contain the ethene functional group and/or vinylformic acid functional group's monomer and the formed acrylic copolymer of (methyl) Acrylic Acid Monomer can have the sense radix that enough and linking agent carries out bond.If tool crosslinkable functional group and contain the ethene functional group and/or vinylformic acid functional group's monomer is lower than 0.5 weight part, formed acrylic copolymer can not have the functional group of sufficient amount and high-load linking agent to carry out bond, and causes by the tackyness of the formed viscose of sticking agent constituent bad.
The weight average molecular weight of acrylic copolymer can be 500,000 to 2,000,000, and preferable 800,000 to 1,800,000, better 1,000,000 to 1,500,000.When the weight average molecular weight of acrylic copolymer less than 500,000 the time, can be bad by the tackyness of the formed viscose of sticking agent constituent, and it is not durable to stick together effect.When the weight average molecular weight of acrylic copolymer greater than 2,000,000 the time, viscose can reduce with respect to the retractility of base material.
Tool crosslinkable functional group and contain the ethene functional group and/or vinylformic acid functional group's the optional freedom of monomer (methyl) vinylformic acid 2-hydroxyl ethyl ester, (methyl) vinylformic acid 2-hydroxypropyl acrylate, (methyl) vinylformic acid 2-hydroxyl ethylene glycol, (methyl) vinylformic acid 2-hydroxyl propylene glycol, (methyl) vinylformic acid, acrylic acid dimer, methylene-succinic acid, maleic acid and group that MALEIC ANHYDRIDE constituted or above-mentioned combination.The main body of (methyl) Acrylic Acid Monomer is (methyl) Acrylic Acid Monomer, and wherein methyl is not essential.(methyl) Acrylic Acid Monomer can comprise that having the alkyl carbon number is (methyl) Acrylic Acid Monomer of 1 to 12, for example, optional freedom (methyl) methyl acrylate, (methyl) vinylformic acid ethyl ester, (methyl) n-butylacrylate, (methyl) vinylformic acid sec-butyl ester, (methyl) vinylformic acid tertiary butyl ester, (methyl) vinylformic acid isobutyl, (methyl) vinylformic acid polyhexamethylene, (methyl) vinylformic acid 2-second polyhexamethylene, (methyl) vinylformic acid n-octyl ester, (methyl) isooctyl acrylate ester, (methyl) vinylformic acid n-nonyl ester, the different nonyl ester of (methyl) vinylformic acid, the positive decyl ester of (methyl) vinylformic acid, group that (methyl) vinylformic acid isodecyl ester and the positive ten dicarbonyl esters of (methyl) vinylformic acid are constituted or above-mentioned combination, but be not limited thereto, and more can comprise having alkyl carbon number (methyl) Acrylic Acid Monomer more than 12.
First solvent has good solubleness for the sticking agent constituent, also to having good solubleness by the formed viscose of sticking agent constituent (or vinylformic acid pressure-sensitive viscose).Therefore, first solvent is for dissolving the solvent of sticking agent constituent or viscose (or vinylformic acid pressure-sensitive viscose) fully.The solubility coefficient of the solubility coefficient of first solvent and sticking agent constituent or viscose (or vinylformic acid pressure-sensitive viscose) is close.The solubility coefficient of the solubility coefficient of first solvent and viscose (or vinylformic acid pressure-sensitive viscose) is preferable to differ positive and negative below 2.The optional free methyl acetate of first solvent, acetone, toluene, ethyl acetate, group that ethanol, benzene, tetrahydrofuran (THF), chloroform, Virahol and methylene dichloride constituted or above-mentioned combination.In an embodiment, the solubleness of viscose (or vinylformic acid pressure-sensitive viscose) is about 8.7～11.0, and this moment, first solvent was to use ethyl acetate (9.1) or acetone (9.8) equal solvent.
Have the optional free acetate of second solvent, dimethyl formamide, dimethyl sulfoxide (DMSO) of the low-volatile characteristic of high boiling point, group that propyl carbinol and butylacetate, isobutyl acetate, dimethylbenzene, chlorobenzene, butanols, ethylene glycol, aniline, mibk and pentyl acetate constituted or above-mentioned combination.Because the evaporation rate of first solvent is fast, and acrylic copolymer is separated out in solvent, so embodiments of the invention use second solvent can slow down the evaporation rate of the solvent of sticking agent constituent, and suppress separating out of acrylic copolymer.Therefore the sticking agent constituent has long using and the activity duration (pot life), with working properties preferably.But the usage ratio of second solvent is restricted.If use too many second solvent, the sticking agent constituent can become, and evaporation rate is crossed slowly and the easy incomplete problem of volatilization that takes place.The usage ratio of second solvent can be described afterwards.
