CN103865470A - Light-curing edge sealing adhesive - Google Patents
Light-curing edge sealing adhesive Download PDFInfo
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- CN103865470A CN103865470A CN201410048908.XA CN201410048908A CN103865470A CN 103865470 A CN103865470 A CN 103865470A CN 201410048908 A CN201410048908 A CN 201410048908A CN 103865470 A CN103865470 A CN 103865470A
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Abstract
The invention discloses a light-curing adhesive and in particular relates to an ultraviolet-curing adhesive. The light-curing adhesive comprises the following components in percentage by mass: 10%-75% of matrix resin, 5%-50% of auxiliary resin, 10%-70% of activated monomer of acrylate, allyl compound or vinyl compound, 5%-15% of adhesion accelerator, 1%-10% of photoinitiator and 0.5-10% of auxiliary agent. The light-curing adhesive provided by the invention has fast curing capability, high bonding strength and low internal stress; an obtained cured layer is soft and has excellent hydrofluoric acid resistance.
Description
Technical field
This reality invention relates to a kind of ultraviolet photo-curing cementing agent, especially relates to the curable adhesive that etching attenuate that one is applied to the liquid-crystalline glasses of flat-panel monitor (FPD) is used.
Background technology
In flat pannel display field, liquid-crystalline glasses is widely used in the display screen of mobile phone, TV, panel computer etc., liquid-crystalline glasses generally forms single liquid crystal layer by colorized optical filtering face, TFT face and liquid crystal layer, and two-layer single liquid crystal layer is bonded together and forms a complete LCD Panel.
Mobile phone, panel computers etc. are high to the thickness requirement of liquid crystal display, and the general first liquid crystal display thickness preparing is larger, need to carry out reduction processing.The method of reduction processing is with hydrofluoric acid etch, because adopting double-sided adhesive, liquid-crystalline glasses screen forms, when hydrofluoric acid etch, easily invade liquid crystal display inside from gap, destroy liquid crystal display, so, before etching, need the limit of liquid-crystalline glasses to carry out encapsulation process, use photocuring edge sealing adhesive, under 365nm ultraviolet ray, irradiate, while irradiating UV glue, produce polyreaction, make UV glue produce the effect of solidifying sclerosis, thereby liquid-crystalline glasses four bandings are stopped.If there is defect in UV glue in coating process, can cause the bonding effect on liquid-crystalline glasses four limits not good, cause acid solution to invade liquid crystal display inside in the process of acid etching, destroy liquid crystal display; In addition, in the process of lapping after liquid-crystalline glasses etching due to the ununiformity of glue bond and tensile strength is low etc. during performance also can cause process of lapping liquid-crystalline glasses unbalance stress and breakage.
Liquid-crystalline glasses is generally light transmissive material, there is high energy surface, more bonding than being easier to, but liquid-crystalline glasses surface is easier to again adsorption moisture, even bonding rear moisture and moisture also can be invaded glass interface, replace bonding effect, or make glued membrane water suction plasticizing, second-order transition temperature, cohesive strength and bonding strength decline, thereby adhesive failure occurs.Some curable adhesive, in order to reach better higher bonding strength, uses in a large number adhesion promoters in formula.These promotor are generally phosphoric acid ester, and polarity is large, show as initial bond strenght high especially, but excessive polar group has strengthened water-intake rate, cause permanent adhesive effect decay larger, can not ensure lasting high-adhesive-strength.
Temperature is high to be had a significant impact curable adhesive, and temperature raises, and can accelerate the oxicracking effect of compound, and hydrolytic action etc. also can cause actual bonding result to decline.
The viscosity of photocuring edge sealing adhesive can affect the bonding effect on liquid-crystalline glasses four limits, if viscosity is lower, infiltrate the gap between glass though be conducive to UV glue, but can affect the adhesive property between glass, cause the loss of adhesion of glass and glue, and in a glue process due to glass between inside and outside pressure reduction can cause Bubble formation, need twice glue to eliminate bubble or repair bubble with full-bodied UV glue; If viscosity is too high, though can increase the sticking power of glass and UV glue, in some glue process, there will be disconnected glue phenomenon, thus and the slow production efficiency that affects of the speed in UV glue infiltration glass gap.Existing UV cure shrinkage is higher in addition, can cause the flexibility of cured film poor on the one hand, and tensile strength is lower, causes the glue at some position and glass to peel off consequently acid solution intrusion liquid crystal display inside in actual handling process; Also can cause on the other hand the edge toothing shape of cured film, this phenomenon can cause in follow-up grinding technics bonding position unbalance stress due to glass and glue so that glass breakage.
Summary of the invention
Technical problem to be solved by this invention is: a kind of tackiness agent in dull and stereotyped liquid-crystalline glasses thinning process with the good ultraviolet light polymerization that hydrofluoric acid resistant performance, bonding strength are high, effect is lasting is provided.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of photocuring edge sealing adhesive, by quality percentage composition, its component comprises: matrix resin 10～75%, assisted resin 5～50%, reactive monomer 10～70%, adhesion promoter 5～15%, light trigger 1～10%, auxiliary agent 0.5～10%;
Described matrix resin is a kind of or any two or more mixture in polyether based polyurethanes acrylate, epoxy acrylate, urethane acrylate, PBAA ester;
Described assisted resin is urethane acrylate or epoxy acrylate;
Described reactive monomer is simple function group acrylate, bifunctional acrylate, multi-functional acrylate, simple function group allylic cpd, bifunctional allylic cpd, polyfunctional group allylic cpd, simple function group vinyl compound, bifunctional vinyl compound, a kind of or any two or more mixture in polyfunctional group vinyl compound.