In an embodiment of the present invention, linking agent comprises isocyanate-based linking agent or metal-chelating system linking agent.
The isocyanate-based linking agent can use for example isocyanate-monomer of tolylene diisocyanate, chlorobenzene vulcabond, HDI, tetramethylene vulcabond, isophorone diisocyanate, xylylene vulcabond, diphenylmethanediisocyanate or hydrogenation diphenylmethanediisocyanate etc., and these isocyanate-monomers are carried out isocyanate compound, cyamelide esterification thing or biuret (biuret) the type compound that addition reaction became with TriMethylolPropane(TMP) etc.Perhaps also can use the isocyanic ester of addition reaction amine ester prepolymer types such as polyether glycol, polyester polyol, acrylic polyol, polybutadiene polyol, polyisoprene polyvalent alcohol etc.
Metal-chelating system linking agent comprises the compound of polyvalent metal coordination in methyl ethyl diketone or methyl aceto acetate with aluminium, iron, copper, zinc, tin, titanium, nickel, antimony, magnesium, vanadium, chromium or zirconium.
In an embodiment, isocyanate-based linking agent and metal-chelating system linking agent use simultaneously.With respect to 100 parts by weight of acrylic based copolymers, the isocyanate-based linking agent is 0.1～10 weight part, preferable 0.5～2 weight part.With respect to 100 parts by weight of acrylic based copolymers, metal-chelating system linking agent is 0.1～10 weight part, preferable 0.5～2 weight part.Utilize the isocyanate-based linking agent and the metal-chelating system linking agent of aforementioned proportion can make the adhering layer that forms by the sticking agent constituent have excellent initial gluing property and the durable gluing property.In addition, the adhering layer that is formed by the sticking agent constituent has good viscoelasticity, can avoid changing because of substrate size the situation of the stress concentration that is caused.For instance, when adhering layer is when sticking together on Polarizer, adhering layer does not have because the Polarizer dimensional change causes stress concentration, and the problem of light leak or irregular colour takes place.When isocyanate-based linking agent and metal-chelating system linking agent surpassed above-mentioned scope, the initial stage gluing property of adhering layer can significantly reduce, and made to be difficult to the two substrates of fitting, and for example polaroid can be difficult for being attached on the glass substrate.And, then can't improve light leakage phenomena when isocyanate-based linking agent or metal-chelating system linking agent during less than above-mentioned scope, also can not get sufficient weather resistance.
In an embodiment of the present invention, the sticking agent constituent also comprises silane coupling agent.Can use silane coupling agent for example ethene Trimethoxy silane, vinyl triethoxysilane, methacryloxypropyl trimethoxy silane etc. contain the polymerizability unsaturated group compound of Siliciumatom; 3-glycidoxypropyltrime,hoxysilane, 3-glycidoxy propyl group methyl dimethoxysilane, 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane etc. contain the silicon compound of epoxy construction; Or one of them or any two above combinations of the silicon compound of 3-aminocarbonyl propyl Trimethoxy silane, N-(2-amido ethyl)-3-aminocarbonyl propyl Trimethoxy silane, N-(2-amido ethyl)-amino-containeds such as 3-aminocarbonyl propyl methyl dimethoxysilane and 3-r-chloropropyl trimethoxyl silane etc.
With respect to 100 parts by weight of acrylic based copolymers, silane coupling agent is 0.001～2 weight part, preferable 0.1～1 weight part.Use silane coupling agent can make adhering layer have good bonding stability, and good heat-resisting and wet fastness.Even when exposing to the open air for a long time in high temperature and high humidity environment, adhering layer still has the bonding reliability.Utilize the silane coupling agent of aforementioned proportion can make the adhering layer of formation meet the weather resistance that the Polarizer purposes is required.When silane coupling agent surpasses above-mentioned scope, not only optics or endurance quality there are not too big improvement, can cause extra cost waste on the contrary.When silane coupling agent was lower than above-mentioned scope, the weather resistance of the adhering layer of formation had inadequate problem.
In an embodiment of the present invention, total solvent can more comprise the 3rd solvent, for example hexane or normal heptane.