By quality percentage composition, its component comprises: matrix resin 35～60%, assisted resin 8～30%, reactive monomer 20～45%, adhesion promoter 6～10%, light trigger 2～8%, auxiliary agent 1～5%.
Described photocuring edge sealing adhesive also comprises pigment or dyestuff 0.5～8wt%.
Described matrix resin provides the essential property of curable adhesive, there is suitable cohesiveness and acid resistance and stability, the present invention selects polyether based polyurethanes acrylate, epoxy acrylate, urethane acrylate or PBAA ester as matrix resin, this resinoid has suitable cementability and stability, simultaneously the normal more suitable matrix resin as tackiness agent of polyester urethane acrylate using in the relative prior art of its acid and alkali-resistance water tolerance.Polyether based polyurethanes acrylate is prepared by polyether polyhydroxy-compound, isocyanic ester, vinylformic acid and acrylate.Polyether polyhydroxy-compound uses conventional polyether glycol, for example polyoxyethylene glycol, polypropylene glycol etc.; Isocyanic ester is 2,4 toluene diisocyanate or isofoer diisocyanate; Crylic acid hydroxy ester is Hydroxyethyl acrylate (HEMA) and vinylformic acid (HPMA); Urethane acrylate can increase and solidify kindliness, the contraction of reduction stress of figure layer, improve sticking power; Epoxy acrylic methyl esters has higher rigidity, tensile strength and thermostability; PBAA ester has good moisture-proof effect, also has good resistance to low temperature simultaneously.
Described assisted resin is urethane acrylate or epoxy acrylate.Assisted resin adds for the bulk property of adjusting tackiness agent, has made up some deficiency of matrix resin, for example tensile strength, high temperature resistant character, hardness etc.
Described matrix resin and the functionality of assisted resin are 2～9, and the number-average molecular weight of matrix resin and assisted resin is 500～10000.The modest viscosity of these resins, solidification process shrinking percentage is lower, has good film forming and adhesion property.The commercial prod of these resins has CN117, CN118, CN962, CN966J75, CN985B88 of Sartomer company etc., 6134A-80,615-100, the 6141H-80 etc. of Changxing chemical company, the Photomer6230 of Cognis company etc.
Further preferred CN962, CN966J75, CN985B88 and/or the 6134A-80 of described resin.
The effect of described reactive monomer is regulation system viscosity, the wettability of promoting tackiness agent and glass, improves curing speed and improve the various performances of solidifying front and back material, as snappiness, hardness etc.In the present invention, reactive monomer is selected from simple function group acrylate, bifunctional acrylate, multi-functional acrylate, simple function group allylic cpd, bifunctional allylic cpd, polyfunctional group allylic cpd, simple function group vinyl compound, bifunctional vinyl compound, polyfunctional group vinyl compound and two or more combination arbitrarily thereof.Simple function group monomer containing functional group can improve adhesive property in UV cured adhesive, and polyfunctional monomer can improve adhesive property by improving cross-linking density.
Described reactive monomer is one or more in following compound: simple function group reactive monomer is as (methyl) 2-ethylhexyl acrylate, (methyl) isobornyl acrylate, (methyl) lauryl acrylate, (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, (methyl) vinylformic acid phenoxy group ethyl ester, (methyl) vinylformic acid ethoxy ethoxy ethyl ester, NVP etc., bifunctional reactive monomer is as (methyl) vinylformic acid ethylene glycol bisthioglycolate (methyl) acrylate, butyleneglycol two (methyl) acrylate, hexylene glycol two (methyl) acrylate, tetraethylene-glycol two (methyl) acrylate, dicyclopentadiene acrylate, tripropylene glycol two (methyl) acrylate, polyoxyethylene glycol (200) two (methyl) acrylate, polyoxyethylene glycol (400) two (methyl) acrylate, polyoxyethylene glycol (600) two (methyl) acrylate, polyoxyethylene glycol (800) two (methyl) acrylate, trimethylolpropane allyl ether, polyfunctional group reactive monomer as trimethylolpropane tris (methyl) acrylate, ethoxylated trimethylolpropane three (methyl) acrylate, Viscoat 295, propoxylation trimethylolpropane tris (methyl) acrylate, tetramethylolmethane three (methyl) acrylate, pentaerythritol triallyl ether, two seasons penta 6 alcohol five (methyl) acrylate etc., and some commercial specific functional groups acrylate are as the Photomer4039(phenolic group oxyethyl group 3EO mono acrylic ester of Cognis company), the CD9050(monofunctional acrylate of Sartomer company) etc.
One or more in the preferred Viscoat 295 of described reactive monomer, dicyclopentadiene acrylate, trimethylolpropane tris (methyl) acrylate, ethoxylated trimethylolpropane three (methyl) acrylate, propoxylation trimethylolpropane tris (methyl) acrylate, tetramethylolmethane three (methyl) acrylate, two seasons penta 6 alcohol five (methyl) acrylate; This compounds has good water tolerance.
Described adhesion promoter is selected from vinylformic acid hydroxyalkyl acrylate, vinylformic acid, containing the acrylate of carboxyl functional group, containing one or more the mixture in the phosphoric acid ester adhesion promoter of unsaturated functional group.
Described light trigger is selected from scission reaction photoinitiator, hydrogen and eliminates one or more the mixture in reaction mechanism light trigger, visible light initiator or radical photoinitiator.
Described scission reaction photoinitiator is as benzoin ether, benzil ketals, methyl phenyl ketone, acyl group phosphorus oxide light trigger, described hydrogen is eliminated reaction mechanism light trigger as benzophenone and tertiary amine title complex, thioxanthone and derivative thereof, two imidazoles, described visible light initiator is as camphorquinone, described radical photoinitiator is as st-yrax contracting methyl ether (the trade name Irgacure of CIBA-GEIGY company 651), 1-hydroxy-cyclohexyl phenyl ketone (trade name Irgacure184), 2-hydroxy-2-methyl-1-phenyl-1-acetone (trade name Darocure 1173), 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholine-1-acetone (trade name Irgacure 907), 2, 4, 6-trimethylbenzoyl-diphenyl phosphine oxide (trade name TPO), 2-phenyl benzyl-2-dimethyl amine-1-(4-morpholine benzyl phenyl) butanone (trade name Irgacure369).Preferably Irgacure 369, Irgacure 907 and/or TPO.Light trigger may be used alone, can also be used in combination, and main curing speed, bondline thickness as requested determines.
Described adhesion promoter is one or both in A-172 silane coupling agent, the methacrylic acid phosphoric acid ester of modest 1121 adhesion promoters of moral, Sartomer CD9051, union carbide corporation.Preferably moral modest 1121 or A-172.
Described auxiliary agent is one or more of oxidation inhibitor, flow agent, defoamer, stablizer.Wherein oxidation inhibitor is one or more of hindered phenol compound, phosphite ester compound, thio-based compound and complex class compound; Preferably hindered phenol compound, as BHT, 2246,1010,1076.Stablizer is one or more in ferrocene compounds, anhydrides compound, phenol compound; Ferrocene compounds is ferrocene, methyl ferrocene, ethyl dicyclopentadienyl iron; Anhydrides compound is Tetra hydro Phthalic anhydride, maleic anhydride, succinyl oxide; Phenol compound is Resorcinol, p methoxy phenol, 2,6 ditertiary butyl p cresol.Preferably ferrocene, methyl ferrocene, ethyl dicyclopentadienyl iron, Tetra hydro Phthalic anhydride, Resorcinol and/or p methoxy phenol; The solvent-borne type defoamer 2700 or 3100 of defoamer Shi Deqian company, deaerating agent Airex900 or the Airex920 etc. of Di Gao company.Preferred solvent type defoamer 3100.
Described filler is pigment or dyestuff.
Described pigment is red pigment, veridian or blue pigments.
Described red pigment is pyrene series pigments, anthraquione pigmentss separately or one of them plants pigment and tetrazo is that yellow pigment or India's phosphorus are the mixture of yellow pigment, for example can select the red pigment of following trade(brand)name: Pigment red 7, Pigment red 14, pigment red 41, pigment red 4 8:1, pigment red 4 8:2, pigment red 4 8:3, pigment red 4 8:4, pigment red 146, Pigment red 177, Pigment red 178, Pigment red 184, Pigment red 185, Pigment red 187, Pigment red 200, Pigment red 202, Pigment red 208, pigment red 21 0, Pigment red 246, Pigment red 254, Pigment red 255, Pigment red 264, Pigment red 272 etc.For example can select the yellow ultramarine of following trade(brand)name: Pigment Yellow 73 1, Pigment Yellow 73 2, Pigment Yellow 73 3, Pigment Yellow 73 4, Pigment Yellow 73 5, Pigment Yellow 73 6, Pigment Yellow 73 10, pigment Yellow 12, pigment yellow 13, pigment Yellow 14, Pigment Yellow 73 15, Pigment Yellow 73 16, pigment yellow 17, Pigment Yellow 73 18, Pigment Yellow 73 24, Pigment Yellow 73 31, Pigment Yellow 73 32, pigment yellow 34, Pigment Yellow 73 35, Pigment Yellow 73 35:1, Pigment Yellow 73 36, Pigment Yellow 73 36:1, Pigment Yellow 73 37, Pigment Yellow 73 37:1, Pigment Yellow 73 40, Pigment Yellow 73 42, Pigment Yellow 73 43, Pigment Yellow 73 53, Pigment Yellow 73 55, Pigment Yellow 73 60, C.I. Pigment Yellow 73 61, Pigment Yellow 73 62, Pigment Yellow 73 63, Pigment Yellow 73 65, Pigment Yellow 73 73, Pigment Yellow 73 74, Pigment Yellow 73 77, pigment yellow 81, pigment yellow 83, Pigment Yellow 73 93, Pigment Yellow 73 94, Pigment Yellow 73 95, Pigment Yellow 73 97, Pigment Yellow 73 98, Pigment Yellow 73 100, Pigment Yellow 73 101, Pigment Yellow 73 104, Pigment Yellow 73 106, Pigment Yellow 73 108, Pigment Yellow 73 109, Pigment Yellow 73 110, Pigment Yellow 73 113, Pigment Yellow 73 114, Pigment Yellow 73 115, Pigment Yellow 73 116, Pigment Yellow 73 117, Pigment Yellow 73 118, Pigment Yellow 73 119, pigment Yellow 12 0, pigment Yellow 12 6, pigment Yellow 12 7, pigment Yellow 12 8, pigment Yellow 12 9, pigment yellow 13 8, pigment yellow 13 9, Pigment Yellow 73 150, Pigment Yellow 73 151, Pigment Yellow 73 152, Pigment Yellow 73 153, pigment yellow 154, Pigment Yellow 73 155, Pigment Yellow 73 156, Pigment Yellow 73 161, Pigment Yellow 73 162, Pigment Yellow 73 164, Pigment Yellow 73 166, Pigment Yellow 73 167, Pigment Yellow 73 168, Pigment Yellow 73 169, pigment yellow 17 0, pigment yellow 17 1, pigment yellow 17 2, pigment yellow 17 3, pigment yellow 17 4, pigment yellow 17 5, pigment yellow 17 6, pigment yellow 17 7, pigment yellow 17 9, Pigment Yellow 73 180, Pigment Yellow 73 181, Pigment Yellow 73 182, Pigment Yellow 73 185, Pigment Yellow 73 187, Pigment Yellow 73 191:1, Pigment Yellow 73 199 etc.