In an embodiment of the present invention, in the gross weight of first solvent, second solvent and the 3rd solvent, the weight of first solvent accounts for 80～99%, preferablely account for 85～95%, the weight of second solvent accounts for 1～20%, and the weight of preferable the 5～15%, the 3rd solvent accounts for 0.01～10%.
The sticking agent constituent that obtains removes total solvent to become adhering layer after can and carrying out polyreaction at thorough mixing.For example, the preparation of adhering layer can be via coating sticking agent constituent on substrate, and is dried removing total solvent, and forms adhering layer on substrate.The cross-linking density of adhering layer is greater than 85%, and preferable 88～93%.
The adhering layer that is formed by the sticking agent constituent of embodiments of the invention can be applicable in the optical component of flat display apparatus, for example Polarizer in the liquid-crystal display, phase reflectance coating, optical compensation films, and optical characteristics that can lifting gear.
For foregoing of the present invention can be become apparent, embodiment cited below particularly is described in detail below:
[preparation acrylic copolymer]
The hydroxyethyl methylacrylate of 94.7 parts by weight of acrylic butyl esters, 4 parts by weight of acrylic, 1 weight part, the ethyl acetate of 185 weight parts and the Diisopropyl azodicarboxylate (AIBN) of 0.1 weight part are put into the four-hole reactor.After with the air in the nitrogen replacement reaction vessel, stirring reaction solution in nitrogen environment, and reaction soln is warming up to 60 ℃.After reaction 10 hours, obtain solid composition and account for (the acrylate copolymer solution (1) of (94.7+4+1)/((94.7+4+1)+0.1+185)=) 35% (w/w).Record the weight average molecular weight (Mw) about 1,500,000 of acrylate copolymer solution by GPC.
[embodiment 1]
In 130 parts by weight of acrylic ester copolymer solution (1), add solvent: the butylacetate of the ethyl acetate of 110 weight parts and 10 weight parts, and obtain the solution (2) that solid composition accounts for ((0.35*130)/(130+120))=18% (w/w).This moment solvent ethyl acetate weight (110+130* (1-35%)): the weight of butylacetate (10) is 95: 5.Be used as 100 weight parts with respect to the solid composition of the acrylate copolymer in the solution (2), in solution (2), add the isocyanate-based linking agent (AD75 of 0.72 weight part, TDI series, manufacturers is Superchimici S.P.A.), the metal-chelating system linking agent (CA190T of 0.72 weight part, the aluminum metal inner complex, manufacturers is I-TAI Chemicals Inc.) and the silane coupling agent (GLYMO of 0.036 weight part, epoxy radicals silicone hydride series, manufacturers is Evonik (Degussa)), after filling part mixing, obtain the sticking agent constituent.
The sticking agent constituent is coated on the PET of release processing film.Then 90 ℃ down oven dry 5 minutes so that solvent evaporates and form the adhering layer of 20 μ m.Then, the PET that will have adhering layer is film adhered on polaroid, places 7 days under 25 ℃, the condition of humidity 65%, to obtain the adhesive type optical component.
[embodiment 2]
Similar to embodiment one, wherein changing solvent is ethyl acetate 80 weight parts and butylacetate 41 weight parts, so the weight of this routine ethyl acetate: the weight of butylacetate is 80: 20.
[embodiment 3]
Similar to embodiment one, wherein changing solvent is ethyl acetate 39 weight parts, butylacetate 41 weight parts and acetone 41 weight parts.The weight of this routine acetone: the weight of ethyl acetate: the weight of butylacetate is 20: 60: 20.
[embodiment 4]
Similar to embodiment one, wherein changing solvent is ethyl acetate 80 weight parts, butylacetate 21 weight parts and acetone 21 weight parts.The weight of this routine acetone: the weight of ethyl acetate: the weight of butylacetate is 10: 80: 10.
[embodiment 5]
Similar to embodiment one, wherein changing solvent is ethyl acetate 80 weight parts, butylacetate 21 weight parts and normal hexane 21 weight parts.The weight of this routine hexane: the weight of ethyl acetate: the weight of butylacetate is 10: 80: 10.
[embodiment 6]
Similar to embodiment one, wherein changing solvent is ethyl acetate 80 weight parts, butylacetate 21 weight parts and heptane 21 weight parts.The weight of this routine heptane: the weight of ethyl acetate: the weight of butylacetate is 10: 80: 10.
[comparative example 1]
Similar to embodiment one, wherein changing solvent is ethyl acetate 80 weight parts and normal hexane 41 weight parts.The weight of this routine hexane: the weight of ethyl acetate is 20: 80.
[comparative example 2]
Similar to embodiment one, wherein changing solvent is that ethyl acetate is 80 weight parts and normal heptane 41 weight parts.The weight of this routine heptane: the weight of ethyl acetate is 20: 80.
[comparative example 3]
Similar to embodiment one, wherein changing solvent is ethyl acetate 39 weight parts, toluene 41 weight parts and normal heptane 41 weight parts.The weight of this routine normal heptane: the weight of toluene: the weight of ethyl acetate is 20: 20: 60.
[comparative example 4]
Similar to embodiment one, wherein changing solvent is ethyl acetate 39 weight parts, toluene 41 weight parts and normal hexane 41 weight parts.The weight of this routine normal hexane: the weight of toluene: the weight of ethyl acetate is 20: 20: 60.
[comparative example 5]
Similar to embodiment one, wherein changing solvent is ethyl acetate 39 weight parts, butylacetate 41 weight parts and normal hexane 41 weight parts.The weight of this routine normal hexane: the weight of ethyl acetate: the weight of butylacetate is 20: 60: 20.
[comparative example 6]
Similar to embodiment one, wherein changing solvent is ethyl acetate 39 weight parts and toluene 82 weight parts.The weight of this routine toluene: the weight of ethyl acetate is 40: 60.
[comparative example 7]
Similar to embodiment one, wherein changing solvent is ethyl acetate 39 weight parts and butylacetate 82 weight parts.The weight of this routine toluene: the weight of ethyl acetate is 40: 60.
[comparative example 8]
Similar to embodiment one, wherein changing solvent is butylacetate 120 weight parts.This routine solvent is all used ethyl acetate.
[character assessment]
Below the character of the material that is prepared into by the condition of various testing evaluation embodiment 1 to 6 and comparative example 1 to 8.
1.[rate of volatilization]
Calculate in the sticking agent constituent, solvent evaporates weight is for originally weighing gross weight 40% required time of (comprising all solvents and (methyl) acrylate copolymer).
The result is presented in the table 1, and appraisal procedure is:
X: required time is following person 11.7 minutes (comprising).
Zero: required time is above, person below 20 minutes 11.8 minutes (comprising).
The speed of sticking agent constituent rate of volatilization can influence the effect of coating.If the rate of volatilization of sticking agent constituent fast (time is short), and the coating action would be fast inadequately, punctual, can be very easy to take place problems such as blob of viscose, tree lace.And if the rate of volatilization of sticking agent constituent slow (time is long) then has to be difficult for doing and for example to cause character problem of unstable such as adhesion.As shown in Table 1, the rate of volatilization of the sticking agent constituent of embodiment 1～6 is moderate.
2.[viscosity]
Under 25 ℃, use viscosmeter PRO II, with the condition of rotor S63, torsion 50～90%, measure the viscosity of sticking agent constituent and get.
The result is presented in the table 1, and appraisal procedure is:
X: greater than 5000cps (centipoise).
Zero: less than 5000cps.
When the viscosity of sticking agent constituent during, represent that it has good coating less than 5000cps.And, then have the problem that mixing, coating and processing are difficult for when viscosity during greater than 5000cps.
3.[can use or the activity duration (pot life)]
(methyl) acrylate copolymer, solvent, linking agent and silane coupling agent are put into diameter 4.8cm, height 9.5cm transparent vessel, (end face of solution is about 2.0～2.5cm) from bottleneck in the bottle, leaves standstill and observe its whole required time of white atomizing to prevent a bottle internal solvent volatilization for the enclosing cover upper cover after stir.
The result is presented in the table 1, and appraisal procedure is:
X: less than 12 hours
△: 12～24 hours
Zero: greater than 24 hours
In the process of preparation sticking agent constituent, what have aqueous vapor and enter in the reaction environment, or solvent itself contains moisture.The white atomizing takes place, as if use the not good problem of display effect that can cause in optical component if react with the sticking agent constituent in aqueous vapor easily in coating process.The composition of degree, speed and the sticking agent constituent of aqueous vapor and the reaction of sticking agent constituent has relation.As shown in Table 1, the sticking agent constituent of embodiment 1 to 6 is difficult for producing reaction with aqueous vapor.