Described veridian is that halogenated phthalocyanines series pigments, tetrazo are that yellow pigment or India's phosphorus are the mixture of yellow pigment and halogenated phthalocyanines series pigments; Phthualocyanine pigment is as pigment green 36, and yellow pigment is a kind of or its combination in azo type pigment, azo condensed type pigment, heterocyclic pigment.For example can select the yellow pigment of following trade(brand)name: Pigment Yellow 73 1, Pigment Yellow 73 2, Pigment Yellow 73 3, Pigment Yellow 73 4, Pigment Yellow 73 5, Pigment Yellow 73 6, Pigment Yellow 73 10, pigment Yellow 12, pigment yellow 13, pigment Yellow 14, Pigment Yellow 73 15, Pigment Yellow 73 16, pigment yellow 17, Pigment Yellow 73 18, Pigment Yellow 73 24, Pigment Yellow 73 31, Pigment Yellow 73 32, pigment yellow 34, Pigment Yellow 73 35, Pigment Yellow 73 35:1, Pigment Yellow 73 36, Pigment Yellow 73 36:1, Pigment Yellow 73 37, Pigment Yellow 73 37:1, Pigment Yellow 73 40, Pigment Yellow 73 42, Pigment Yellow 73 43, Pigment Yellow 73 53, Pigment Yellow 73 55, Pigment Yellow 73 60, C.I. Pigment Yellow 73 61, Pigment Yellow 73 62, Pigment Yellow 73 63, Pigment Yellow 73 65, Pigment Yellow 73 73, Pigment Yellow 73 74, Pigment Yellow 73 77, pigment yellow 81, pigment yellow 83, Pigment Yellow 73 93, Pigment Yellow 73 94, Pigment Yellow 73 95, Pigment Yellow 73 97, Pigment Yellow 73 98, Pigment Yellow 73 100, Pigment Yellow 73 101, Pigment Yellow 73 104, Pigment Yellow 73 106, Pigment Yellow 73 108, Pigment Yellow 73 109, Pigment Yellow 73 110, Pigment Yellow 73 113, Pigment Yellow 73 114, Pigment Yellow 73 115, Pigment Yellow 73 116, Pigment Yellow 73 117, Pigment Yellow 73 118, Pigment Yellow 73 119, pigment Yellow 12 0, pigment Yellow 12 6, pigment Yellow 12 7, pigment Yellow 12 8, pigment Yellow 12 9, pigment yellow 13 8, pigment yellow 13 9, Pigment Yellow 73 150, Pigment Yellow 73 151, Pigment Yellow 73 152, Pigment Yellow 73 153, pigment yellow 154, Pigment Yellow 73 155, Pigment Yellow 73 156, Pigment Yellow 73 161, Pigment Yellow 73 162, Pigment Yellow 73 164, Pigment Yellow 73 166, Pigment Yellow 73 167, Pigment Yellow 73 168, Pigment Yellow 73 169, pigment yellow 17 0, pigment yellow 17 1, pigment yellow 17 2, pigment yellow 17 3, pigment yellow 17 4, pigment yellow 17 5, pigment yellow 17 6, pigment yellow 17 7, pigment yellow 17 9, Pigment Yellow 73 180, Pigment Yellow 73 181, Pigment Yellow 73 182, Pigment Yellow 73 185, Pigment Yellow 73 187, Pigment Yellow 73 191:1, Pigment Yellow 73 199 etc., or can use the mixture of one or more pigment.
Described blue pigments is the mixture of halogenated phthalocyanines series pigments, halogenated phthalocyanines series pigments and dioxazines purple pigment; The blue pigments of such as following trade(brand)name: pigment Blue 15: 1, pigment Blue 15: 2, pigment Blue 15: 3, pigment Blue 15: 3, pigment Blue 15: 4, pigment Blue 15: pigment blue 16, pigment blue 17, Pigment blue 21, Pigment blue 22, Pigment blue, Pigment blue 64, Pigment blue 76 etc. 6,, violet pigment is as pigment violet 19, pigment Violet 23.