4.[initial stage adhesion (pulling force) test]
Adhesion is by puller system (Dachang is made by wide rhenium instrument) test.The PET adhesive film that has adhering layer on the surface is cut into the wide long strip type test piece of 25mm.After release film in the test piece removed, using 2Kg spreading roller to make test piece stick together face, to stick in TN on glass, and after under the environment of 23 ± 1 ℃/50 ± 2%RH (relative humidity), placing 20 minutes, utilize puller system to measure test piece and stick together 180 degree adhesions in the face of glass with the speed that draws high of 300mm/min.
The result is presented in the table 1, and appraisal procedure is:
X: less than 500gf/25mm
Zero: greater than 500gf/25mm
The adhesion of test piece is represented the adhesion deficiency less than 500gf/25mm, the element that may cause the sticking agent attaching rocks the top in being transported to the client way quite makes sticking agent separate with element, or presents the phenomenon of peeling off because of temperature contrast in airtight high temperature transportation means.As shown in Table 1, the adhering layer of embodiment 1 to 6 has excellent adhesion (greater than 500gf/25mm), even therefore under hot and humid harsh environment, still can avoid the risk of peeling off.
5.[gel fraction]
After the oven dry of sticking agent constituent, get the sample of suitable weight and put into ethyl acetate immersion 24 hours, filter with filter screen then.To there be residue filter screen from the teeth outwards to place in 110 ℃ the baking oven after 2 hours, the weight of residue (with whole filtering net (the comprising residue) weighing of taking away, then the weight that obtains being deducted the original weight of filter screen (before filtering)) is promptly obtained gel fraction divided by the weight of primary sample.
The result is presented in the table 1, and appraisal procedure is:
X: less than 80%
Zero: greater than 80%
Gel fraction is bigger, and the cross-linking density between the expression sticking agent is higher.Cross-linking density is high more, is entangled with manyly more, and the intensity of glue is strong more, and therefore the back is difficult for producing the space under hot and humid environment, and produces the defect problem of foaming etc.
The solvent composition of table 1 embodiment and comparative example and the character of material
Though the present invention discloses as above with preferred embodiment; right its is not in order to qualification the present invention, any those who are familiar with this art, without departing from the spirit and scope of the present invention; when can doing a little change and retouching, so protection scope of the present invention is as the criterion when looking the claim person of defining.
Claims (17)
1. sticking agent constituent is characterized in that this sticking agent constituent comprises:
Acrylic copolymer;
Total solvent comprises first solvent and second solvent, and wherein the boiling point of this second solvent is higher than 111 degree Celsius; And
Linking agent;
Wherein this sticking agent constituent can form viscose after carrying out polymerization, and this first solvent has good solubleness for this viscose;
The weight of this first solvent: the weight of this second solvent is 80～99: 1～20.
2. sticking agent constituent as claimed in claim 1 is characterized in that this acrylic copolymer is formed by the following material of copolymerization:
(a) Acrylic Acid Monomer or methacrylic acid monomer 85 to 99.5 weight parts; And
(b) tool crosslinkable functional group and contain the ethene functional group and/or vinylformic acid functional group's monomer 0.5 to 15 weight part, wherein (a) with (b) add up to totally 100 weight parts.
3. sticking agent constituent as claimed in claim 2 is characterized in that this tool crosslinkable functional group and contains the ethene functional group and/or vinylformic acid functional group's monomer is to be selected from by vinylformic acid 2-hydroxyl ethyl ester, methacrylic acid 2-hydroxyl ethyl ester, methacrylic acid 2-hydroxypropyl acrylate, vinylformic acid 2-hydroxypropyl acrylate, methacrylic acid 2-hydroxyl ethylene glycol, vinylformic acid 2-hydroxyl ethylene glycol, methacrylic acid 2-hydroxyl propylene glycol, vinylformic acid 2-hydroxyl propylene glycol, methacrylic acid, vinylformic acid, acrylic acid dimer, methylene-succinic acid, maleic acid and group that MALEIC ANHYDRIDE constituted or above-mentioned combination.
4. sticking agent constituent as claimed in claim 1 is characterized in that this sticking agent constituent is applied to optical component.
5. sticking agent constituent as claimed in claim 1 is characterized in that this second solvent is selected from by acetate, dimethyl formamide, dimethyl sulfoxide (DMSO), group that propyl carbinol, butylacetate, isobutyl acetate, dimethylbenzene, chlorobenzene, butanols, ethylene glycol, aniline, mibk and pentyl acetate constituted or above-mentioned combination.
6. sticking agent constituent as claimed in claim 1 is characterized in that the boiling point of this second solvent is higher than the boiling point of this first solvent.
7. sticking agent constituent as claimed in claim 1, the weight average molecular weight that it is characterized in that this acrylic copolymer is 500,000 to 2,000,000.
8. sticking agent constituent as claimed in claim 1 is characterized in that this total solvent also comprises the 3rd solvent, and the 3rd solvent comprises hexane or normal heptane.
9. sticking agent constituent as claimed in claim 8 is characterized in that the weight of the 3rd solvent accounts for 0.01～10% in the gross weight of this first solvent, this second solvent and the 3rd solvent.
10. sticking agent constituent as claimed in claim 1, it is characterized in that the weight of this first solvent: the weight of this second solvent is 85～95: 5～15.
11. sticking agent constituent as claimed in claim 1, it is characterized in that this linking agent comprises isocyanate-based linking agent or metal-chelating system linking agent, this sticking agent constituent also comprises silane coupling agent, wherein with respect to this acrylic copolymers of 100 weight parts, this isocyanate-based linking agent is 0.1～10 weight part, or this metal-chelating system linking agent is 0.1～10 weight part, or this silane coupling agent is 0.001～2 weight part.
12. sticking agent constituent as claimed in claim 11 is characterized in that this acrylic copolymer with respect to 100 weight parts, this silane coupling agent is 0.1～1 weight part.
13. sticking agent constituent as claimed in claim 11 is characterized in that this acrylic copolymer with respect to 100 weight parts, this isocyanate-based linking agent is 0.5～2 weight part, and this metal-chelating system linking agent is 0.5～2 weight part.
14. sticking agent constituent as claimed in claim 11 is characterized in that this isocyanate-based linking agent and this metal-chelating system linking agent use simultaneously.
15. sticking agent constituent as claimed in claim 1 is characterized in that this first solvent is to be selected from by methyl acetate, acetone, toluene, ethyl acetate, group that ethanol, benzene, tetrahydrofuran (THF), chloroform, Virahol and methylene dichloride constituted or above-mentioned combination.
16. sticking agent constituent as claimed in claim 1, it is characterized in that the weight of this acrylic copolymer: the weight of this total solvent is 18: 82.
17. an adhering layer is characterized in that this adhering layer is formed by following method:
Provide as any described sticking agent constituent among the claim 1-16; And
This sticking agent constituent is carried out polymerization and solvent evaporates is fallen, to obtain this adhering layer.
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| CN103635546A (en) * | 2011-08-18 | 2014-03-12 | 藤仓化成株式会社 | Coating composition for chromium thin film coating |
| TWI575043B (en) * | 2014-02-21 | 2017-03-21 | 藤森工業股份有限公司 | Adhesive composition and surface protection film |
| WO2020177111A1 (en) * | 2019-03-07 | 2020-09-10 | Dow Global Technologies Llc | Formaldehyde free adhesive composition |
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| CN101429416A (en) * | 2007-11-07 | 2009-05-13 | 3M新设资产公司 | Adhesion agent composition for environment-friendly water transfer printing volume label |
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| CN1281883A (en) * | 2000-06-13 | 2001-01-31 | 湖北省化学研究所 | Multi-component copolymer acrylate adhesive, its preparation method and application for covering aluminium plate with polyimide |
| US20060035071A1 (en) * | 2004-08-10 | 2006-02-16 | Tdk Corporation | Release layer paste and method of production of multilayer type electronic device |
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| CN103635546A (en) * | 2011-08-18 | 2014-03-12 | 藤仓化成株式会社 | Coating composition for chromium thin film coating |
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| TWI575043B (en) * | 2014-02-21 | 2017-03-21 | 藤森工業股份有限公司 | Adhesive composition and surface protection film |
| WO2020177111A1 (en) * | 2019-03-07 | 2020-09-10 | Dow Global Technologies Llc | Formaldehyde free adhesive composition |
| CN111918945A (en) * | 2019-03-07 | 2020-11-10 | 陶氏环球技术有限责任公司 | Formaldehyde-free binder composition |
| US11485886B2 (en) | 2019-03-07 | 2022-11-01 | Dow Global Technologies Llc | Formaldehyde free adhesive composition |
| CN111918945B (en) * | 2019-03-07 | 2023-04-21 | 陶氏环球技术有限责任公司 | Formaldehyde-free adhesive composition |
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