Described UV photocuring edge sealing adhesive preparation process is: in container, add matrix resin and stablizer, stirring and dissolving, add again reactive monomer and light trigger, stirring and dissolving, then add assisted resin, reactive monomer and auxiliary agent, stirring and dissolving, finally adds defoamer, obtains UV photocuring edge sealing adhesive after mixing and stirring.
Compared with prior art, the present invention has following beneficial effect:
1) the present invention selects a kind of or its mixture in polyether based polyurethanes acrylate, urethane acrylate, epoxy acrylate, PBAA ester as matrix resin, make curable adhesive of the present invention there is suitable cementability and stability, the normal more suitable matrix resin as tackiness agent of urethane acrylate using in the relative prior art of its acid and alkali-resistance water tolerance, wherein the employing of PBAA ester has also increased the lower temperature resistance of curable adhesive of the present invention;
2) assisted resin of the present invention is the bulk property in order to adjust tackiness agent and adding, made up matrix resin in tensile strength, heatproof character, some deficiency of the aspects such as hardness, has obviously improved the performance of the aspect such as tackiness, heatproof of tackiness agent;
3) relative prior art, the present invention has also selected the esters of acrylic acid reactive monomer of water-tolerant, makes curable adhesive of the present invention still retain good bonding strength under high humidity or hot and humid condition;
4) curable adhesive provided by the invention, has the stickiness more better than the curable adhesive of prior art, especially glass is had to high bonding strength, and high-temp resisting high-humidity resisting, and acid resistance excellence, has broad application prospects.
brief description of the drawings
Fig. 1 is crenellated phenomena test comparison figure after solidifying;
Fig. 2 is coating test comparison figure.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with case study on implementation, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
The embodiment of the present invention provides that a kind of more existing edge sealing adhesive bonding strength is higher, the etching attenuate that is applicable to liquid-crystalline glasses, the preparation method that can improve the edge sealing adhesive of yield, comprises the following steps: each raw material of the described edge sealing adhesive of preparation is stirred at the temperature lower than 30 DEG C; The proportioning of each raw material of the described described edge sealing adhesive of preparation is: matrix resin 30～50%, assisted resin 10～30%, reactive monomer 25%～45%, adhesion promoter 6～10%, light trigger 3%～5%, auxiliary agent 2%～5%, pigment or dyestuff 0.5%～5%; The above-mentioned raw materials that preparation is mixed is uniformly mixed at the temperature of 20 DEG C～50 DEG C.
Tested viscosity, if test result does not meet the viscosity threshold value of setting, adjusts viscosity to described viscosity threshold value, the range of viscosities of the edge sealing adhesive that the viscosity threshold value of described setting makes.Viscosity is the significant parameter that determines edge sealing adhesive performance, and viscosity is too large, is unfavorable for the coating of edge sealing adhesive; Cannot prevent that acid solution from impacting and invading liquid crystal inside and viscosity is too little, therefore the viscosity of edge sealing adhesive need meet the viscosity threshold value of setting, and one is preferably in embodiment, and viscosity threshold setting was 300～2000 milli handkerchief seconds.
Embodiment 1
Polyurethane acroleic acid light-cured resin 46%, the light trigger 369 of polyether based polyurethanes acrylate 8%, 1%, trimethylolpropane tris (methyl) acrylate 15%, tetramethylolmethane three (methyl) acrylate 15%, containing the phosphoric acid ester adhesion promoter 6% of unsaturated functional group, auxiliary agent 2% and pigment P.R.2547%, be uniformly mixed and get final product.
Embodiment 2
The edge sealing adhesive that the embodiment of the present invention also provides another edge sealing adhesive preparation method and the method to make, is with difference in embodiment 1, prepares each raw material composition and proportioning (mass percent) difference of this edge sealing adhesive, specific as follows:
Polyether based polyurethanes acrylate 40%, the light trigger 369 of epoxy acrylic 15%, 2%, trimethylolpropane tris (methyl) acrylate 18%, ethoxylated trimethylolpropane three (methyl) acrylate 16%, containing acrylate adhesion promoter 6% and other auxiliary agents 3% of carboxyl functional group, be uniformly mixed and get final product.
Embodiment 3
The embodiment of the present invention also provides the edge sealing adhesive that in the 3rd, edge sealing adhesive preparation method and the method make, and is with the difference part of embodiment 1 and 2, and each raw material composition and the proportioning (mass percent) of preparing this edge sealing adhesive are as follows:
Polyurethane acroleic acid light-cured resin 50%, the light trigger 907 of PBAA ester 15%, 2%, ethoxylated trimethylolpropane three (methyl) acrylate 10%, tetramethylolmethane three (methyl) acrylate 14%, containing the acrylate adhesion promoter 3% of carboxyl functional group, containing phosphoric acid ester adhesion promoter 3% and other auxiliary agents 3% of unsaturated functional group, be uniformly mixed and get final product.
The sealed plastic box that the embodiment of the present invention provides preparation method and makes according to the method, in the time of glue, the disconnected bad incidence of glue is low, the neat in edge of UV glue after solidifying, without crenellated phenomena, and cured film has excellent snappiness and tensile strength, thereby can avoid acid solution to invade liquid crystal display inside, but also can reduce the breakage rate of glass in grinding step, improve the high yield of product.
For the superiority of edge sealing adhesive of the present invention is described better, as shown in Fig. 1～2, edge sealing adhesive that the embodiment of the present invention 1 to 3 provides and existing edge sealing adhesive are listed below and have carried out coating and stripping strength contrast experiment's result.
Concrete test condition is as follows: experiment employing 2.5 generation line liquid-crystalline glasses, in this contrast test experiment, adopt edge sealing adhesive provided by the invention and existing edge sealing adhesive, and some glue process adopts the artificial glue of putting.
Contrast experiment's test result is as follows:
The first, solidify rear crenellated phenomena test comparison result as shown in Figure 1, as can be seen from Figure 1: edge sealing adhesive of the present invention (upper figure) does not have zigzag fashion in the cured film at liquid-crystalline glasses edge; And existing edge sealing adhesive (figure below) has obvious sawtooth pattern in the cured film at liquid-crystalline glasses edge, four limits of whole liquid-crystalline glasses are almost taken.The crenellated phenomena of this degree can cause the bonding unbalance stress of liquid-crystalline glasses and cured film to cause liquid-crystalline glasses that film easily occurs in handling process peeling off with glass, causes acid solution to invade liquid crystal display inner or grind breakage.
The second, as shown in Figure 2, existing edge sealing adhesive (upper figure) there will be the disconnected glue of the discontinuous coating of edge sealing adhesive bad to coating test comparison result in the time of glue, incidence higher (10%～15%); Edge sealing adhesive of the present invention (figure below) in the time applying, the discontinuous coating bad incidence of glue very low (<1%) of breaking.Edge sealing adhesive of the present invention can keep good continuity in coating situation, but, the viscosity of existing edge sealing adhesive is generally large than described viscosity threshold value, with edge sealing adhesive of the present invention in the time that identical coating speed applies, disconnected glue bad phenomenon happens occasionally, and existing edge sealing adhesive can keep good continuity in coating situation.
The 3rd, acid resistance test comparison result is as shown in table 1, and by the acid etch experiment of same level, the resistance to etching time of edge sealing adhesive of the present invention is greater than 80min; And the resistance to etching test same period of traditional edge sealing adhesive average is less than 60min.As can be seen here, edge sealing adhesive bonding strength of the present invention will be higher than existing edge sealing adhesive.
Table 1
| Edge sealing adhesive classification | Embodiment 1 | Embodiment 2 | Embodiment 3 | Existing edge sealing adhesive |
| Acidproof etching time | 90min | 85min | 95min | 50min |
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited to this, any be familiar with those skilled in the art the present invention disclose technical scope in; can expect easily changing or replacing, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (9)
1. a photocuring edge sealing adhesive, by quality percentage composition, its component comprises: matrix resin 10～75%, assisted resin 5～50%, reactive monomer 10～70%, adhesion promoter 5～15%, light trigger 1～10%, auxiliary agent 0.5～10%;
Described matrix resin is a kind of or any two or more mixture in polyether based polyurethanes acrylate, epoxy acrylate, urethane acrylate, PBAA ester;
Described assisted resin is urethane acrylate or epoxy acrylate;
Described reactive monomer is simple function group acrylate, bifunctional acrylate, multi-functional acrylate, simple function group allylic cpd, bifunctional allylic cpd, polyfunctional group allylic cpd, simple function group vinyl compound, bifunctional vinyl compound, a kind of or any two or more mixture in polyfunctional group vinyl compound.
2. a kind of photocuring edge sealing adhesive according to claim 1, is characterized in that: by quality percentage composition, its component comprises: matrix resin 35～60%, assisted resin 8～30%, reactive monomer 20～45%, adhesion promoter 6～10%, light trigger 2～8%, auxiliary agent 1～5%.
3. a kind of photocuring edge sealing adhesive according to claim 1 and 2, is characterized in that: described photocuring edge sealing adhesive also comprises pigment or dyestuff, its quality percentage composition is 0.5～8%.
4. a kind of photocuring edge sealing adhesive according to claim 1 and 2, is characterized in that: described matrix resin and the functionality of assisted resin are 2～9, the number-average molecular weight of matrix resin and assisted resin is 500～10000.
5. according to a kind of photocuring edge sealing adhesive described in claim 1 or 2, it is characterized in that: described reactive monomer is selected from one or more in following substances: (methyl) 2-ethylhexyl acrylate, (methyl) isobornyl acrylate, (methyl) lauryl acrylate, (methyl) Hydroxyethyl acrylate, (methyl) Propylene glycol monoacrylate, (methyl) vinylformic acid phenoxy group ethyl ester, (methyl) vinylformic acid ethoxy ethoxy ethyl ester, NVP etc., (methyl) vinylformic acid ethylene glycol bisthioglycolate (methyl) acrylate, butyleneglycol two (methyl) acrylate, hexylene glycol two (methyl) acrylate, tetraethylene-glycol two (methyl) acrylate, dicyclopentadiene acrylate, tripropylene glycol two (methyl) acrylate, polyoxyethylene glycol two (methyl) acrylate, polyoxyethylene glycol two (methyl) acrylate, polyoxyethylene glycol two (methyl) acrylate, polyoxyethylene glycol two (methyl) acrylate, trimethylolpropane allyl ether, trimethylolpropane tris (methyl) acrylate, ethoxylated trimethylolpropane three (methyl) acrylate, Viscoat 295, propoxylation trimethylolpropane tris (methyl) acrylate, tetramethylolmethane three (methyl) acrylate, pentaerythritol triallyl ether, two seasons penta 6 alcohol five (methyl) acrylate, phenolic group oxyethyl group 3EO mono acrylic ester, monofunctional acrylate.
6. a kind of photocuring edge sealing adhesive according to claim 1 and 2, is characterized in that: described adhesion promoter is selected from vinylformic acid hydroxyalkyl acrylate, vinylformic acid, containing the acrylate of carboxyl functional group, containing one or more the mixture in the phosphoric acid ester adhesion promoter of unsaturated functional group.
7. a kind of photocuring edge sealing adhesive according to claim 1 and 2, is characterized in that: described light trigger is selected from scission reaction photoinitiator, hydrogen and eliminates one or more the mixture in response class light trigger, visible light initiator or free radical photo-initiation.
8. a kind of photocuring edge sealing adhesive according to claim 7, is characterized in that: described light trigger is selected from one or more the mixture in the title complex, thioxanthone, thioxanthone derivative, two imidazoles, camphorquinone of benzoin ether, benzil ketals, methyl phenyl ketone, acylphosphine oxide, benzophenone and tertiary amine.
9. a kind of photocuring edge sealing adhesive according to claim 1, is characterized in that: described auxiliary agent is one or more in oxidation inhibitor, flow agent, defoamer, stablizer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410048908.XA CN103865470B (en) | 2014-02-12 | 2014-02-12 | A kind of photocuring edge sealing adhesive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410048908.XA CN103865470B (en) | 2014-02-12 | 2014-02-12 | A kind of photocuring edge sealing adhesive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103865470A true CN103865470A (en) | 2014-06-18 |
| CN103865470B CN103865470B (en) | 2016-04-06 |
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| CN104497944A (en) * | 2014-11-18 | 2015-04-08 | 惠晶显示科技（苏州）有限公司 | Developable UV cured hydrofluoric acid-resistant protection glue |
| CN104497204A (en) * | 2014-11-18 | 2015-04-08 | 惠晶显示科技（苏州）有限公司 | Alkali-soluble resin and alkali-soluble resin-containing UV cured hydrofluoric acid-resistant protection glue composition |
| CN105440894A (en) * | 2014-09-28 | 2016-03-30 | 上海维凯光电新材料有限公司 | Light-cured coating composition for metal surface corrosion resistance |
| CN105505287A (en) * | 2016-02-02 | 2016-04-20 | 苏州索梦得电子有限公司 | Waterproof UV glue |
| CN105647399A (en) * | 2016-01-05 | 2016-06-08 | 北京天山新材料技术有限公司 | Ultralow-water-absorptivity UV-curing laminated adhesive |
| CN105713549A (en) * | 2016-02-02 | 2016-06-29 | 苏州索梦得电子有限公司 | UV heating dual-curing glue |
| CN106047269A (en) * | 2016-05-26 | 2016-10-26 | 惠晶显示科技（苏州）有限公司 | Acid-resistant alkali-resistant UV (ultraviolet) glass edge sealing adhesive |
| CN106433492A (en) * | 2016-09-18 | 2017-02-22 | 深圳市华星光电技术有限公司 | Lateral light-shading glue and frameless display device |
| CN106433538A (en) * | 2016-08-31 | 2017-02-22 | 深圳市华星光电技术有限公司 | Visible light curing type frame seal adhesive composition |
| CN106497497A (en) * | 2016-10-09 | 2017-03-15 | 广州惠利电子材料有限公司 | Antiacid peelable glue and its preparation method and application |
| CN106547168A (en) * | 2016-10-28 | 2017-03-29 | 深圳市华星光电技术有限公司 | A kind of black-matrix material compositionss and application |
| CN107384109A (en) * | 2017-07-25 | 2017-11-24 | 烟台德邦科技有限公司 | A kind of high reliability UV solidifications conformal coating and preparation method thereof |
| CN107429123A (en) * | 2015-04-09 | 2017-12-01 | 协立化学产业株式会社 | Light-cured type adhesive composition |
| CN108707449A (en) * | 2018-06-13 | 2018-10-26 | 河源然生新材料有限公司 | A kind of high-performance glass thinning glue and preparation method thereof |
| CN109957368A (en) * | 2017-12-22 | 2019-07-02 | 比亚迪股份有限公司 | A kind of LED-UV solidification Optical adhesive composition, preparation method and its solidify coating |
| CN110997732A (en) * | 2017-08-24 | 2020-04-10 | 株式会社大阪曹达 | Photocurable resin composition, ink, and coating material |
| CN112063356A (en) * | 2020-09-16 | 2020-12-11 | 东莞市派乐玛新材料技术开发有限公司 | Ultraviolet curing adhesive and preparation method and application thereof |
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| CN115044344A (en) * | 2022-07-29 | 2022-09-13 | 浙江国能科技有限公司 | UV hydrolysis adhesive for temporary fixing of microelectronic device and preparation method thereof |
| CN115124970A (en) * | 2022-07-29 | 2022-09-30 | 浙江国能科技有限公司 | Polyurethane three-proofing adhesive and preparation method and application thereof |
| WO2023135855A1 (en) * | 2022-01-12 | 2023-07-20 | 積水フーラー株式会社 | Composition for thin layer glass temporary fixation |
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| CN101392152A (en) * | 2008-09-28 | 2009-03-25 | 广东恒大新材料科技有限公司 | Photo-setting adhesive |
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| CN105440894A (en) * | 2014-09-28 | 2016-03-30 | 上海维凯光电新材料有限公司 | Light-cured coating composition for metal surface corrosion resistance |
| CN105440894B (en) * | 2014-09-28 | 2019-05-31 | 上海维凯光电新材料有限公司 | For Metal surface anti-corrosion light solidifying paint composition |
| CN104497204A (en) * | 2014-11-18 | 2015-04-08 | 惠晶显示科技（苏州）有限公司 | Alkali-soluble resin and alkali-soluble resin-containing UV cured hydrofluoric acid-resistant protection glue composition |
| CN104497944A (en) * | 2014-11-18 | 2015-04-08 | 惠晶显示科技（苏州）有限公司 | Developable UV cured hydrofluoric acid-resistant protection glue |
| CN107429123B (en) * | 2015-04-09 | 2020-09-15 | 协立化学产业株式会社 | Photocurable adhesive composition |
| CN107429123A (en) * | 2015-04-09 | 2017-12-01 | 协立化学产业株式会社 | Light-cured type adhesive composition |
| CN105647399B (en) * | 2016-01-05 | 2018-09-28 | 北京天山新材料技术有限公司 | A kind of UV curing overlay film glue of ultralow water absorption rate |
| CN105647399A (en) * | 2016-01-05 | 2016-06-08 | 北京天山新材料技术有限公司 | Ultralow-water-absorptivity UV-curing laminated adhesive |
| CN105505287A (en) * | 2016-02-02 | 2016-04-20 | 苏州索梦得电子有限公司 | Waterproof UV glue |
| CN105713549B (en) * | 2016-02-02 | 2019-04-26 | 苏州索梦得电子有限公司 | A kind of double solidified glues of UV heating |
| CN105713549A (en) * | 2016-02-02 | 2016-06-29 | 苏州索梦得电子有限公司 | UV heating dual-curing glue |
| CN105505287B (en) * | 2016-02-02 | 2018-07-10 | 苏州索梦得电子有限公司 | A kind of waterproof UV glue |
| CN106047269A (en) * | 2016-05-26 | 2016-10-26 | 惠晶显示科技（苏州）有限公司 | Acid-resistant alkali-resistant UV (ultraviolet) glass edge sealing adhesive |
| CN106433538A (en) * | 2016-08-31 | 2017-02-22 | 深圳市华星光电技术有限公司 | Visible light curing type frame seal adhesive composition |
| CN106433492A (en) * | 2016-09-18 | 2017-02-22 | 深圳市华星光电技术有限公司 | Lateral light-shading glue and frameless display device |
| CN106497497B (en) * | 2016-10-09 | 2019-06-14 | 广州惠利电子材料有限公司 | Antiacid peelable glue and its preparation method and application |
| CN106497497A (en) * | 2016-10-09 | 2017-03-15 | 广州惠利电子材料有限公司 | Antiacid peelable glue and its preparation method and application |
| CN106547168A (en) * | 2016-10-28 | 2017-03-29 | 深圳市华星光电技术有限公司 | A kind of black-matrix material compositionss and application |
| CN107384109B (en) * | 2017-07-25 | 2020-02-07 | 烟台德邦科技有限公司 | High-reliability UV (ultraviolet) curing conformal coating and preparation method thereof |
| CN107384109A (en) * | 2017-07-25 | 2017-11-24 | 烟台德邦科技有限公司 | A kind of high reliability UV solidifications conformal coating and preparation method thereof |
| CN110997732A (en) * | 2017-08-24 | 2020-04-10 | 株式会社大阪曹达 | Photocurable resin composition, ink, and coating material |
| CN110997732B (en) * | 2017-08-24 | 2022-04-15 | 株式会社大阪曹达 | Photocurable resin composition, ink, and coating material |
| CN109957368A (en) * | 2017-12-22 | 2019-07-02 | 比亚迪股份有限公司 | A kind of LED-UV solidification Optical adhesive composition, preparation method and its solidify coating |
| CN108707449A (en) * | 2018-06-13 | 2018-10-26 | 河源然生新材料有限公司 | A kind of high-performance glass thinning glue and preparation method thereof |
| CN112280440A (en) * | 2019-07-25 | 2021-01-29 | 上海飞凯光电材料股份有限公司 | UV adhesive coating, preparation method thereof and preparation method of coated workpiece |
| CN112063356A (en) * | 2020-09-16 | 2020-12-11 | 东莞市派乐玛新材料技术开发有限公司 | Ultraviolet curing adhesive and preparation method and application thereof |
| CN112063356B (en) * | 2020-09-16 | 2022-06-03 | 东莞市派乐玛新材料技术开发有限公司 | Ultraviolet curing adhesive and preparation method and application thereof |
| WO2023135855A1 (en) * | 2022-01-12 | 2023-07-20 | 積水フーラー株式会社 | Composition for thin layer glass temporary fixation |
| CN115044344A (en) * | 2022-07-29 | 2022-09-13 | 浙江国能科技有限公司 | UV hydrolysis adhesive for temporary fixing of microelectronic device and preparation method thereof |
| CN115124970A (en) * | 2022-07-29 | 2022-09-30 | 浙江国能科技有限公司 | Polyurethane three-proofing adhesive and preparation method and application thereof |
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